SPME Literature (Part III)
Compiled by Carlos López C./Chemist
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(1) Comparison of two sample preparation techniques for sniffing experiments with broccoli (Brassica oleracea var. italica Plenck), Ulrich_D, Krumbein_A, Schonhof_I, Hoberg_E, FED CTR BREEDING RES CULTIVATED PLANTS,INST QUAL ANAL,NEUER WEG 22-23,D-06484 QUEDLINBURG,GERMANY INST VEGETABLE & ORNAMENTAL CROPS,GROSSBEEREN,GERMANY, NAHRUNG-FOOD, 1998, Vol.42, No.6, pp.392-394 . The suitability of the headspace solid phase microextraction (HS-SPME) for gas chromatography-olfactometry (GC-O) with aroma extract dilution analysis in comparison to the dynamic head space sampling on a Tenax trap was tested exemplarily by the aroma volatiles of fresh broccoli. A high number of odour sensations in qualitative olfactometry was registered with both sample preparation techniques. The key aroma compounds of the fresh broccoli material are represented by high flavour dilution factors with dynamic head space sampling and headspace SPME. The SPME method has found to be a convenient and fast technique suitable especially for qualitative GC-O. The adsorption selectivity of the fiber and the substance discrimination have to be taken into account for quantitative use like aroma extract dilution analysis.
(2) Solid-phase microextraction (SPME) of drugs and poisons from biological samples, Liu_JT, Cheng_P, Suzuki_O, CHINA MED UNIV,DEPT FORENS CHEM,NEW DELHI 110001,INDIA HAMAMATSU UNIV,SCH MED,DEPT LEGAL MED,HAMAMATSU,SHIZUOKA 43131,JAPAN, FORENSIC SCIENCE INTERNATIONAL, 1998, Vol.97, No.2-3, pp.93-100 . Solid-phase microextraction (SPME), a new solvent-free sample preparation technique, was invented by C. Arthur and J. Pawliszyn in 1990. This method mainly was applied for the extraction of volatile and semi-volatile organic pollutants in water samples. However, since 1995, SPME has been developed to various biological samples, such as whole blood, plasma, urine, hair and breath, in order to extract drugs and poisons in forensic field. The main advantages of SPME are: high sensitivity, solventless, small sample volume, simplicity and rapidity. We have reviewed the papers published in recent years about SPME in biological samples, and sorted out main experimental conditions, such as fibers, matrixes, the extraction approaches and time, as well as the acceleration method. We would expect SPME technique to have a promising future for toxicological analysis in forensic practice.
(3) Use of automated SPME coupled to GC-AED for the determination of metazachlor in waste water, Wenner_A, Wortberg_M, BASF AG,BASF AGR CTR LIMBURGERHOF,POB 120,D-67114 LIMBURGERHOF,GERMANY BASF AG,BASF AGR CTR LIMBURGERHOF,D-67114 LIMBURGERHOF,GERMANY, HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY, 1998, Vol.21, No.12, pp.661-664 IS: 0935-6304.
(4) Determination of urinary mercury and methylmercury by solid phase microextraction and GC/MS, Guidotti_M, Vitali_M, PMP USL RIETI,VIA SALARIA AQUILA 8,I-02100 RIETI,ITALY UNIV ROMA LA SAPIENZA,IST IGIENE G SANARELLI,CATTEDRA IGIENE AMBIENTALE,I-00185 ROME,ITALY, HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY, 1998, Vol.21, No.12, pp.665-666 IS: 0935-6304 .
(5) The application of solid phase microextraction in the analysis of organophosphorus pesticides in a food plant AU: Chen_WQ, Poon_KF, Lam_MHW NA: CITY UNIV HONG KONG,DEPT BIOL & CHEM,CTR ENVIRONM SCI & TECHNOL,TAT CHEE AVE,KOWLOON,HONG KONG CITY UNIV HONG KONG,DEPT BIOL & CHEM,CTR ENVIRONM SCI & TECHNOL,KOWLOON,HONG KONG XIAMEN UNIV,SEDC LAB MARINE ECOL ENVIRONM,XIAMEN,PEOPLES R CHINA XIAMEN UNIV,ENVIRONM SCI RES CTR,XIAMEN,PEOPLES R CHINA JN: ENVIRONMENTAL SCIENCE & TECHNOLOGY, 1998, Vol.32, No.23, pp.3816-3820 IS: 0013-936X DT: Article AB: A SPME method for the determination of organophosphorus pesticide residues in a local food plant, Chrysanthemum coronarium, was established. Pesticide residues were extracted by SPME fiber (with 100 mu m poly(dimethylsiloxane) coating) from a biphasic water/plant tissues mixture and determined by GC-FPD. An equilibrium model was derived for the system and revealed that pesticide recoveries were related to the water:plant tissues ratio, f(r) and the partition coefficient, K-WV, for the distribution of pesticides between the aqueous phase and the plant tissues. The model was verified by four organophosphorus pesticides, namely phorate, diazinon, methyl parathion, and ethion. The best fitted K-WV values (P < 0.05) for the pesticides were found to be 4.73 +/- 0.32 x 10(-2) (phorate); 1.11 +/- 0.10 x 10(-1) (diazinon); 9.18 +/- 0.95 x 10(-2) (methyl parathion); and 8.21 +/- 1.28 x 10(-3) (ethion). Remarkable correlation between the K-WV of the organophosphorus pesticides and their octanol/water partition coefficients, K- OW, was also established.
(6) Optimization of solid-phase microextraction for the speciation of butyl- and phenyltins using experimental designs AU: Lespes_G, Desauziers_V, Montigny_C, PotinGautier_M NA: ECOLE MINES,LAB GENIE ENVIRONM IND,6 AVE CLAVIERES,F-30319 ALES,FRANCE ECOLE MINES,LAB GENIE ENVIRONM IND,F-30319 ALES,FRANCE JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.826, No.1, pp.67-76 IS: 0021-9673 DT: Article AB: This paper deals with the optimization of solid-phase microextraction (SPME) for organotin speciation in water. The analytical method consists of an in situ ethylation, simultaneous solid-phase microextraction of the derivatives, followed by a gas chromatographic analysis with flame photometric detection. Experimental design methodology was used to evaluate the influence of six analytical parameters on the mean peak area (S-mean). The adsorption of the compounds on the SPME fibre was found to be the most important parameter and two other factors are positively significant: the adsorption time and the sample volume. The adsorption profiles and the optimal operating conditions were determined from the modelling of S- mean. The detection limits range from 2 to 4 ng l(-1) (monophenyltin excepted: 18 ng l(-1)) and linearity is from 50 to 600 ng l(-1). The relative standard deviations are 7-10% for five determinations. Water samples were analysed in order to verify the accuracy of the optimized method by comparing results with those obtained using a conventional solvent extraction of the ethylated organotins.
(7) Determination of the plasticizer N-butylbenzenesulfonamide and the pharmaceutical Ibuprofen in wastewater using solid phase microextraction (SPME) AU: Huppert_N, Wurtele_M, Hahn_HH NA: UNIV KARLSRUHE,INST AQUAT ENVIRONM ENGN,AM FASANENGARTEN,D- 76128 KARLSRUHE,GERMANY JN: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY, 1998, Vol.362, No.6, pp.529-536 IS: 0937-0633 DT: Article AB: A rapid, inexpensive and solvent-free method for the simultaneous determination of the polyamide plasticizer N- butylbenzenesulfonamide (NBBS) and the widely used pharmaceutical Ibuprofen by solid phase microextraction (SPME) combined with gas chromatography/mass spectrometry (GC/MSD) in wastewater samples was developed. Besides the optimized analytical conditions, results of investigations with varying analytical parameters are reported. Problems, which may occur during the analytical procedure (e.g. salt deposits, adsorption phenomena, carry-over), are discussed. For the determination of Ibuprofen, it is important to carry out the extraction under acidic conditions with sufficiently buffered samples; the GC/MSD system must be very clean and well maintained. SPME allows an extraction of Ibuprofen without derivatization of its carboxylic group. For quantification in complex matrices, the standard addition technique is necessary. Limit of detection and limit of determination are 0.1 mu g/L for both analytes. NBBS and Ibuprofen were detected in several raw and treated wastewater samples from municipal wastewater treatment plants in the range from < 0.1 to 3.5 mu g/L. KP: ORGANIC-COMPOUNDS, BUTYL BENZENESULFONAMIDE, WATER, MS, IDENTIFICATION, POLLUTANTS
(8) Application of SPME (solid phase micro-extraction) to the analysis of drinkable water from three locations in the state of Sao Paulo. LA: Portuguese AU: Valente_ALP, Augusto_F, Montero_L, daRocha_EC, Pawliszyn_J NA: UNICAMP,INST QUIM,CP 6154,BR-13083970 CAMPINAS,SP,BRAZIL UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA JN: QUIMICA NOVA, 1998, Vol.21, No.6, pp.804-806 IS: 0100-4042 DT: Article AB: The technique of solid phase microextraction (SPME) was used for the extraction of halogenated contaminants of water samples from three cities of the State of Sao Paulo and the extracts were submitted to gas chromatographic analysis with electron capture detection (GC-ECD). In the samples of water collected at the city of Sao Paulo the detected level of trihalomethanes (THM) expressed as the sum of chloroform, dibromochloromethane and dichlorobromomethane, were higher than the permissible limit established by the Brazilian regulation, In the samples collected at the two other cities the level of any of the three THM remained below the sensitivity of the ECD.
(9) Solid phase microextraction coupled to capillary electrophoresis AU: Whang_CW, Pawliszyn_J NA: TUNGHAI UNIV,DEPT CHEM,TAICHUNG 40704,TAIWAN UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA JN: ANALYTICAL COMMUNICATIONS, 1998, Vol.35, No.11, pp.353-356 IS: 1359-7337 DT: Article AB: An on-column interface, coupling the solid phase microextraction (SPME) sampling technique with capillary electrophoresis (CE), has been constructed. This interface facilitates the direct insertion of a thin silica fiber into the inlet end of a separation capillary and, therefore, the zero-dead volume connection requirement for hyphenation between SPME and CE is fully realized. The performance of the interface was evaluated by SPME-CE analysis of the priority pollutant phenols using a laboratory-made 40 mu m od poly(acrylate) (PA)- coated silica fiber connected to a 75 mu m id separation capillary. The results clearly demonstrate that the interface is effective for on-line coupling SPME with CE.
(10) Headspace solid phase microextraction for the analysis of volatiles in a meat product: Dry-cured Iberian ham AU: Ruiz_J, Cava_R, Ventanas_J, Jensen_MT NA: UNIV EXTREMADURA,FAC VET,CACERES 10071,SPAIN DANISH INST AGR SCI,RES CTR FOULUM,DEPT ANIM PROD QUAL,DK-8830 TJELE,DENMARK JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, Vol.46, No.11, pp.4688-4694 IS: 0021-8561 DT: Article AB: The application of solid-phase microextraction (SPME) combined with gas chromatography/mass spectrometry for the analysis of dry-cured Iberian ham volatile compounds has been studied. To determine the optimal conditions to extract volatile compounds, several extraction times and temperatures conditions were tested. The majority of the 82 volatile compounds tentatively identified coincided with those reported for different types of dry-cured ham in the literature. In addition, SPME successfully extracted high molecular weight compounds, some of them being reported for the first time in this type of meat product. Both extraction time and temperature dramatically increased less volatile compounds' chromatographic area and consequently total area (P < 0.0001).
(11) Use of digital aroma technology and SPME CC-MS to compare volatile compounds produced by bacteria isolated from processed poultry AU: Arnold_JW, Senter_SD NA: USDA,RICHARD B RUSSELL AGR RES CTR,POB 5677,ATHENS,GA,30604 JN: JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, 1998, Vol.78, No.3, pp.343-348 IS: 0022-5142 DT: Article AB: Digital aroma technology, solid-phase micro-extraction (SPME) and gas chromatographic mass spectral (GC-MS) analysis of the headspace volatile organic compounds were used to compare bacterial species important for food safety and common to biofilms in the poultry processing environment. The instrument for digital aroma technology, called the electronic nose, measured changes in resistance of polymer sensors caused by volatile gases from the headspace of samples. Graphical output by the Sammon mapping technique produced patterns of differences or similarities among the samples. Artificial neural network software was used to model groups of samples and classify subsequent unknowns. Compounds isolated from the headspace of sealed cultures using polydimethylsiloxane SPME fibres and identified by GC-MS analyses were predominantly alcohols and indole. These qualitative profiles were repetitive for specific organisms in relation to purity and repeatability of the cultures, differed by species and were used as objective standards to compare the graphical outputs of the electronic nose.
(12) Solid phase microextraction in headspace analysis. Dynamics in non-steady state mass transfer AU: Ai_J NA: INT PAPER,CORP RES CTR,1422 LONG MEADOW RD,TUXEDO PK,NY,10987 US TOBACCO MFG CO INC,NASHVILLE,TN,37203 JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.22, pp.4822-4826 IS: 0003-2700 DT: Article AB: Previously proposed models (Ai, J. Anal. Chem. 1997, 69, 1230- 6; 3260-6) dealing with the dynamics of solid-phase microextraction (SPME) were based on the assumption that a steady-state mass transfer is in effect throughout the SPME extraction process. In reality, a steady-state mass transfer may not be established at the initial stage of headspace SPME, which involves mass transfer across two interfaces. The rate of analyte transfer at the condensed phase/headspace interface may not be equal to the extraction rate at the headspace/SPME polymer film interface. An improved model is proposed in this report to handle the situation of the non-steady-state mass transfer for the headspace SPME. A mathematical solution is obtained for the dynamic process of the non-steady-state mass transfer by correlating the variation of the analyte concentration in the headspace with the analyte extraction rate. This solution provides an equation relating the extracted amount of analyte to the extraction time a little more complicated than the previous models. It also gives a better description of experimental observations.
(13) Analysis of estrogens and anabolic steroids by SPME with on- fiber derivatization and GC/MS AU: Okeyo_PD, Snow_NH NA: SETON HALL UNIV,DEPT CHEM,400 S ORANGE AVE,S ORANGE,NJ,07079 SETON HALL UNIV,DEPT CHEM,S ORANGE,NJ,07079 JN: JOURNAL OF MICROCOLUMN SEPARATIONS, 1998, Vol.10, No.7, pp.551- 556 IS: 1040-7685 DT: Article AB: The solid-phase micro-extraction (SPME), Bis(trimethylsilyl) trifluoroacetamide (BSTFA) headspace derivatization on the SPME fiber, and gas chromatography-mass spectrometry (GC/MS) analysis of steroids from aqueous and biological solutions are shown. The effects of extraction and derivatization parameters have been shown. The extraction time of several steroids was shown to be approximately 30 min., which is typical of SPME methods. The analyte solution pH and ionic strength may have dramatic effects on the extraction recovery and should be optimized as part of method development. The incubation temperature may have several influences on the recovery from the derivatization reaction. Each analyte has a separate optimum temperature for derivatization. Thus, for mixtures, a compromise will be necessary. The analysis of anabolic steroids of abuse is shown. A detection limit of less than 200 pg/mL for testosterone from water is seen. Calibration for testosterone from water indicates a linear range to at least 1000 ng/ml, or three to four orders of magnitude. Several other steroids were extracted from urine at 10-100 ng/mL levels, and calibration for these compounds also exhibited linear behavior. The SPME with on-fiber headspace derivatization is a promising technique for the analysis of polar or nonvolatile compounds.
(14) Analysis of water samples for trace levels of oxygenate and aromatic compounds using headspace solid-phase microextraction and comprehensive two-dimensional gas chromatography AU: Gaines_RB, Ledford_EB, Stuart_JD NA: US COAST GUARD ACAD,DEPT SCI,NEW LONDON,CT ZOEX CORP,LINCOLN,NE,68502 UNIV CONNECTICUT,DEPT CHEM U60,STORRS,CT,06269 JN: JOURNAL OF MICROCOLUMN SEPARATIONS, 1998, Vol.10, No.7, pp.597- 604 IS: 1040-7685 DT: Article AB: Headspace solid-phase microextraction (SPME) and comprehensive two-dimensional gas chromatography (C2DGC) have been applied to the quantitative analysis of trace levels of oxygenate and aromatic compounds. The oxygenates studied were methyl-tert- butyl ether (MTBE) and ethyl butyl ether (EBE). The aromatics studied were the BTEX compounds, benzene, toluene, ethylbenzene, and xylenes. Both the oxygenates and aromatics are components of gasoline commonly found in groundwater near leaking underground storage tanks. The method involves extraction and preconcentration using a fused-silica fiber coated with a combination of polydimethylsiloxane and porous carbon followed by a volatility-by-polarity comprehensive two- dimensional gas chromatographic analysis with flame ionization detection. Experimental results yielded method detection limits of 360-630 parts per trillion (v/v), with calibration plots exhibiting a linear range over approximately three orders of magnitude. Reproducibility, as indicated by typical relative standard deviation (RSD) values for replicate runs, was 10%. C2DGC resolved all oxygenate and BTEX components from all traditional one-dimensional GC coeluters present in standard gasoline samples. The method is fast, is experimentally simple, and uses no solvent, (C) 1998 John Wiley & Sons, Inc.*. KP: GASOLINE WA: solid-phase microextraction, headspace, comprehensive two- dimensional gas chromatography, thermal modulator, groundwater monitoring, MTBE, BTEX
(15) Determination of chlorophenols using SPME and GC/MS AU: Guidotti_M, Ravaioli_G NA: PRESIDIO MULTIZONALE PREVENZ,SETTORE AMBIENTE,VIA SALARIA AQUILA 8,I-02100 RIETI,ITALY JN: ANNALI DI CHIMICA, 1998, Vol.88, No.9-10, pp.629-635 IS: 0003-4592 DT: Article AB: This paper presents a method for the analysis of chlorophenols in water samples using the solid phase microextraction (SPME) technique and GC-MS. This method was applied to the analysis of these micro-pollutants in the water samples coming from twelve different aqueducts in the Rieti province and in the water of the river Turano. This method proved to be fast, reliable and accurate, together with being suited for routine analysis as it eliminates lengthy extraction procedures; as well as a drastic reduction of solvents use, makes it environmentally friendly.
(16) Using solid-phase microextraction to determine partition coefficients to humic acids and bioavailable concentrations of hydrophobic chemicals AU: Ramos_EU, Meijer_SN, Vaes_WHJ, Verhaar_HJM, Hermens_JLM NA: UNIV UTRECHT,TOXICOL RES INST,ENVIRONM TOXICOL & CHEM SECT,POB 80-176,NL-3508 TD UTRECHT,NETHERLANDS UNIV UTRECHT,TOXICOL RES INST,ENVIRONM TOXICOL & CHEM SECT,NL- 3508 TD UTRECHT,NETHERLANDS JN: ENVIRONMENTAL SCIENCE & TECHNOLOGY, 1998, Vol.32, No.21, pp.3430-3435 IS: 0013-936X DT: Article AB: In the current study, the suitability of negligible depletion solid-phase microextraction (nd-SPME) to determine free fractions of chemicals in aquatic environments was explored. The potential interferences of the dissolved matrix (i.e., humic acids) with the SPME measurements were tested. Results show that nd-SPME measures only the freely dissolved fraction and that the measurements are not disturbed by the humic acids. In addition, nd-SPME was used to determine partition coefficients between dissolved organic carbon and water for four hydrophobic chemicals. Obtained values are in excellent agreement with previously reported data. Finally, the bioaccumulation of hexachlorobenzene and PCB 77 to Daphnia magna was determined in the presence and absence of humic acids. The bioconcentration factors (BCF) were calculated based on total as well as on free concentration. Lower BCF values are obtained in the presence of humic acids using total concentrations, whereas equal BCFs are found using free concentrations measured with nd-SPME. Therefore, we can conclude that negligible depletion SPME is a good technique to determine bioavailable concentrations of hydrophobic chemicals in aquatic environments.
(17) Analysis of volatile organic compounds in environmental water samples and soil gas by solid-phase microextraction AU: Nilsson_T, Montanarella_L, Baglio_D, Tilio_R, Bidoglio_G, Facchetti_S NA: COMMISS EUROPEAN COMMUNITIES,INST ENVIRONM,I-21020 ISPRA,VA,ITALY JN: INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY, 1998, Vol.69, No.3, pp.217-226 IS: 0306-7319 DT: Article AB: The basic principle of solid-phase microextraction (SPME) is equilibration. Therefore, all possible interferences on the extraction process should be taken into account in order to perform a reliable calibration for the quantitative analysis of environmental samples. Humic acids and suspended mineral oxides showed no effect on the SPME analysis of volatile organic compounds (VOCs), whereas salt had a positive effect on the extraction efficiency. The linearity was good in all cases, the precision of repeated analysis was around 5% average standard deviation, and detection limits were in the ng/l range. Thus, SPME can be applied for the quantitative analysis of VOCs in various environmental water samples, such as sea water, groundwater and heterogeneous samples like river and lake water containing suspended solids. SPME was established also as an alternative to liquid-liquid extraction in the study of TiO2- catalysed photodegradation mechanisms. Finally, two new SPME sampling probes were designed and tested for rapid, on-site measurements of organic micropollutants in groundwater and soil gas. SPME is suited ideally to provide low-cost evaluation of groundwater properties in unconventional hydrogeologic settings, such as underground excavations, and to provide preliminary data on which to base the selection of boreholes for more extensive casing installation and instrumentation.
(18) Development of a technique for the analysis of inorganic mercury salts in soils by gas chromatography mass spectrometry AU: Barshick_CM, Barshick_SA, Britt_PF, Lake_DA, Vance_MA, Walsh_EB NA: OAK RIDGE NATL LAB,DIV CHEM & ANALYT SCI,OAK RIDGE,TN,37831 JN: INTERNATIONAL JOURNAL OF MASS SPECTROMETRY, 1998, Vol.178, No.1-2, pp.31-41 IS: 1387-3806 DT: Article AB: A technique has been developed to analyze environmentally relevant samples for organic and inorganic mercury compounds. A solid phase microextraction (SPME) fiber was used as a sampling medium in both water and water/soil slurries. Quantification of inorganic mercury was accomplished through a chemical alkylation reaction designed to convert an inorganic mercury salt to an organomercury compound prior to GC/MS analysis; this was found to be the rate limiting step in the analysis. Two alkylating reagents were investigated: methylpentacyanocobaltate (III) (K-3[Co(CN)(5)CH3]) and methylbis(dimethylglyoximato)pyridinecobalt (III) (CH3Co(dmgH(2)Py). Methylbis(dimethylglyoximato)pyridinecobalt (III) was found to be superior for this application because it produced a single reaction product, methylmercury iodide, with an efficiency of similar to 95%. Detection limits were similar to 7 ppb in water and similar to 2 ppm in soil. The poorer results in soil were due to an increase in background signal (similar to 10 times compared to water) and a reduction in analyte signal las much as 100 times). This reduction in signal intensity is believed to be caused by complex soil chemistry. Manipulation of the solution chemistry [e.g. oxidation of mercury (0) --> mercury (II)], before or during the alkylation step, may improve the detection limits and increase the number of elements amenable to analysis. (Int J Mass Spectrom 178 (1998) 31-41)
(19) Headspace solid-phase microextraction for the determination of volatile and semi-volatile pollutants in water and air AU: Llompart_M, Li_K, Fingas_M NA: UNIV SANTIAGO,FAC QUIM,DEPT QUIM ANALIT NUTR & BROMATOL,E-15706 SANTIAGO COMPOSTE,SPAIN ENVIRONM CANADA,ENVIRONM TECHNOL CTR,EMERGENCIES SCI DIV,OTTAWA,ON K1A 0H3,CANADA JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.824, No.1, pp.53-61 IS: 0021-9673 DT: Article AB: In this work we report the use of solid-phase microextraction (SPME) to extract and concentrate water-soluble volatile as well as semi-volatile pollutants. Both methods of exposing the SPME fibre were utilised: immersion in the aqueous solution (SPME) and in the headspace over the solution (HSSPME). The proposed HSSPME procedure was compared to conventional static headspace (HS) analysis for artificially spiked water as well as real water samples, which had been, equilibrated with various oil and petroleum products. Both techniques gave similar results but HSSPME was much more sensitive and exhibited better precision. Detection limits were found to be in the sub-ng/ml level, with precision better than 5% R.S.D. in most cases. To evaluate the suitability of SPME for relatively high contamination level analysis, the proposed HSSPME method was applied to the screening of run-off water samples that had heavy oil suspended in them from a tire fire incident. HSSPME results were compared with liquid-liquid extraction. Library searches were conducted on the resulting GC-MS total ion chromatograms to determine the types of compounds found in such samples. Both techniques found similar composition in the water samples with the exception of alkylnaphthalenes that were detected only by HSSPME. A brief study was carried out to assess using SPME for air monitoring. By sampling and concentrating the volatile organic compounds in the coating of the SPME fibre without any other equipment, this new technique is useful as an alternative to active air monitoring by means of sampling pumps and sorbent tubes.
(20) Determination of methylmercury in biological samples and sediments by capillary gas chromatography coupled with atomic absorption spectrometry after hydride derivatization and solid phase microextraction AU: He_B, Jiang_GB, Ni_ZM NA: CHINESE ACAD SCI,ECOENVIRONM SCI RES CTR,POB 2871,BEIJING 100085,PEOPLES R CHINA CHINESE ACAD SCI,ECOENVIRONM SCI RES CTR,BEIJING 100085,PEOPLES R CHINA JN: JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, 1998, Vol.13, No.10, pp.1141-1144 IS: 0267-9477 DT: Article AB: A method for the extraction and determination of methylmercury in biological samples and sediments by solid phase microextraction (SPME) combined with capillary gas chromatography-atomic absorption spectrometry (GC-AAS) has been proposed. The methylmercury chloride was converted to its hydride form by potassium tetrahydroborate (KBH4) in a closed headspace vial prior to extraction. A laboratory-assembled SPME device including a capillary fused-silica fiber and a modified microsyringe was used throughout the experiment. The extraction is an equilibrium process that depends on the methylmercury hydride partitioning between the liquid phase and the fiber. When the equilibrium was reached, the fiber was directly transferred to a GC column by means of the microsyringe, where the analyte was thermally desorbed inside a heated injector and subsequently the column effluent was atomized by a heated stainless steel tube and detected by an on-line coupled AAS. Several factors affecting the SPME procedure such as fiber pretreatment with hydrofluoric acid, pH buffering, addition of salt and sampling time have been investigated and optimized. The reproducibility of the SPME procedure was 91% and the detection limit based on the signal equal to 3 times the baseline noise, was 26 ng. The method was applied to determination of methylmercury in biological samples and sediments.
(21) Use of a simple method for sampling cuticular hydrocarbons from live social wasps AU: Turillazzi_S, Sledge_MF, Moneti_G NA: UNIV FLORENCE,DIPARTIMENTO BIOL ANIM & GENET,VIA ROMANA 17,I- 50125 FLORENCE,ITALY UNIV FLORENCE,DIPARTIMENTO BIOL ANIM & GENET,I-50125 FLORENCE,ITALY JN: ETHOLOGY ECOLOGY & EVOLUTION, 1998, Vol.10, No.3, pp.293-297 IS: 0394-9370 DT: Article AB: The classical methods of cuticular hydrocarbon extraction in insects involve the use of solvents and therefore the killing of specimens. We describe here a simple and inexpensive method that allows for the sampling of cuticular hydrocarbons from live social insects in the field. We compare the results of our method with those of the classical solvent extraction method, as well as those of solid phase micro-extraction (SPME), and show that the method is both reliable and suitable for use in the natural environment. We describe For the first time the cuticular compounds of the social wasp Polistes nimphus.
(22) Solvent-free method for the determination of polynuclear aromatic hydrocarbons in waste water by solid-phase microextraction high performance liquid chromatography with photodiode-array detection AU: Negrao_MR, Alpendurada_MF NA: UNIV OPORTO,FAC PHARM,HYDROL LAB,RUA ANIBAL CUNHA 164,P-4050 OPORTO,PORTUGAL UNIV OPORTO,FAC PHARM,HYDROL LAB,P-4050 OPORTO,PORTUGAL WATER INST NO REG,P-4050 OPORTO,PORTUGAL JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.823, No.1-2, pp.211-218 IS: 0021-9673 DT: Article AB: Solid-phase microextraction (SPME) has rapidly been established among the practical alternatives for sample preparation for gas chromatography. Nevertheless polynuclear aromatic hydrocarbons (PAHs) are more effectively monitored by high-performance Liquid chromatography (HPLC), but initially, there was no simple way to introduce analytes extracted by SPME into an HPLC system. A SPME-HPLC interface was developed by Supelco, which enables one to take advantages of the time and solvent savings offered by SPME. In the present work six PAHs from the European Union directives: fluoranthene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, benzo[ghi]perylene, indeno[1,2,3-cd]pyrene were evaluated after optimization of a sample preparation method with a 100-mu m poly(dimethylsiloxane) fiber. Repeatability, reproducibility, correlation coefficients, linearity, recoveries and limits of detection where determined and are indicated.
(23) Analysis of volatile halogenated hydrocarbons in water by solid-phase microextraction and GC-MS LA: Czech AU: Janda_V, Viden_I NA: INST CHEM TECHNOL,TECH 5,CR-16628 PRAGUE 6,CZECH REPUBLIC JN: CHEMICKE LISTY, 1998, Vol.92, No.9, pp.751-755 IS: 0009-2770 DT: Article AB: Experience with solid-phase microextraction (SPME) in the analysis of volatile halogenated hydrocarbons in water samples is described. Gas chromatography-mass spectrometry was used as the final analytical method. It was found that SPME provides reproducible results, especially when the method of internal standard is used for the calibration. The detection limit of the SPME-GC-MS is below 1 mu g.1(-1) for most of the volatile halogenated hydrocarbons tested, even if the MS instrument is operated in the full-scan mode. Advantages of the SPME can be summarized as follows: the method is simple, rapid and straightforward, does not require solvents, and only a small volume of water sample is needed.
(24) Determination of geosmin and 2-methylisoborneol in water using solid-phase microextraction and gas chromatography-chemical ionisation electron impact ionisation-ion-trap mass spectrometry AU: McCallum_R, Pendleton_P, Schumann_R, Trinh_MU NA: UNIV S AUSTRALIA,SCH CHEM TECHNOL,POROUS MAT RES GRP,THE LEVELS CAMPUS,MAWSON LAKES,SA 5095,AUSTRALIA UNIV S AUSTRALIA,SCH CHEM TECHNOL,POROUS MAT RES GRP,MAWSON LAKES,SA 5095,AUSTRALIA JN: ANALYST, 1998, Vol.123, No.10, pp.2155-2160 IS: 0003-2654 DT: Article AB: A method for the determination of geosmin and 2- methylisoborneol (MIB) in water by solid-phase microextraction (SPME) is presented. Various SPME fibre chemistries have been compared for their efficiency in extracting MIB from water. Extraction conditions including the extraction time and temperature have been optimised. A 30 ml water sample is extracted for 20 min at 60 degrees C using a divinylbenzene fibre, and the extract analysed by gas chromatography with ion- trap mass spectrometry detection. d(5)-Geosmin and d(3)-MIB are added as internal standards to compensate for any variability in the SPME process which is not carried out to equilibrium. Chemical ionisation, using acetonitrile as the reagent gas, was found to give superior sensitivity to electron impact ionisation (EI) for the detection of MIB. EI was used as the ionisation mode for detection of geosmin. The method shows good linearity over the concentration range 5-40 ng l(-1) and gives detection limits of 1 ng l(-1) for both geosmin and MIB. Recovery (93-110%) and precision (3-12%) over this concentration range, for both raw and treated drinking waters, are comparable to currently employed methods such as closed- loop stripping analysis (CLSA). The method offers the advantage of being simple to use, with much shorter analysis times in comparison to CLSA.
(25) Determination of amphetamine, methamphetamine and dimethamphetamine in human urine by solid-phase microextraction (SPME) gas chromatography mass spectrometry AU: Myung_SW, Min_HK, Kim_S, Kim_M, Cho_JB, Kim_TJ NA: KOREA ADV INST SCI & TECHNOL,BIOANAL & BIOTRANSFORMAT RES CTR,POB 131,SEOUL 130650,SOUTH KOREA KYONGGI UNIV,DEPT CHEM,SUWON 440760,SOUTH KOREA JN: JOURNAL OF CHROMATOGRAPHY B, 1998, Vol.716, No.1-2, pp.359-365 IS: 0378-4347 DT: Article AB: A simple and rapid assay method for three stimulant drugs (amphetamine, methamphetamine, and dimethamphetamine) in human urine using solid-phase microextraction was developed. In solid-phase microextraction, the drugs were equilibrated between the adsorbent coated-fiber and aqueous sample matrix. After adsorption of the analytes, the fiber was directly transferred to the injector of a gas chromatograph, where the analytes were thermally desorbed and subsequently separated by the gas chromatograph and detected by mass spectrometer. The solid-phase microextraction method, which did not require solvents, was found to be a fast and simple analytical method. We optimized the solid-phase microextraction technique, for factors such as the NaCl salt effect (30%), pH effect (pH=12.4), equilibration time (30 min), desorption time (1 min) and coated-fiber type (100 mu m poly(dimethylsiloxane)) and detected the stimulants in human urine, obtained from human subjects. The detection limits of each drug were below 1-10 ng/ml. The developed method can be applied to the abused drug test. (C) 1998 Elsevier Science B.V. All rights reserved.
(26) Solid-phase microextraction and gas chromatography for rapid analysis of pesticides AU: Miege_C, Dugay_J NA: ECOLE SUPER PHYS & CHIM IND VILLE PARIS,LAB ENVIRONM & CHIM ANALYT,CNRS,ERS 657,10 RUE VAUQUELIN,F-75231 PARIS 05,FRANCE JN: ANALUSIS, 1998, Vol.26, No.6, pp.M137-M143 IS: 0365-4877 DT: Article AB: Solid-phase microextraction (SPME) combined with gas chromatography (GC) is a fast and simple technique for the handling of aqueous samples using coated fused-silica fibres. Fully automated devices are commercially available. Several applications have demonstrated the potential of the technique for both screening and quantification of pesticides in water samples with detection limits in the range from 5 to 100 ng/L using mass spectrometry detection.
(27) Solid-phase microextraction gas chromatography direct deposition infrared spectrometry as a convenient method for the determination of volatile compounds from living organisms AU: Auger_J, Rousset_S, Thibout_E, Jaillais_B NA: UNIV TOURS,UPRESA 6035 CNRS,IRBI,PARC GRANDMONT,F-37200 TOURS,FRANCE UNIV TOURS,SAVIT,F-37200 TOURS,FRANCE JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.819, No.1-2, pp.45-50 IS: 0021-9673 DT: Article AB: Gas chromatography-direct deposition infrared spectrometry (GC- DD-IR) permits coupling of GC to IR at a level of sensitivity of routine GC-MS coupling but the presence of ice resulting from Living organisms limits the usefulness of the system. Headspace solid-phase microextraction (SPME) coupled to GC-DD- IR leads to a rigorous absence of water and can be applied to unknown volatiles trapped in situ in combination with SPME-GC- MS. For instance we succeeded in identification of the asparagus fly male pheromone and 1 min of an individual emission is sufficient to obtain a good LR spectrum in real time.
(28) Strategies for the analysis of chlorobenzenes in soils using solid-phase microextraction coupled with gas chromatography ion trap mass spectrometry. AU: Sarrion_MN, Santos_FJ, Galceran_MT NA: UNIV BARCELONA,DEPT QUIM ANALIT,DIAGONAL 647,E-08028 BARCELONA,SPAIN UNIV BARCELONA,DEPT QUIM ANALIT,E-08028 BARCELONA,SPAIN JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.819, No.1-2, pp.197-209 IS: 0021-9673 DT: Article AB: Solid-phase microextraction (SPME) was examined as a possible alternative to Soxhlet extraction in the analysis of chlorobenzenes at high concentrations (up to 65 mu g g(-1)) in soils. Gas chromatography-ion trap mass spectrometry (GC-IT-MS) was used and different strategies were tested in order to obtain suitable responses for chlorobenzenes. Two headspace SPME methods, using fibres coated with polydimethylsiloxane (PDMS) as stationary phase, in splitless and split injection modes, respectively, and a direct SPME method using 100-mu m PDMS fibre were studied. For headspace SPME, 7-mu m and 100-mu m PDMS fibres were used and good sensitivity was obtained by adding 200 mu l of water to the soil, at a sampling temperature of 30 degrees C and absorption times of 40 and 60 min, respectively. For direct SPME, which involves extraction of chlorobenzenes from stirred soil solutions using a 100-mu m PDMS fibre, the effect of the addition of different organic solvents, such as methanol or acetone, on the sensitivity and the extraction time was evaluated. The shortest time to reach equilibrium (50 min) was achieved when a mixture acetone-water (30:70) was added to the sample. Repeatabilities lower than 8% were obtained for headspace and direct SPME with 100-mu m PDMS fibre, whereas for 7-mu m PDMS fibre, repeatabilities were slightly higher (between 7 and 11%). The SPME methods were applied to the analysis of chlorobenzenes in an industrially contaminated clay soil, CRM-530, which is a candidate reference material. Chlorobenzenes in this soil were quantified by standard addition, which led to good reproducibility (R.S.D. between 2 and 10%) for headspace and direct SPME with the 100- mu m PDMS fibre and acceptable detection Limits (30 to 100 pg g(-1) of soil). The results were consistent with those obtained in a European intercomparison exercise.
(29) Application of solid phase microextraction and gas chromatography time-of-flight mass spectrometry for rapid analysis of flavor volatiles in tomato and strawberry fruits AU: Song_J, Fan_LH, Beaudry_RM NA: MICHIGAN STATE UNIV,DEPT HORT,E LANSING,MI,48824 JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, Vol.46, No.9, pp.3721-3726 IS: 0021-8561 DT: Article AB: Solid phase microextraction (SPME), a relatively new sampling technique, was examined as a means to investigate volatile compounds produced by tomato (Lycopersicon esculentum Mill.) and strawberry (Fragaria x ananassa Duch.) fruit. SPME had sufficient sorptive capacity to permit detection of aroma compounds having a variety of functional groups. The advantages of using SPME were its simplicity, absence of solvent, and speed. Fiber cleaning, sample collection, and desorption required similar to 6 min. The total analysis time was similar to 10 min per sample when SPME was combined with rapid gas chromatographic (GC) separation and time-of-flight mass spectrometry (TOFMS). The major volatile compounds detected from tomato and strawberry and their relative abundance were comparable with published results from purge-and-trap/GC/FID analyses. One of the primary flavor impact compounds in strawberry, 2,5-dimethyl-4-methoxy-3(2H)-furanone was detected by using SPME/GC/TOFMS. SPME appears to be suitable for rapid and quantitative analysis of volatile aroma compounds in tomato and strawberry fruit.
(30) Isolation and quantitation of volatile cocaine chemicals by SPME/GC and the relevance to detector dog alerts to suspected drug money. AU: Norelus_A, Furton_KG, Hsu_YL, Luo_T, Lopez_F, Rose_S NA: FLORIDA INT UNIV,DEPT CHEM,MIAMI,FL,33199 JN: ABSTRACTS OF PAPERS OF THE AMERICAN CHEMICAL SOCIETY, 1998, Vol.216, No.Pt3, pp.27-PRES IS: 0065-7727 DT: Meeting Abstract
(31) Headspace solid-phase microextraction and gas chromatographic determination of dinitroaniline herbicides in human blood, urine and environmental water AU: Guan_FY, Watanabe_K, Ishii_A, Seno_H, Kumazawa_T, Hattori_H, Suzuki_O NA: HAMAMATSU UNIV,SCH MED,DEPT LEGAL MED,3600 HANDA CHO,HAMAMATSU,SHIZUOKA 431319,JAPAN HAMAMATSU UNIV,SCH MED,DEPT LEGAL MED,HAMAMATSU,SHIZUOKA 431319,JAPAN SHOWA UNIV,SCH MED,DEPT LEGAL MED,SHINAGAWA KU,TOKYO 142,JAPAN AICHI MED UNIV,DEPT LEGAL MED,NAGAKUTE,AICHI 48011,JAPAN JN: JOURNAL OF CHROMATOGRAPHY B, 1998, Vol.714, No.2, pp.205-213 IS: 0378-4347 DT: Article AB: Solid-phase microextraction (SPME) is a unique extraction and sampling technique, and it has been used for separation of volatile organics from water or other simple matrices. In this study, we have used SPME to separate dinitroaniline herbicides from complicated matrices of human urine and blood in order to broaden its application to biomedical analysis. The SPME conditions were optimized for water, urine and blood samples, in terms of pH, salt additives, extraction temperature, and fiber exposure time. Urine or water (1.0 ml) spiked with herbicides and 0.28 g of anhydrous sodium sulfate was preheated at 70 degrees C for 10 min, and a polydimethylsiloxane-coated fiber for SPME was exposed to the headspace at 70 degrees C for another 30 min; while spiked blood (0.5 ml) diluted with water (0.5 ml) was treated at 90 degrees C in the same way. The herbicides were extractable under these conditions, and could be determined by gas chromatography-electron capture detector (GC-ECD). The recoveries of the herbicides, measured at the concentrations of 0.50 and 1.0 ng/ml urine or water, or 6.0 and 20 ng/0.5 mi blood, ranged from 35 to 64% for different herbicides from water or urine, and from 3.2 to 7.2% from blood. The headspace SPME yielded clean extracts of dinitroaniline herbicides from urine, blood or water, which could be directly analyzed by GC-ECD without further purification. The peak areas of the extracted herbicides were proportional to their concentrations in the range 0.1-10 ng/ml in water or urine, or 1-60 ng/0.5 ml in blood. The lowest detectable concentration of the herbicides lay in 0.1 ng/ml water or urine, or in 0.5 ng/0.5 ml blood. The intra- and inter-day coefficients of variation were within 14% for most of the analytes. Although the recoveries of the herbicides were rather low, the linearity of calibration curve and the precision were good. The developed method is more sensitive and much simpler in sample preparation than previously reported ones. With the established SPME method, a dosed herbicide was successfully separated and determined in rats' blood.
(32) Analysis of volatile fruit components by headspace solid-phase microextraction AU: Ibanez_E, LopezSebastian_S, Ramos_E, Tabera_J, Reglero_G NA: CSIC,INST FERMENTAC IND,JUAN CIERVA 3,E-28006 MADRID,SPAIN CSIC,INST FERMENTAC IND,E-28006 MADRID,SPAIN JN: FOOD CHEMISTRY, 1998, Vol.63, No.2, pp.281-286 IS: 0308-8146 DT: Article AB: A method based on headspace solid-phase microextraction (HS- SPME) has been developed for the analysis of volatile compounds in fruits. Conditions of sampling have been tuned. Repeatability and recoveries obtained with this method have been determined by using a mixture of typical components of fruit aroma. Several fruits, such as raspberries, strawberries, blackberries, banana and mango, have been analysed by the proposed method. The patterns obtained include compounds typically found in fresh fruits and compounds formed during processing or storage. The results showed the use of the technique for fruit characterization and its potential as a routine method for analyzing changes in key flavour compounds during different fruit processing regimes.
(33) Determination of benzophenone-3 and metabolites in water and human urine by solid-phase microextraction and quadrupole ion trap GC-MS AU: Felix_T, Hall_BJ, Brodbelt_JS NA: UNIV TEXAS,DEPT CHEM & BIOCHEM,AUSTIN,TX,78712 JN: ANALYTICA CHIMICA ACTA, 1998, Vol.371, No.2-3, pp.195-203 IS: 0003-2670 DT: Article AB: In this paper, a novel technique has been developed for the determination of benzophenone-3 and its metabolites in urine using solid-phase microextraction (SPME) combined with gas chromatography-quadrupole ion trap mass spectrometry (GC-MS). Benzophenone-3 is a common ingredient found in sunscreens and other products. Because benzophenone-3 and other sunscreening compounds may be absorbed into the body, methods for monitoring the accumulation, metabolism, and excretion of these compounds need to be developed. Three kinds of SPME fibers were used and compared for this study. Parameters for the detection were examined in an aqueous medium and are listed as follows: equilibrium time, multiple extractions from the same vial vs. different vials, the maximum desorption temperature and time, and the effects of both salt and solvent on the extraction efficiency. Human urine samples were then spiked with standard benzophenone solutions and analyzed with the SPME method to determine linear range, limit of detection, and precision. Linear range determinations fell within 10-1000 ng/ml with precisions averaging 7% RSD. Ultimately a urine specimen taken after a human subject had applied a commercially available sunscreen product was tested for benzophenone and its metabolites. Benzophenone-3 and 2,4-dihydroxybenzophenone were detected and the former was subjected to both SPME and SPE quantitation methods with comparable results of 260 and 200 ng/ml, respectively.
(34) Solid phase micro-extraction (SPME) fibre performance in turbid aqueous samples AU: Rogers_HR, Comber_SDW NA: WRC PLC,HENLEY RD,MARLOW SL7 2HD,BUCKS,ENGLAND JN: CHEMOSPHERE, 1998, Vol.37, No.8, pp.1413-1418 IS: 0045-6535 DT: Article AB: The performance of solid phase microextraction (SPME) fibres was assessed in river water samples containing suspended solids. The effects of repeated immersion and the influence of variable solids loadings were considered for a soluble (phenol) and moderately hydrophobic organic contaminant (1,2- dimethytnaphthalene) For 1,2-dimethylnaphthalene the extractive efficiency of fibres declined progressively with repeated immersion in solutions with high solids levels (1 g l(-1)) and with increased suspended solids concentrations. However, for phenol there was no decrease in extractive efficiency with increased solids concentrations. Results suggest that SPME efficiency is not likely to be significantly reduced in typical natural waters, or effluent samples with solids concentrations concentrations <1 g l(-1).
(35) SPME method development for headspace analysis of volatile flavor compounds. AU: Roberts_DD, Pollien_P NA: NESTLE RES CTR,CH-1000 LAUSANNE 26,SWITZERLAND JN: ABSTRACTS OF PAPERS OF THE AMERICAN CHEMICAL SOCIETY, 1998, Vol.216, No.Pt1, pp.146-AGFD IS: 0065-7727 DT: Meeting Abstract
(36) Optimization of solid-phase microextraction followed by high performance liquid chromatography(SPME/HPLC) for analysis of explosives. AU: Wu_LM, Furton_KG NA: FLORIDA INT UNIV,DEPT CHEM,MIAMI,FL,33199 FLORIDA INT UNIV,INT FORENS RES INST,MIAMI,FL,33199 JN: ABSTRACTS OF PAPERS OF THE AMERICAN CHEMICAL SOCIETY, 1998, Vol.216, No.Pt1, pp.84-ANYL IS: 0065-7727 DT: Meeting Abstract
(37) Source identification of underground fuel spills by SPME and chemometrics. AU: Moores_A, Ritter_J, Lavine_B NA: CLARKSON UNIV,DEPT CHEM,POTSDAM,NY,13699 JN: ABSTRACTS OF PAPERS OF THE AMERICAN CHEMICAL SOCIETY, 1998, Vol.216, No.Pt1, pp.128-ANYL IS: 0065-7727 DT: Meeting Abstract
(38) Solid-phase microextraction and its utilization in environmental analysis LA: Czech AU: Sedlakova_J, Matisova_E, Slezackova_M NA: SLOVAK TECH UNIV,FAC CHEM TECHNOL,KATEDRA ANALYT CHEM,RADLINSKEHO 9,BRATISLAVA 81237,SLOVAKIA JN: CHEMICKE LISTY, 1998, Vol.92, No.8, pp.633-642 IS: 0009-2770 DT: Review AB: The solid-phase microextraction (SPME) is a new method for the extraction of organic compounds from environmental samples which eliminates the use of solvents. Stationary phases coating fused silica fibre are used to extract the analytes from the sample. After extraction the sorbed substances are introduced into the GC system, where they are thermally desorbed and analyzed. The SPME methods are classified according to the physical-chemical principle as direct methods and headspace methods. The review deals mainly with the utilization of SPME for the preconcentration of organic pollutants from environmental matrices giving 100 references
(39) Analysis of wine bouquet components using headspace solid-phase microextraction capillary gas chromatography AU: Garcia_DDLC, Reichenbaher_M, Denzer_K, Hurlbeck_C, Bartzsch_C, Feller_KH NA: UNIV JENA,INST ANORGAN & ANALYT CHEM,LESSINGSTR 8,D-07743 JENA,GERMANY UNIV JENA,INST ANORGAN & ANALYT CHEM,D-07743 JENA,GERMANY FACHHSCH JENA,FACHBEREICH MED TECH,JENA,GERMANY JN: HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY, 1998, Vol.21, No.7, pp.373-377 IS: 0935-6304 DT: Article AB: Headspace solid-phase microextraction (HS/SPME) was studied and optimized for the capillary gas chromatographic (CGC) analysis of wine aroma compounds, The results were compared with those obtained using the direct sampling mode (DI/SPME) and using liquid/liquid extraction with Kaltron. The aromatic patterns obtained by HS/SPME-CGC were applied to the chemometric classification of wine varieties. The HS/SPME-CGC standard additional method is an appropriate technique for the quantitative analysis of volatile wine aroma compounds.
(40) Solid-phase microextraction for determining the binding state of organic pollutants in contaminated water rich in humic organic matter AU: Porschmann_J, Kopinke_FD, Pawliszyn_J NA: ENVIRONM RES CTR,PERMOSERSTR 15,D-04318 LEIPZIG,GERMANY UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.816, No.2, pp.159-167 IS: 0021-9673 DT: Article AB: Solid-phase microextraction (SPME) in both conventional and headspace mode was used for determining the freely available and reversibly bound fraction of phenols and polycyclic aromatic hydrocarbons in contaminated water rich in dissolved polymeric organic matter (DOM). The SPME results obtained by using internal calibration with deuterated surrogates gave the total analyte concentration based on the identical partitioning behaviour of both, native pollutants and deuterated spikes, and agreed well with data from exhaustive LLE. Data obtained with direct and headspace SPME are very similar. Investigated matrices include both contaminated water and artificial DOM solutions. The DOM compounds were isolated from different aquatic and terrestrial sources and cover a wide range of hydrophobicity. A new approach based on progressive dilution of samples rich in DOM was developed for determining both the freely-dissolved fraction of an unknown analyte and its partition coefficients. Theoretical considerations provide strong evidence that the commonly used term 'concentration' in SPME analysis should be replaced by the more appropriate term 'activity' of the solute.
(41) Sampling techniques for gas chromatographic mass spectrometric analysis of long-chain free fatty acids from insect exocrine glands AU: Maile_R, Dani_FR, Jones_GR, Morgan_ED, Ortius_D NA: UNIV KEELE,DEPT CHEM,KEELE ST5 5BG,STAFFS,ENGLAND AARHUS UNIV,DEPT ECOL & GENET,DK-8000 AARHUS C,DENMARK JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.816, No.2, pp.169-175 IS: 0021-9673 DT: Article AB: Many features of gas chromatographic equipment can hinder the detection of free carboxylic acids, so that these polar and reactive substances do not lend themselves well to gas chromatography through adsorption and peak tailing. Therefore the normal practice is the derivatization to esters. The analysis of small quantities of insect exocrine secretions using this method is not quantitative. Factors affecting the quantitative analysis of free fatty acids have been explored. Two sampling methods, either by solid-phase micro-extraction (SPME) or the solid injector technique we developed and traditionally used, were found to be reliable if particular precautions are observed. These are the use of deactivated injection liners and glass wool in the injector. Deactivated pre- and post-columns prevent the detection of long-chain fatty acids even if the latter are present in mu g amounts. By avoiding preheating of the samples in the injector and removing the glass powder of the sample capillaries after each injection, enhanced results have been observed with the Keele injector. For the SPME, absorption from headspace and moderate sample heating temperatures showed better results compared with high-temperature sample heating. (C) 1998 Elsevier Science B.V. All rights reserved.
(42) Tiime since discharge of shotguns AU: Andrasko_J, Norberg_T, Stahling_S NA: NATL LAB FORENS LAB,SKL,S-58194 LINKOPING,SWEDEN JN: JOURNAL OF FORENSIC SCIENCES, 1998, Vol.43, No.5, pp.1005-1015 IS: 0022-1198 DT: Article AB: A method for estimation of the time since the latest discharge of a shotgun is presented. This method is based on SPME (Solid Phase Micro-Extraction) sampling from the atmosphere inside the shotgun barrel. Two analytical systems were used in parallel, the GC/TEA and GC/FID(MS) system. These two systems detect various combustion products and the estimation of time since the latest discharge is based on the rate of escape of the volatile discharge residues from the barrel as a function of time. If the ammunition used in the suspect firearm is known, the use of decay curves for the actual firearm and the actual ammunition is fairly straightforward. For unknown ammunition, repetitive samplings must be performed and the results fitted to decay curves obtained for other ammunition types according to the proposed procedure. Generally, the method presented in this study can give an indication whether a weapon was fired, e.g., 2 to 3 days, 1 to 2 weeks, or more than 3 weeks ago. Some factors that may impact data interpretation were studied, such as the effect of cleaning the barrel, the number of shots fired, the eventual disturbance to the system by SPME sampling and the effect of temperature of the storage. WA: forensic science, firearms, time since discharge, SPME, gas chromatography (GC), GC-TEA, firearm discharge residues
(43) Microcolumn liquid chromatography coupled with solid phase micro extraction (SPME/micro-LC) for the analysis of benzodiazepines in human urine AU: Jinno_K, Taniguchi_M, Sawada_H, Hayashida_M NA: TOYOHASHI UNIV TECHNOL,SCH MAT SCI,TOYOHASHI,AICHI 4418580,JAPAN NIPPON MED COLL,DEPT LEGAL MED,TOKYO 1130022,JAPAN JN: ANALUSIS, 1998, Vol.26, No.5, pp.M27-M30 IS: 0365-4877 DT: Article AB: The interface technique between SPME and micro-LC has been evaluated for benzodiazepines analysis in human urine, Three SPME fiber coatings such as polyacrylate (PA), carbowax/template (CW/TEP) and sol-gel C-11 polydimethylsiloxane (PDMS) were compared in the performance for SPME process such as extraction efficiency, extraction time and total analysis time required. As the results using the CW/TEP fiber for SPME and 1.0 mm i.d, LC column as the separation medium the analysis of benzodiazepines in patient's urine can be performed in 2 hours with very low solvent consumption less than 1.5 mL solvents in whole analytical procedures.
(44) Biogenesis of Geranium oil compounds: On the origin of oxygen in cis-/trans-rose oxide AU: Wust_M, Beck_T, Mosandl_A NA: UNIV FRANKFURT,INST LEBENSMITTELCHEM,BIOZENTRUM,MARIE CURIE STR 9,D-60439 FRANKFURT,GERMANY UNIV FRANKFURT,INST LEBENSMITTELCHEM,BIOZENTRUM,D-60439 FRANKFURT,GERMANY JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, Vol.46, No.8, pp.3225-3229 IS: 0021-8561 DT: Article AB: By feeding experiments with labeled [1,1-H-2(2), O- 18]citronellol, it could be shown that Pelargonium graveolens is able to convert the fed precursor into cis-/trans-rose oxide. The labeling pattern and diastereomeric ratio of the resulting cis-/trans-rose oxides are in agreement with a mechanism which includes the enzymatic oxidation of citronellol in the allylic position and subsequent cyclization of the resulting diol to cis-/trans-rose oxide with retention of the oxygen of [1,1-H-2(2),O-18]citronellol.
(45) Biological degradation of diesel fuel in water and soil monitored with solid-phase micro-extraction and GC-MS AU: Eriksson_M, Swartling_A, Dalhammar_G NA: ROYAL INST TECHNOL,KTH,DEPT BIOCHEM & BIOTECHNOL,S-10044 STOCKHOLM,SWEDEN ROYAL INST TECHNOL,KTH,DEPT CHEM,S-10044 STOCKHOLM,SWEDEN JN: APPLIED MICROBIOLOGY AND BIOTECHNOLOGY, 1998, Vol.50, No.1, pp.129-134 IS: 0175-7598 DT: Article AB: Solid-phase micro-extraction (SPME) was used for monitoring degradation of hydrocarbons in diesel-fuel-contaminated (1% v/v) water and soil. Natural soil bacteria with and without external addition of inoculum were used. Directly after a 10-s exposure of the sample, the polydimethylsiloxane fibre was injected into the GC-MS. This method strongly reduced the time of analysis compared to a conventional liquid/liquid extraction. A comparison of SPME and pentane extraction of diesel oil was made and found to be consistent. The degradation of diesel fuel in water was monitored for 10 weeks using SPME. After 5 weeks all hydrocarbons were degraded except for the decahydronaphthalenes. These compounds were approximately 3% of the total hydrocarbons in the diesel oil used and remained undegraded throughout the study although none of the chemical or physical parameters was limiting. In the soil study the degradation of diesel fuel in normal soil was completed after 3 weeks, when the only remaining substances were decahydronaphthalenes. All samples were compared to sterile references to make up for evaporation losses. SPME proved to be a fast and reliable method to monitor changes in concentrations of semivolatile organic compounds.
(46) Methods for determining the vapour pressure of active ingredients used in crop protection. Part V: Thermogravimetry combined with Solid Phase MicroExtraction (SPME) AU: Krohl_T, Kastel_R, Konig_W, Ziegler_H, Kohle_H, Parg_A NA: BASF AG,CROP PROTECT PROD DEV,D-67114 LIMBURGERHOF,GERMANY JN: PESTICIDE SCIENCE, 1998, Vol.53, No.4, pp.300-310 IS: 0031-613X DT: Article AB: The well-established evaporation rate method for determining the vapour pressure of active ingredients in crop protection down to the order of 10(-12) mbar can be supplemented by the new sample preparation technique of Solid Phase MicroExtraction (SPME). With this technique, it is possible to identify evaporating substances by analysis after partitioning into the polymer coating of a thin fibre in the outlet-gas flow of thermogravimetric equipment. The active ingredients fenpropimorph, kresoxim-methyl, metolachlor, clomazone and (Z)-9-dodecenyl acetate were used in this study, which showed that, despite the relatively small amount of collected material, an analytical identification of the evaporating compound by SPME/GC can be successfully achieved. In particular, the experiments have demonstrated a clear correlation between the linearity of the weight loss curve and the evaporation process of a pure compound. In the case of organic compounds that are unstable to heat, the SPME method can also be utilized to show whether, and at what temperatures, decomposition of the sample into fragments of higher volatility occurs. For example, the insecticide dimethoate showed a clear temperature dependence of both evaporation behaviour and in the SPME/GC analysis.
(47) Simple method for estimating polychlorinated biphenyl concentrations on soils and sediments using subcritical water extraction coupled with solid-phase microextraction AU: Hawthorne_SB, Grabanski_CB, Hageman_KJ, Miller_DJ NA: UNIV N DAKOTA,ENERGY & ENVIRONM RES CTR,POB 9018,GRAND FORKS,ND,58202 JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.814, No.1-2, pp.151-160 IS: 0021-9673 DT: Article AB: A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a sealed extraction cell, heated at 250 degrees C for 15 to 60 min, cooled, and the PCB concentrations in the extractant water determined by SPME and GC-electron- capture detection. When PCB 103 and 169 (not found in contaminated samples) are used as internal standards ro calibrate for the soil/water and water/SPME equilibria, quantitative results for individual PCB congeners typically agree within 80 to 130% of the concentrations based on Soxhlet extraction and conventional GC analysis. The reproducibility of replicate subcritical water extraction/SPME determinations is typically 10 to 15% relative standard deviation. Analysts of water extracts stored for 24 h agrees with fresh extracts, demonstrating that extracts can be stored for later SPME analysis without significant loss of the PCBs from the extractant water. The method is simple to perform, uses held- rugged and inexpensive apparatus, and generates no organic solvent waste.
(48) Determination of methylmercury in fish and aqueous samples using solid-phase microextraction followed by gas chromatography atomic fluorescence spectrometry AU: Cai_Y, Monsalud_S, Furton_KG, Jaffe_R, Jones_RD NA: FLORIDA INT UNIV,DEPT CHEM,UNIV PK,MIAMI,FL,33199 FLORIDA INT UNIV,SE ENVIRONM RES PROGRAM,MIAMI,FL,33199 FLORIDA INT UNIV,DEPT BIOL SCI,MIAMI,FL,33199 JN: APPLIED ORGANOMETALLIC CHEMISTRY, 1998, Vol.12, No.8-9, pp.565- 569 IS: 0268-2605 DT: Article AB: An analytical method is described for methylmercury determination in fish and aqueous samples using solid-phase microextraction (SPME) followed by gas chromatography-atomic fluorescence spectrometry (GC-AFS). The procedure involves aqueous-phase derivatization of methylmercury species with sodium tetraethylborate in a sample vial and subsequent extraction with a silica fiber coated with poly(dimethylsiloxane). The mercury derivatives are desorbed in the splitless injection port of a gas chromatograph and subsequently analyzed by GC-AFS, The headspace SPME procedure is used and parameters affecting the extraction, adsorption and desorption are evaluated, Results for methylmercury analysis in standard reference material (DORM-2) and fish samples are presented.
(49) Identification of volatile compounds in sunflower oil by headspace SPME and ion-trap GC/MS AU: Keszler_A, Heberger_K, Gude_M NA: HUNGARIAN ACAD SCI,CENT RES INST CHEM,POB 17,H-1525 BUDAPEST,HUNGARY UNILEVER RES LABS VLAARDINGEN,NL-3130 AC VLAARDINGEN,NETHERLANDS JN: HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY, 1998, Vol.21, No.6, pp.368-370 IS: 0935-6304
(50) Determination of persistent organochlorine compounds in blood by solid phase micro extraction and GC-ECD AU: Rohrig_L, Puttmann_M, Meisch_HU NA: UNIV SAARLAND,ZENTRUM UMWELTFORSCH,D-66125 SAARBRUCKEN,GERMANY LABOR DR LATZA & PARTNER,D-66386 ST INGBERT,GERMANY JN: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY, 1998, Vol.361, No.2, pp.192-196 IS: 0937-0633 DT: Article AB: Biomonitoring of persistent organochlorine compounds in blood using the solid phase microextraction technique (SPME) and gas chromatography with electron capture detection (GC-ECD) is described. Polar substances as tri-, tetra- and penta- chlorophenols are analyzed simultaneously with less polar compounds such as hexachlorobenzene (HCB), alpha-, beta-, and gamma-hexachlorocyclohexane (HCH), dichlorodiphenyltrichloroethane (DDT) and its derivatives and with some important congeners of the polychlorinated biphenyls (PCB). No derivatization is needed for the determination of the phenolic compounds. The results show a good reproducibility down to the lower mu g/L-region. The method is very fast and of low cost compared to the classic extraction and determination procedures.
(51) Optimization of solid-phase microextraction analysis for headspace flavor compounds of orange juice AU: Jia_MY, Zhang_QH, Min_DB NA: OHIO STATE UNIV,DEPT FOOD SCI & TECHNOL,2121 FYFFE RD,COLUMBUS,OH,43210 OHIO STATE UNIV,DEPT FOOD SCI & TECHNOL,COLUMBUS,OH,43210 JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, Vol.46, No.7, pp.2744-2747 IS: 0021-8561 DT: Article AB: The headspace flavor compounds of orange juice were isolated by solid-phase microextraction (SPME) fiber coated with 100 mu m of poly(dimethylsiloxane) and separated by gas chromatography. The effects of the orange juice temperature from 25 to 80 degrees C and the adsorption time from 5 to 40 min an the equilibrium of flavor compounds between the SPME coating and the orange juice indicated that the equilibrium time decreased as the sample temperature increased. The equilibrium of the flavor compounds between the SPME coating and the orange juice required 30 min at 40 degrees C or 20 min at 60 degrees C. The amount of orange flavor compounds adsorbed by SPME coating decreased as the orange juice temperature increased from 25 to 80 degrees C. The resolution of the gas chromatogram increased as the inside diameter of the injection port liner decreased from 1 to 0.75 mm. The concentrations of ethyl butyrate, octanal, decanal, alpha-pinene, and limonene in orange juice were 0.4, 1.1, 1.0, 1.4, and 254 ppm, respectively. The coefficients of variation for the analyses of ethyl butyrate, octanal, decanal, alpha-pinene, and limonene ranged from 4.4% for 0.4 ppm ethyl butyrate to 1.6% for 254 ppm Limonene.
(52) Headspace analysis in chemical ecology: Effects of different sampling methods on ratios of volatile compounds present in headspace samples AU: Agelopoulos_NG, Pickett_JA NA: IACR ROTHAMSTED,BIOL & ECOL CHEM DEPT,HARPENDEN AL5 2JQ,HERTS,ENGLAND JN: JOURNAL OF CHEMICAL ECOLOGY, 1998, Vol.24, No.7, pp.1161-1172 IS: 0098-0331 DT: Article AB: The effects that different headspace sampling methods have on the analysis of the ratios of compounds present in the headspace of a synthetic mixture and a biological sample were evaluated using the following methods: solid-phase microextraction (SPME), a syringe, and the porous polymers Porapak Q, Tenax TA, and Hayesep Q (thermal and solvent desorption). The performance of each method was only evaluated for a certain sampling period and under given experimental conditions. The test mixture comprised pentan-3-ol, 4-penten-1- ol, (E)-2-hexenal, hexan-1-ol, heptanal, (1S,SS)-(-)-alpha- pinene, 6-methyl-5-hepten-2-one, hexyl acetate, (R)-(+)- limonene, and undecane. SPME gave significantly different ratios of pentan-3-ol, 4-penten-1-, hexan-1-ol, heptanal, (1S,5S)-(-)-alpha-pinene, 6-methyl-5-hepten-2-one, hexyl acetate, limonene, and undecane compared with the other methods. No significant differences were observed between the syringe and the porous polymers or between the three different porous polymers used. The method of release of the trapped analytes from the polymers, thermal or solvent desorption, did not affect the ratios of compounds. The effects that different sampling methods have on the ratios of compounds present in the headspace of a biological sample, ripe banana, were evaluated. The headspace was sampled using SPME and the porous polymers Porapak Q and Tenax TA (Thermal desorption). The following compounds were identified in the headspace of ripe bananas: 2- methylbutyl acetate, pentyl acetate, 2-methylbutyl propanoate, butyl butanoate, and pentyl butanoate. SPME gave significantly different ratios of 2-methylbutyl acetate, pentyl acetate, butyl butanoate, and pentyl butanoate when compared to Porapak Q and Tenax TA. No significant differences on the ratios of compounds present in the headspace of ripe banana were observed when the two polymers were compared. The use of different sampling methods in headspace analysis of biological samples is discussed.
(53) Determination of free fatty acids and lactones in cheese by solid phase microextraction (SPME) AU: Wijesundera_C, Drury_L, Walsh_T NA: FOOD SCI AUSTRALIA,GRAHAM RD,HIGHETT,VIC 3190,AUSTRALIA JN: AUSTRALIAN JOURNAL OF DAIRY TECHNOLOGY, 1998, Vol.53, No.2, p.140 IS: 0004-9433 DT: Article
(54) Trace analysis of explosives in seawater using solid-phase microextraction and gas chromatography ion trap mass spectrometry AU: Barshick_SA, Griest_WH NA: OAK RIDGE NATL LAB,OAK RIDGE,TN,37831 JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.14, pp.3015-3020 IS: 0003-2700 DT: Article AB: Complex matrixes typically cannot be analyzed directly to obtain the selectivity and sensitivity required for most trace analysis applications. To circumvent this problem, solid-phase microextraction (SPME) techniques were used to preconcentrate analytes selectively prior to gas chromatographic/ion trap mass spectrometric analysis. This approach was applied to the trace analysis of explosives and their metabolites in seawater. The choice of SPME sorbent phase was shown to be important especially for the amino metabolites of trinitrotoluene (TNT) and RDX, which were extracted better on polar phases. Although equilibration times were quite lengthy, on the order of 30 min or greater, a sampling time of only 10 min was shown to be sufficient for achieving low part-per-billion (ppb) to part- per-trillion (ppt) detection limits for TNT and the amino metabolites in real seawater samples. While SPME was ideal for rapid screening of explosives in seawater samples, methods for improving the reproducibility and accuracy of quantification are still being investigated.
(55) Determination of fresh onion (Allium cepa L.) volatiles by solid phase microextraction combined with gas chromatography mass spectrometry AU: Jarvenpaa_EP, Zhang_ZY, Huopalahti_R, King_JW NA: TURKU UNIV,DEPT BIOCHEM & FOOD CHEM,FIN-20014 TURKU,FINLAND ARS,NATL CTR AGR UTILIZAT RES,USDA,PEORIA,IL,61604 JN: ZEITSCHRIFT FUR LEBENSMITTEL-UNTERSUCHUNG UND-FORSCHUNG A-FOOD RESEARCH AND TECHNOLOGY, 1998, Vol.207, No.1, pp.39-43 IS: 1431-4630 DT: Article AB: Solid-phase microextraction (SPME) was used for the extraction of the volatiles of yellow onions (Allium cepa L.), where the primary volatiles are produced enzymatically after rupture of the plant cells. The SPME-GC analysis of successive samples at timed intervals provided information comparable with that obtained previously by headspace techniques; however, SPME was more convenient and faster to perform. Moreover, the SPME-GC-MS system employed permit ted easy monitoring of the fast changes in the volatile composition. Because ambient temperatures were used in the analysis, the method described should produce only minor artefacts during the absorption and desorption steps of SPME, The most important compound found in the headspace of sliced onions by SPME-GC-MS after 1 min emission of volatiles was thiopropanal S-oxide. Also, some dipropenyl disulphides and propenyl propyl disulphides were identified. After 30 min, most of the thiopropanal-S-oxide disappeared, and other sulphur and non-sulphur compounds appeared in the GC chromatograms. The major constituents were diprop(en)yl disulphides. Similar constituents were also found in the water-slurred onions by headspace and di rect SPME.
(56) Analysis of selected gaseous organic micro-pollutants in air by means of solid phase microextraction gas chromatography mass spectrometry, calibration problems AU: Namiesnik_J, Gorlo_D, Wolska_L, Zygmunt_B NA: GDANSK TECH UNIV,FAC CHEM,DEPT ANALYT CHEM,PL-80956 GDANSK,POLAND JN: ANALUSIS, 1998, Vol.26, No.4, pp.170-174 IS: 0365-4877 DT: Article AB: In this work, problems related to calibration of solid phase microextraction (SPME) device were described. The effects of humidity and temperature on organic pollutants sampling from gaseous matrices on a 100 mu m FDMS coated SPME fiber were studied. Standard gaseous mixtures used in these studies were generated by the permeation method and humidified to known levels of relative humidity. The SPME-GC-MS based procedure was used to determine organic vapours (carbon tetrachloride, toluene, chlorobenzene, p-xylene and n-decane) in a laboratory air
(57) Solid phase microextraction (SPME) of the herbicide atrazine in aqueous soil suspensions AU: Tugulea_AM, Sarna_LP, Webster_GRB NA: UNIV MANITOBA,DEPT SOIL SCI,WINNIPEG,MB R3T 2N2,CANADA JN: INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY, 1997, Vol.68, No.2, pp.137-153 IS: 0306-7319 DT: Article AB: A new method for the direct SPME of atrazine in soil slurries (20 g soil/L) followed by cleaning of the fibre has been developed enabling sequential extraction of at least 15 soil samples with good reproducibility. No relevant interferences were observed using an EC detector at the lowest atrazine concentration examined (<10(-7) mol/L). Good resolution was obtained and the method was linear over the range of concentrations studied (<10(-7)-10(-4) mol/L). Data from the SPME-GC method correlate very well with the data from microfiltration-HPLC measurements, suggesting that by both methods the freely dissolved atrazine alone is being measured. Thus a new simple, clean, solventless extraction technique, easily compatible with capillary GC, has been added to the arsenal of methods available for the analysis of less volatile compounds from soils and water bodies with a high content of particulate and humic materials.
(58) Rapid analysis of geosmin and 2-methylisoborneol in water using solid phase micro extraction procedures AU: Lloyd_SW, Lea_JM, Zimba_PV, Grimm_CC NA: ARS,USDA,SRRC,1100 ROBERT E LEE BLVD,NEW ORLEANS,LA,70124 JN: WATER RESEARCH, 1998, Vol.32, No.7, pp.2140-2146 IS: 0043-1354 DT: Article AB: Geosmin (GSM) and 2-methylisoborneol (MIB) are algae metabolites with muddy/musty odors which contaminate water supplies and can be absorbed by aquatic organisms. Humans can perceive them in water and aquatic food products at ng/l (parts per trillion) concentrations. A rapid method employing solid phase micro extraction (SPME) has been developed for the analysis of GSM and MIB in water. Routine quantification at mu g/l concentrations can be accomplished using gas chromatography and flame ionization detection (FID) on a 6 ml aqueous sample with a total analysis time of less than 15 min. Concentration levels of MIB and GSM at 10 ng/l (parts per trillion) can be detected under optimal conditions employing GC/MS in selected ion monitoring mode. Standard solutions and water samples from MIB producing algae cultures were used to compare SPME against purge and trap (P&T) using both flame ionization and mass spectrometric detection. Results obtained from SPME and PET were similar in terms of reproducibility and sensitivity. This paper reports a simple, rapid method for monitoring the algal production of MIB and GSM at the mu g/l range which can be extended to the drinking water levels at the ng/l range of concentrations.
(59) Solid phase microextraction and headspace solid phase microextraction for the determination of polychlorinated biphenyls in water samples AU: Llompart_M, Li_K, Fingas_M NA: UNIV SANTIAGO DE COMPOSTELA,FAC QUIM,DEPT QUIM ANALIT NUTR & BROMATOL,E-15706 SANTIAGO COMPOSTE,SPAIN ENVIRONM TECHNOL CTR,ENVIRONM CANADA,EMERGENCIES SCI DIV,OTTAWA,ON,CANADA JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.13, pp.2510-2515 IS: 0003-2700 DT: Article AB: A solid-phase microextraction (SPME) method has been developed for the quantification of polychlorinated biphenyls (PCBs) in water samples. Parameters such as sampling time, volume of water, volume of headspace, temperature, addition of salts, and agitation of the sample were studied. Because the time for reaching equilibrium between phases takes several hours or days, depending on the experimental conditions, it was necessary to work in nonequilibrium conditions to keep the sample analysis to a reasonable time. The possibility of sampling the headspace over the water sample (HSSPME), instead of immersing the fiber into the water (SPME), was also investigated, and despite the low partition of PCB into the headspace, HSSPME offered higher sensitivity than SPME at 100 degrees C, The adsorption kinetics for SPME at room temperature, SPME at 100 degrees C, and HSSPME at 100 degrees C were investigated and compared. The proposed HSSPME method exhibits excellent linearity and sensitivity. The detection limit was in the sub-ng/L level. This method has been applied to a real industrial harbor water and compared with liquid- liquid extraction. Both techniques offered similar results, but HSSPME was much more sensitive and considerably faster, by eliminating all the manual process intensive sample workup, and reduces solvent consumption entirely. The only drawback was that matrix effects were observed, but with the addition of deuterated surrogates to the sample or the use of a standard addition calibration, accurate quantification can be achieved.
(60) Determination of carbonyl compounds in water by derivatization - solid-phase microextraction and gas chromatographic analysis AU: Bao_ML, Pantani_F, Griffini_O, Burrini_D, Santianni_D, Barbieri_K NA: WATER SUPPLY FLORENCE,VIA VILLAMAGNA 39,I-50126 FLORENCE,ITALY WATER SUPPLY FLORENCE,I-50126 FLORENCE,ITALY UNIV FLORENCE,DEPT PUBL HLTH EPIDEMIOL & ENVIRONM ANALYT CHEM,I-50121 FLORENCE,ITALY JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.809, No.1-2, pp.75-87 IS: 0021-9673 DT: Article AB: The solid-phase microextraction (SPME) technique was evaluated for the determination of 23 carbonyl compounds in water. The carbonyl compounds in water were derivatized with o-(2,3.4,5,6- pentafluorobenzyl)-hydroxylamine hydrochloride (PFBHA), extracted with SPME from liquid or headspace and analyzed by GC with electron capture detection (GC-ECD). The effects of agitation techniques and the addition of salt (NaCl) on extraction, the absorption-time and absorption-concentration profiles were examined. The precision of the SPME technique for the determination of carbonyl compounds was evaluated with spiked bidistilled water, ozonated drinking water, and rain water. The relative standard deviations obtained from different spiked water matrix were similar, and in the range of 5.7- 21.1%. The precision can be further improved by using an internal standard. With 4 ml of water sample, the limits of detection for most of the tested carbonyl compounds using liquid or headspace SPME-GC-ECD were similar and in the range of 0.006-0.2 mu g/l, except for glyoxal and methylglyoxal, which showed low sensitivity when using headspace SPME. In the analysis of an ozonated drinking water sample, the SPME techniques gave comparable results to those of the conventional liquid-liquid extraction method.
(61) Pattern recognition of Swiss cheese aroma compounds by SPME/GC and an electronic nose AU: Jou_KD, Harper_WJ NA: OHIO STATE UNIV,DEPT FOOD SCI & TECHNOL,2121 FYFFE RD,COLUMBUS,OH,43210 JN: MILCHWISSENSCHAFT-MILK SCIENCE INTERNATIONAL, 1998, Vol.53, No.5, pp.259-263 IS: 0026-3788 DT: Article AB: Analysis of Swiss cheese flavor by electronic nose and Solid Phase Micro Extraction (SPME/GC) was conducted. Distinct GC chromatographic patterns for 5 selected Swiss cheeses were observed. Differentiation of Swiss cheeses by an electronic nose and GC predominant peaks could be related to flavor characteristics of the cheeses. The predominant volatile compounds in cheeses strongly affect the nose discriminant plot. An optimum Artificial Neural Network (ANN) successfully performed pattern recognition and closeness of cheeses was tested. Overall results suggest that ANN associated with GC patterns and nose discriminant plot provided an objective way for judging cheese flavor.
(62) Design of an automated analysis system for the determination of organic compounds in continuous air stream using solid-phase microextraction AU: Eisert_R, Pawliszyn_J, Barinshteyn_G, Chambers_D NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA 3M CANADA CO,LONDON,ON N6A 4T1,CANADA JN: ANALYTICAL COMMUNICATIONS, 1998, Vol.35, No.6, pp.187-189 IS: 1359-7337 DT: Article AB: An automated solid-phase microextraction (SPME) unit coupled to gas chromatography was used to determine organic compounds in air. The target analyte was released from microcapsules into the air at ambient temperature. A fully automated system was designed to facilitate the monitoring of the organic analytes in the continuous air stream. A thin layer of the capsules was prepared by spraying an aqueous solution containing the microcapsules on one side of a glass slide. The slide was exposed to an air stream, which served as a carrier for the analyte vapors. The exposed air was passed through a flow- through cell that was mounted on the autosampler carousel, The SPME assembly, which was fitted with poly(dimethylsiloxane) fiber, was controlled by standard autosampler software. In the dynamic measurement mode, the fiber was inserted in the cell and the analytes partitoned onto the coating. The performance of the sampling device was characterized with respect to mass loading on the fiber, linearity, exposure time and precision. The primary objective of the study was to characterize the release of the pheromone Gossyplure [(Z)-7-(Z8)-11- hexadecadien-1-ol acetate] from microcapsules, The precision of the SPME method was, in general, less than 7% RSD using 18 repetitive extractions. The method was found to be linear over at least three orders of magnitude. The sampling interval was typically 30 min.
(63) Headspace solid-phase microextraction analysis of volatile sulphides and disulphides in wine aroma AU: Mestres_M, Busto_O, Gausch_J NA: UNIV ROVIRA & VIRGILI,ESCOLA ENOL TARRAGONA,DEPT QUIM ANALIT & QUIM ORGAN,UNITAT ENOL,CERTA,E-43005 TARRAGONA,SPAIN JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.808, No.1-2, pp.211-218 IS: 0021-9673 DT: Article AB: Sulphur compounds (S-compounds) are important constituents of wine off-flavours. Headspace solid-phase microextraction (HS- SPME) combined with gas chromatography coupled to flame photometric detection (GC-FPD) was used to develop a suitable method to analyse volatile sulphides and disulphides. This is a very simple and fast technique which gives good reproducibility at mu g/l levels (relative standard deviations<10%). The analytes were extracted from the headspace of the samples by using either polydimethylsiloxane or polyacrylate coated fused- silica fibers in an SPME unit. Then, the fiber was inserted into the injector of a gas chromatograph and the extracted S- compounds were thermally desorbed. The influence of different parameters, such as ionic strength, stirring, headspace volume, ethanol concentration, time and temperature of extraction, was studied. The extraction of the fibers varies considerably for the different sulphur compounds studied. The most volatile compounds were the least extracted by the coating fibers tested. The standard additions technique, applied to real samples, gave the recoveries >94%. The detection limits range between 3 mu g/l and 50 ng/l. The overall process was successfully applied to identify and quantify S-compounds in white and red wines. (C) 1998 Elsevier Science B.V. All rights reserved.
(64) Solid-phase microextraction for quantitative analysis of organophosphorus pesticides in environmental water samples AU: Beltran_J, Lopez_FJ, Cepria_O, Hernandez_F NA: UNIV JAUME 1,EXPT SCI DEPT,POB 224,E-12080 CASTELLO DE PLANA,SPAIN JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.808, No.1-2, pp.257-263 IS: 0021-9673 DT: Article AB: Solid-phase microextraction (SPME) is a relatively new technique that appears as a convenient and efficient extraction method in contrast with more complex techniques used for pesticide residue analysis based on liquid-liquid and solid- phase extraction. This extraction procedure involves the absorption of analytes into a polymeric film coated onto a fine silica fiber directly dipped in the aqueous sample. An SPME procedure for the determination of 12 organophosphorus pesticides in clean environmental water samples at low ng/ml concentration level has been developed by optimising variables involved in extraction and desorption. The absorption equilibrium has been estimated by mathematical treatment of the process using an expression that describes experimental absorption time profiles. The method was evaluated according to the reproducibility, linearity range and limits of detection using two different fiber coatings: 100 mu m polydimethylsiloxane and 85 mu m polyacrylate. The limits of detection obtained using nitrogen-phosphorus detection ranged between 0.01 and 0.2 ng/ml with relative standard deviations lower than 15% at the 1 ng/ml level. The method showed good linearity between 0.1 and 10 ng/ml with regression coefficients ranging between 0.97 and 0.999. Determination df organophosphorus pesticides in water samples in concentration below 0.1 ng/ml can be easily carried out with this fist, economic and solvent-free SPME procedure. (
(65) Simple analysis of local anaesthetics in human blood using headspace solid-phase microextraction and gas chromatography mass spectrometry electron impact ionization selected ion monitoring AU: Watanabe_T, Namera_A, Yashiki_M, Iwasaki_Y, Kojima_T NA: HIROSHIMA UNIV,SCH MED,DEPT LEGAL MED,MINAMI KU,1-2-3 KASUMI,HIROSHIMA 7348551,JAPAN JN: JOURNAL OF CHROMATOGRAPHY B, 1998, Vol.709, No.2, pp.225-232 IS: 0378-4347 DT: Article AB: A simple method for analysis of five local anaesthetics in blood was developed using headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry-electron impact ionization selected ion monitoring (GC-MS-EI-SLM). Deuterated lidocaine (d(10)-lidocaine) was synthesized and used as a desirable internal standard (I.S.). A vial containing a blood sample, 5 M sodium hydroxide and d(10)-lidocaine (LS.) was heated at 120 degrees C. The extraction fiber of the SPME system was exposed for 45 min in the headspace of the vial. The compounds adsorbed on the fiber were desorbed by exposing the fiber in the injection port of a GC-MS system. The calibration curves showed linearity in the range of 0.1-20 mu g/g for lidocaine and mepivacaine, 0.5-20 mu g/g for bupivacaine and 1- 20 mu g/g for prilocaine in blood. No interfering substances were found, and the time for analysis was 65 min for one sample. In addition, this proposed method was applied to a medico-legal case where the cause of death was suspected to be acute local anaesthetics poisoning. Mepivacaine was detected in the left and right heart blood samples of the victim at concentrations of 18.6 and 15.8 mu g/g, respectively.
(66) Determination of organoarsenicals in the environment by solid- phase microextraction gas chromatography mass spectrometry AU: Szostek_B, Aldstadt_JH NA: ARGONNE NATL LAB,DIV ENVIRONM RES,9700 S CASS AVE,ARGONNE,IL,60439 ARGONNE NATL LAB,DIV ENVIRONM RES,ARGONNE,IL,60439 JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.807, No.2, pp.253-263 IS: 0021-9673 DT: Article AB: The development of a method for the analysis of organoarsenic compounds that combines dithiol derivatization with solid-phase microextraction (SPME) sample preparation and gas chromatography-mass spectrometry (GC-MS) is described. Optimization focused on a SPME-GC-MS procedure for determination of 2-chlorovinylarsonous acid (CVAA), the primary decomposition product of the chemical warfare agent known as Lewisite. Two other organoarsenic compounds of environmental interest, dimethylarsinic acid and phenylarsonic acid, were also studied. A series of dithiol compounds was examined for derivatization of the arsenicals, and the best results were obtained either with 1,3-propanedithiol or 1,2-ethanedithiol. The derivatization procedure, fiber type, and extraction time were optimized. For CVAA, calibration curves were linear over three orders of magnitude and limits-of-detection were <6.10(- 9) M in solution, the latter a more than 400x improvement compared to conventional solvent extraction GC-MS methods. A precision of <10% R.S.D. was typical for the SPME-GC-MS procedure. The method was applied to a series of water samples and soil/sediment extracts, as well as to aged soil samples that had been contaminated with Lewisite. (C) 1998 Elsevier Science B.V. All rights reserved. KP: MONOMETHYLARSONIC ACID, DERIVATIZATION, SAMPLES, SPECIATION, WATER WA: soil, warfare agents, organoarsenic compounds, chlorovinylarsonous acid, arsenic
(67) Use of solid phase microextraction of volatile compounds in whey protein concentrates AU: Yang_J, Li_WL, Harper_WJ NA: OHIO STATE UNIV,DEPT FOOD SCI & TECHNOL,COLUMBUS,OH,43210 JN: MILCHWISSENSCHAFT-MILK SCIENCE INTERNATIONAL, 1998, Vol.53, No.4, pp.209-212 IS: 0026-3788 DT: Article AB: The use of solid phase microextraction (SPME) to extract volatiles from whey protein concentrates was evaluated in this study. Best results were obtained by stirring the WPC solution at 40 degrees C for at 4 h. Variability in the reproducibility of different SPME fibers requires testing of the fibers before use. SPME recovered almost 3 times as many compounds from WPC than did either acetonitrile extraction or distillation and provides a simple and useful method for estimation of volatile compounds in whey protein concentrates.
(68) Improved extraction of ethanol from human body fluids by headspace solid-phase microextraction with a carboxen- polydimethylsiloxane-coated fiber AU: Lee_XP, Kumazawa_T, Sato_K, Seno_H, Ishii_A, Suzuki_O NA: SHOWA UNIV,SCH MED,DEPT LEGAL MED,SHINAGAWA KU,1-5-8 HATANODAI,TOKYO 1428555,JAPAN SHOWA UNIV,SCH MED,DEPT LEGAL MED,SHINAGAWA KU,TOKYO 1428555,JAPAN HAMAMATSU UNIV,SCH MED,DEPT LEGAL MED,HAMAMATSU,SHIZUOKA 431319,JAPAN JN: CHROMATOGRAPHIA, 1998, Vol.47, No.9-10, pp.593-595 IS: 0009-5893 DT: Article AB: Ethanol can be extracted from human whole blood and urine by headspace solid-phase microextraction (SPME) with a Carboxen- polydimethylsiloxane-coated fiber. Whole-blood containing ethanol, with isobutanol as internal standard (IS), is heated at 60 degrees C in the presence of (NH4)(2)SO4 and sodium dithionite. A Carboxen-polydimethylsiloxane-coated SPME fiber is then exposed to the headspace in the vial for 15 min and then injected into a mdium-bore capillary GC injection port. For urine the SPME procedure is essentially the same as that for whole blood except that the sodium dithionite is omitted. Recoveries of ethanol and IS were, respectively, 1.98 and 28.1% for whole blood, and 2.91 and 35.1% for urine. The calibration curves for ethanol were linear in the range 2.5-400 mg L-1 for whole blood and 0.5-400 mg L-1 for urine; the detection limits for whole blood and urine were 0.5 mg L-1 and 0.2 mg L-1, respectively. Data obtained for determination of ethanol after the drinking of beer are presented for two subjects. This SPME method with the new fiber for ethanol and IS resulted in sensitivity 40-1080 times greater than that obtained with the previous SPME method employing a Carbowax-divinylbenzene-coated fiber.
(69) Rapid SPME/LC/MS/MS analysis of N-methylcarbamate pesticides in water AU: Volmer_DA, Hui_JPM NA: MERCK KGAA,CENT RES ANAL ZD A ZFA,FRANKFURTER STR 250,D-64271 DARMSTADT,GERMANY NATL RES COUNCIL CANADA,INST MARINE BIOSCI,HALIFAX,NS B3H 3Z1,CANADA JN: ARCHIVES OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY, 1998, Vol.35, No.1, pp.1-7 IS: 0090-4341 DT: Article AB: Solid-phase microextraction combined with fast short-column liquid chromatography/electrospray ionization tandem mass spectrometry (SPME/LC/MS/MS) was used for isolating and analyzing nine N-methylcarbamate pesticides from water samples. Several SPME parameters, such as polarity of fibers, extraction time, and effect of ionic strength, were investigated and their impact on the SPME/LC/MS/MS technique was studied. The method was shown to be sensitive with detection limits between 0.3 and 1.9 mu g/L and reproducible with precision between 4.5 and 12.7% RSD. The versatility of the method was exhibited by its excellent linearity in the concentration range of 2-2,000 mu g/L in drinking water. A comparison of the SPME/LC/MS/MS method with LC/MS/MS methods utilizing traditional sample preparation techniques shows that the former offers similar performance in terms of precision and linearity, but is clearly easier to use and faster to perform.
(70) Some applications of solid phase micro extraction (SPME) in the analysis of pesticide residues in food AU: Volante_M, Cattaneo_M, Bianchi_M, Zoccola_G NA: PMIP UO CHIM,AZIENDA SANITARIA LOCALE,VIA CADORNA 8,I-22100 COMO,ITALY JN: JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH PART B-PESTICIDES FOOD CONTAMINANTS AND AGRICULTURAL WASTES, 1998, Vol.33, No.3, pp.279-292 IS: 0360-1234 DT: Article AB: The Solid Phase Micro-Extraction (SPME) technique was applied to analyze chlorpropham in potatoes and amitraz in honey. The homogenized sample, suspended in water and stirred, was extracted with a 100 mu m thick polidimetylsiloxane fiber and desorbed into the injection port of a gas chromatograph/mass- spectrometer (quadrupole) operating in single: ion monitoring. Sensitivities down to 0.01 mg/Kg and linear responses in the range of 0.01 - 0.1 mg/Kg were obtained. The results of SPME pesticide residue analysis in potatoes corresponded to those obtained with a traditional multiresidue method.
(71) Fast screening method for wine headspace compounds using solid- phase microextraction (SPME) and capillary GC technique AU: Vas_GY, Koteleky_K, Farkas_M, Dobo_A, Vekey_K NA: MINIST AGR,RES INST VITICULTURE & ENOL,EGER,HUNGARY HUNGARIAN ACAD SCI,CENT RES INST CHEM,BUDAPEST,HUNGARY JN: AMERICAN JOURNAL OF ENOLOGY AND VITICULTURE, 1998, Vol.49, No.1, pp.100-104 IS: 0002-9254 DT: Article AB: Solid-phase microextraction (SPME) coupled to capillary gas chromatography-mass spectrometry (GC-MS) was used for determination of volatile wine components. This combination offers a simple, quick, and sensitive approach suitable for characterization of wine aroma compounds without a complicated sample preparation procedure. Wines are characterized by ''aromagrams'', a set of identified components with corresponding relative abundances. Reproducibility (RSD errors of relative peak abundances) due to the analytical procedure are ca. 4%; variations among different samples of the same type of wine from the same region are ca. 8%. SPME-GC(-MS) has been shown to yield far larger differences among different wine types (Chardonnay, Muscat Ottonel, and Tramini) and among the same type of wine produced in different regions, showing the utility of the technique in wine analysis.
(72) Recent advances in solid-phase microextraction AU: Lord_HL, Pawliszyn_J NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA JN: LC GC-MAGAZINE OF SEPARATION SCIENCE, 1998, No.SS, pp.41-46 IS: 0888-9090 DT: Article AB: Solid-phase microextraction (SPME) offers several advantages for sample preparation, including reduced time per sample, less sample manipulation, an elimination of organic solvents, and reduced analyte loss. Although originally introduced for the analysis of volatile organic compounds in environmental samples, the technique now has gained acceptance for a wide variety of additional applications. In this article, the authors summarize some of their recent work in the application of SPME to new analytes and matrices, the design of new interfaces for separation and detection, and the development of new microextraction technologies.
(73) Trace explosives signatures from World War II unexploded undersea ordnance AU: Darrach_MR, Chutjian_A, Plett_GA NA: CALTECH,JET PROP LAB,4800 OAK GROVE DR,PASADENA,CA,91109 CALTECH,JET PROP LAB,PASADENA,CA,91109 JN: ENVIRONMENTAL SCIENCE & TECHNOLOGY, 1998, Vol.32, No.9, pp.1354-1358 IS: 0013-936X DT: Article AB: Trace explosives signatures of TNT and DNT have been extracted from multiple sediment samples adjacent to unexploded undersea ordnance at Halifax Harbor, Canada. The ordnance was hurled into the harbor during a massive explosion some 50 years earlier, in 1945 after World War II had ended. Laboratory sediment extractions were made using the solid-phase microextraction (SPME) method in seawater and detection using the Reversal Electron Attachment Detection (READ) technique and, in the case of DNT, a commercial gas chromatograph/mass spectrometer (GC/MS). Results show that, after more than 50 years in the environment, ordnance that appeared to be physically intact gave good explosives signatures at the parts per billion level, whereas ordnance that had been cracked open during the explosion gave no signatures at the 10 parts per trillion sensitivity level. These measurements appear to provide the first reported data of explosives signatures from undersea unexploded ordnance.
(74) Determination of cannabinoids in water and human saliva by solid-phase microextraction and quadrupole ion trap gas chromatography mass spectrometry AU: Hall_BJ, SatterfieldDoerr_M, Parikh_AR, Brodbelt_JS NA: UNIV TEXAS,DEPT CHEM & BIOCHEM,AUSTIN,TX,78712 JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.9, pp.1788-1796 IS: 0003-2700 DT: Article AB: Solid-phase microextraction (SPME) is applied to the determination of cannabidiol, Delta(8)-tetrahydrocannabinol (Delta(8)THC), Delta(9)-tetrahydrocannabinol (Delta(9)-THC), and cannabinol in pure water and human saliva. The inherent extraction behavior of the cannabinoids in pure water is evaluated along with optimization of the method in human saliva. The commercially available poly(dimethylsiloxane) (PDMS) SPME fibers were found to be the best class for the cannabinoid analysis. Partition coefficients were found to be extremely large for all of the cannabinoids (log K > 4.0). Equilibrium times for the 7- and 30-mu m PDMS fibers were 50 and 240 min, respectively. A shorter extraction time of 10 min with the 30-mu m PDMS fiber may be used for multiple extractions from the same vial, thus conserving the sample necessary for analysis and speeding up the total analysis time. Recoveries for the cannabinoids ire saliva, relative to pure water, were dramatically improved by a method developed in our laboratory involving addition of glacial acetic acid to the sample vial prior to performing SPME. Using this method, recoveries relative to SPME in pure welter ranged from 21 to 47% depending on the cannabinoid. The linear range for spiked saliva samples was established at 5-500 ng/mL (r(2) > 0.994) with precisions between 11 and 20% RSD. The ultimate level of detection by SPME for the cannabinoids in saliva was 1.0 ng/mL, with signal-to-noise values of greater than or equal to 12. A saliva sample collected 30 min after marijuana smoking was subject to SPME and traditional liquid-liquid extraction analysis, Internal standard quantitation results for Delta(9)- THC by both methods yielded comparable results, indicating that the SPME method of analysis is highly accurate and precise. The level of Delta(9)-THC by SPME was found to be 9.54 ng/mL for the saliva sample.
(75) Adsorption versus absorption of polychlorinated biphenyls onto solid-phase microextraction coatings AU: Yang_Y, Hawthorne_SB, Miller_DJ, Liu_Y, Lee_ML NA: UNIV N DAKOTA,ENERGY & ENVIRONM RES CTR,CAMPUS BOX 9018,GRAND FORKS,ND,58202 UNIV N DAKOTA,ENERGY & ENVIRONM RES CTR,GRAND FORKS,ND,58202 BRIGHAM YOUNG UNIV,DEPT CHEM & BIOCHEM,PROVO,UT,84602 JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.9, pp.1866-1869 IS: 0003-2700 DT: Article AB: Absorption-based polymeric solid-phase microextraction (SPME) fibers with poly(dimethylsiloxane) (PDMS) coatings were used to determine the partitioning coefficients of polychlorinated biphenyls (PCBs) between the sorptive fiber coatings and water. Previous models showing very good correlations between octanol- water partitioning coefficients (K-ow) and absorption-based fiber-water partitioning coefficients (K-dv) for low-molecular- weight analytes failed to predict K-dv values for PCBs. In fact, K-dv values for PCBs were 1-7 orders of magnitude lower than those predicted by K-ow and actually showed a strong negative correlation between K-ow and K-dv for higher molecular weight analytes (MW >similar to 200), K-dv values obtained using PDMS fibers with 7- and 100-mu m coatings also disagree, demonstrating that K-dv cannot be used to describe the partitioning behavior of PCBs between PDMS and water. However, when PCB partitioning cofficients were calculated on the basis of surface area (K-ds), the K-ds values obtained using 7- and 100-mu m PDMS fibers agreed reasonably well, demonstrating that surface adsorption is be primary mechanism controlling PCB (and likely other higher molecular weight solutes) partitioning from water to SPME sorbents.
(76) Gas-phase postderivatization following solid-phase microextraction for determining acidic herbicides in water AU: Lee_MR, Lee_RJ, Lin_YW, Chen_CM, Hwang_BH NA: NATL CHUNGHSING UNIV,DEPT CHEM,TAICHUNG 40227,TAIWAN JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.9, pp.1963-1968 IS: 0003-2700 DT: Article AB: This study analyzes acidic herbicides from an aqueous sample by developing a methylated postderivatization on the fiber following solid-phase microextration (SPME) with diazomethane gas procedure combined with GC/MS. Analysis results indicate that a silica fiber coated with polyacrylate (PA) yields a higher extraction efficiency than that obtained with poly(dimethylsiloxane) (PDMS) using the SPME technique. Detection limits are achieved at the level of 10-30 ng/L, Linearity is obtained over a wide range, with precision below 12% RSD. In addition, the significant reduction in extraction efficiency is attributed to the concentration of humic acids exceeding 5 mg/L. Various degradation compounds of acidic herbicides in basic solution are also detected, including 2,4- dichlorophenol, 2,4,5-trichlorophenol, 4-chloro-3-methylphenol, pentachlorinated biphenyl, and tetrachlorinated biphenyl. Moreover, the amount of pentachlorinated biphenyl and tetrachlorinated biphenyl increases over time.
(77) Solid-phase microextraction of monocyclic aromatic amines from biological fluids AU: DeBruin_LS, Josephy_PD, Pawliszyn_JB NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA UNIV GUELPH,DEPT CHEM & BIOCHEM,GUELPH WATERLOO CTR GRAD WORK CHEM,GUELPH,ON N1G 2W1,CANADA JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.9, pp.1986-1992 IS: 0003-2700 DT: Article AB: A solid-phase microextraction (SPME) protocol was developed for the quantitative analysis of monocyclic aromatic amines from biological fluids, me headspace SPME sampling technique was optimized for extraction and concentration of five target analytes (aniline, o-toluidine, 2-chloroaniline, 2,6- dimethylaniline, 2,4,6-trimethylaniline) from urine, blood, and milk. The temperature, pH, and ionic strength of the matrix sample were modified to allow maximum adsorption of the analytes onto the SPME fiber. This method is rapid yet sensitive and can be completed in 15 min on a 5-mL sample. SPME/GC/MS analysis yielded good reproducibility (RSD >11%) for each analyte from urine, blood, and milk, Method detection limits for the various biological fluids were determined and ranged from 0.40 ppb for 2,4,6-trimethylaniline in urine to 7.7 ppb for aniline in blood. This SPME sampling protocol can be applied to the biomonitoring of monocyclic aromatic amines from occupational, environmental, and medical exposure.
(78) Determination of tobacco alkaloids using solid phase microextraction and GC-NPD AU: Yang_SS, Smetena_I NA: PHILLIP MORRIS INC,RES CTR,RICHMOND,VA,23261 JN: CHROMATOGRAPHIA, 1998, Vol.47, No.7-8, pp.443-448 IS: 0009-5893 DT: Article AB: The sampling approaches using solid phase microextraction (SPME) were evaluated for the analysis of tobacco alkaloids. Because of their low volatility and ionic nature, sampling alkaloids from the headspace of dry or met tobacco samples often required more effort to improve extraction efficiency. Directly dipping the SPME fiber coated with polydimethylsiloxane film into the tobacco extract was proved to be a simple, effective tool for sampling alkaloids from tobacco. When combined with the practice of fast GC and nitrogen-phosphorus detection, nicotine and a group of selected minor alkaloids (i.e., nornicotine, myosmine, anabasine and anatabine) were separated with baseline resolution within 3 min. The detection limits for these alkaloids are below 0.1 mu g mL(-1). In addition, the carry-over problem frequently occurred in alkaloids analysis was eliminated. The influence of tobacco matrix and fiber aging on the partition of alkaloids, as well as the use of an internal standard to compensate these deviations, were also studied.
(79) Application of solid-phase microextraction and gas chromatography mass spectrometry for the determination of chlorophenols in urine AU: Lee_MR, Yeh_YC, Hsiang_WS, Chen_CC NA: NATL CHUNGHSING UNIV,DEPT CHEM,TAICHUNG 40227,TAIWAN JN: JOURNAL OF CHROMATOGRAPHY B, 1998, Vol.707, No.1-2, pp.91-97 IS: 0378-4347 DT: Article AB: This study investigated the feasibility of applying solid-phase microextraction (SPME) combined with gas chromatography-mass spectrometry to analyze chlorophenols in urine. The SPME experimental procedures to extract chlorophenols in urine were optimized with a polar polyacrylate coated fiber at pH 1, extraction time for 50 min and desorption in GC injector at 290 degrees C for 2 min. The linearity was obtained with a precision below 10% R.S.D. for the studied chlorophenols in a wide range from 0.1 to 100 mu g/l. In addition, sample extraction by SPME was used to estimate the detection limits of chlorophenols in urine, with selected ion monitoring of GC-RIS operated in the electron impact mode and negative chemical ionization mode. Detection limits were obtained at the low ng/l levels. The application of the methods to the determination of chlorophenols in real samples was tested by analyzing urine samples of sawmill workers. The chlorophenols were found in workers, the urinary concentration ranging from 0.02 mu g/l (PCP) to 1.56 mu g/l (2,4-DCP) depending on chlorophenols. The results show that trace chlorophenols have been detected with SPME-GC-MS in the workers of sawmill where chlorophenol- containing anti-stain agents had been previously used.
(80) Determination of amphetamine and methamphetamine in human hair by headspace solid-phase microextraction and gas chromatography with nitrogen-phosphorus detection AU: Koide_I, Noguchi_O, Okada_K, Yokoyama_A, Oda_H, Yamamoto_S, Kataoka_H NA: OKAYAMA PREFECTURAL POLICE HEADQUARTERS,CRIMINAL INVEST LAB,1- 3-2 TONDA CHO,OKAYAMA 700,JAPAN OKAYAMA UNIV,FAC PHARMACEUT SCI,OKAYAMA 700,JAPAN JN: JOURNAL OF CHROMATOGRAPHY B, 1998, Vol.707, No.1-2, pp.99-104 IS: 0378-4347 DT: Article AB: A simple and rapid method for the determination of amphetamine (AP) and methamphetamine (MA) in human hair was developed by headspace solid-phase microextraction (SPME) and gas chromatography with nitrogen-phosphorus detection (GC-NPD). The hair (1 mg) was dissolved in 0.2 ml of a 5 M sodium hydroxide solution in a tightly sealed vial by shaking at 75 degrees C for about 5 min. In order to adsorb AP and MA on the SPME fiber, 100 mu m of polydimethylsiloxane fiber was exposed to the headspace of the vial, and the vial was heated at 55 degrees C for 20 min. Then the fiber was removed from the vial and inserted into the injection port of the GC-NPD system using a CBJ-17 capillary column. The compounds adsorbed on the fiber were analyzed by exposing the fiber at 220 degrees C for 30 s in the GC injection port. By using this method, AP and MA in human hair could be analyzed simply and rapidly without any interference from coexisting substances. The percentages of AP and MA extracted from human hair by the SPME method were 48 and 62%, respectively, and relative standard deviations were below 10% (n=5). The calibration curves for AP and MA were linear in the ranges of 0.4-15 and 4-160 ng/mg hair, respectively. The detection limits of AP and MA at a signal-to-noise ratio of three were 0.1 and 0.4 ng/mg hair, respectively. This method could be applied to the analysis of an abuser's hair sample.
(81) Solid-phase microextraction for the analysis of some alcohols and esters in beer: Comparison with static headspace method AU: Jelen_HH, Wlazly_K, Wasowicz_E, Kaminski_E NA: ACAD AGR POZNAN,INST FOOD TECHNOL,WOJSKA POLSKIEGO 31,PL-60624 POZNAN,POLAND JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, Vol.46, No.4, pp.1469-1473 IS: 0021-8561 DT: Article AB: Headspace solid-phase microextraction (SPME) has been used for the determination of 12 alcohols and esters in beer. SPME analysis parameters using polyacrylate fiber have been defined and compared with the static headspace (SHS) method used as a reference. Limits of detection, linearity, and repeatability of both methods have been determined using standard solutions. Limits of detection of SPME were generally lower than of the SHS method, and addition of salt enhanced SPME adsorption. Both methods were characterized by high repeatability and good linearity. Results of beer analyses obtained by using these two methods were highly correlated, which indicates the possibility of SPME application as an inexpensive alternative to automated SHS in the analysis of higher alcohols and esters in beer.
(82) Identification of volatile organic compounds present in different honeys through SPME and GC/MS LA: Italian AU: Guidotti_M, Vitali_M NA: PRESIDIO MULTIZONALE PREVENZ,VIA SALARIA AQUILA 8,I-02100 RIETI,ITALY JN: INDUSTRIE ALIMENTARI, 1998, Vol.37, No.368, p.351 (4 pages) IS: 0019-901X DT: Article AB: Several different single-flower honeys were investigated in order to verify the possibility of a classification on the basis of analytical data on their flavours and/or fragrances composition. For this purpose the headspace of 18 honey samples produced From 6 different flowers was analysed by gaschromatography/mass spectrometry. For each single-flower honey analysed the obtained data allow a characterisation based on the identification of several specific compounds present in that single-flower group of samples and not in others.
(83) Use of solid-phase microextraction capillary gas chromatography (SPME-CGC) for the varietal characterization of wines by means of chemometrical methods AU: Garcia_DD, Reichenbacher_M, Danzer_K, Hurlbeck_C, Bartzsch_C, Feller_KH NA: UNIV JENA,INST ANORGAN & ANALYT CHEM,LESSINGSTR 8,D-07743 JENA,GERMANY UNIV JENA,INST ANORGAN & ANALYT CHEM,D-07743 JENA,GERMANY FH JENA,FACHBEREICH MED TECH,D-07743 JENA,GERMANY JN: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY, 1998, Vol.360, No.7- 8, pp.784-787 IS: 0937-0633 DT: Article AB: The extraction of wine aroma compounds was studied by direct- SPME (DI/SPME), headspace-SPME (HS/SPME) and multiple- headspace-extraction-SPME (MHE/SPME). The aromagrams obtained by HS/SPME-CGC were evaluated with chemometrical methods for the varietal classification of wines.
(84) Octanol/water-partitioning of four HCH isomers at 5, 25 AND 45 degrees C AU: Paschke_A, Schuurmann_G NA: UFZ CTR ENVIRONM RES,DEPT CHEM ECOTOXICOL,PERMOSERSTR 15,D- 04318 LEIPZIG,GERMANY JN: FRESENIUS ENVIRONMENTAL BULLETIN, 1998, Vol.7, No.5-6, pp.258- 263 IS: 1018-4619 DT: Article AB: The octanol/water partition coefficient (K-ow) of alpha-, beta- , gamma- and delta-hexachlorocyclohexane (HCH) was determined at 5, 25 and 45 degrees C using the slow-stirring method followed by solid-phase microextraction (SPME) and gas chromatography. The temperature variation of log K-ow is greater between 5 and 25 degrees C (approximate to -0.006 K-1) than from 25 to 45 degrees C (< -0.001 K-1). A preliminary thermodynamic analysis shows that the HCH transfer from water and octanol is slightly exothermic with a gain of entropy. In this respect, no significant differences have been found between the isomers.
(85) Solid-phase microextraction of polychlorinated biphenyls AU: Yang_Y, Miller_DJ, Hawthorne_SB NA: UNIV N DAKOTA,ENERGY & ENVIRONM RES CTR,15 N 23RD ST,POB 9018,GRAND FORKS,ND,58202 UNIV N DAKOTA,ENERGY & ENVIRONM RES CTR,GRAND FORKS,ND,58202 JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.800, No.2, pp.257-266 IS: 0021-9673 DT: Article AB: The extraction and analysis of 21 polychlorinated biphenyls (PCBs) ranging from di-to decachlorobiphenyls in ocean, wetland and leachate water samples were achieved using solid-phase microextraction (SPME) with a 100-mu m poly(dimethylsiloxane) (PDMS) fiber and gas chromatography-electron capture detection (GC-ECD). Severe carryover between samples (e.g., 20%) occurs on both stir bars and the SPME fibers demonstrating that it is important to use a new stir bar for each sample, as well as to perform SPME-GC blanks between samples to avoid quantitative errors. The equilibrium partitioning coefficients of individual PCB congeners between FDMS and water were found to be surprisingly different compared to their octanol-water partitioning coefficient (K-ow), demonstrating that K-ow cannot be used to estimate the partitioning behavior of PCBs in the SPME process. Using a 15-min SPME extraction, SPME analysis with GC-ECD was linear (r(2) greater than or equal to 0.97) from similar to 5 pg/ml to the solubility limit of each congener. Concentrations in water samples obtained by 15-min SPME extractions compared favorably with those obtained by toluene extractions, demonstrating that SPME combined with GC isa useful technique for the rapid determination of PCBs in water samples. (
(86) Determination of urinary pentachlorophenol by SPME and GC/MS AU: Guidotti_M, Vitali_M NA: PRESIDIO MULTIZONALE PREVENZ ASL RIETI,VIA SALARIA LAQUILA 8,I- 02100 RIETI,ITALY UNIV ROMA LA SAPIENZA,CATTEDRA IGIENE AMBIENTALE,IST IGIENE,I- 00185 ROME,ITALY JN: HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY, 1998, Vol.21, No.2, pp.137-139 IS: 0935-6304 .
(87) Solid-phase microextraction and cuticular hydrocarbon differences related to reproductive activity in queenless ant Dinoponera quadriceps AU: Monnin_T, Malosse_C, Peeters_C NA: UNIV PARIS 06,ECOL LAB,CNRS URA 258,7 QUAI ST BERNARD,F-75252 PARIS 05,FRANCE UNIV PARIS 13,CNRS URA 667,LAB ETHOL EXPT & COMPAREE,F-93430 VILLETANEUSE,FRANCE INRA,UNITE PHYTOPHARM & MEDIATEURS CHIM,F-78026 VERSAILLES,FRANCE JN: JOURNAL OF CHEMICAL ECOLOGY, 1998, Vol.24, No.3, pp.473-490 IS: 0098-0331 DT: Article AB: We extracted the cuticular hydrocarbons from live Dinoponera quadriceps ants (10 colonies collected from Brazil) with the solventless solid-phase microextraction (SPME) technique. Gas chromatography of the SPME samples (N = 233 measurements) compared with pentane extracts (N = 10) resulted in similar profiles. Eighty-one compounds belonging to the main long-chain hydrocarbon families were identified by GC-MS. There is no morphologically specialized queen in D. quadriceps and only one aggressively dominant worker (alpha) mates and reproduces in each colony. The alpha ant (N = 26 individuals) always yielded higher amounts and percentages of g-hentriacontene (9-C-31:1) than her sterile nestmates (N = 47). Since SPME is not destructive, it allowed for the repeated extraction of the same individuals, demonstrating that the alpha ant (virgin or mated) always had higher levels of 9-hentriacontene. This difference appears related to ovarian activity and may function as a signal of the alpha's dominance status.
(88) A versatile and quantitative volatile-delivery system for laboratory bioassays AU: Bartelt_RJ, Zilkowski_BW NA: USDA ARS,NATL CTR AGR UTILIZAT RES,BIOACT AGENTS RES UNIT,1815 N UNIV ST,PEORIA,IL,61604 JN: JOURNAL OF CHEMICAL ECOLOGY, 1998, Vol.24, No.3, pp.535-558 IS: 0098-0331 DT: Article AB: A versatile moving-air system is described for delivering volatiles into a wind tunnel or other bioassay device. The system controls up to four volatile sources at one time. There is a calibrated, adjustable splitter for each source so that any percentage of a source's airstream, or none of it, can be directed to the system outlet at any moment. Thus, the system allows the sample volatiles to be bioassayed in any order and at any level or in mixtures of any desired proportions. Volatile sources of many types can be used, including single chemicals in slow-release formulations, mixtures of chemicals, or volatiles from living organisms. The volatile stream can be sampled by solid-phase microextraction (SPME) just before it enters the wind tunnel. Analysis of the SPME sample by gas chromatography allows absolute delivery rates of volatile components to be calculated. System performance was characterized with physical measurements and with bioassay experiments involving Carpophilus humeralis (F.) (Coleoptera: Nitidulidae). One bioassay experiment demonstrated how volatiles from a microbial culture (fermenting bread dough) and a synthetic counterpart (an aqueous solution of acetaldehyde, ethanol, I-propanol, isobutanol, 3-methyl-1-butanol, 2-methyl- 1-butanol, and ethyl acetate) could be compared at a range of dose levels, with just one sample of each type. These natural and synthetic volatile sources delivered very similar amounts of the above compounds and produced nearly identical dose- response curves. In another experiment, three bread dough volatiles (ethanol, acetaldehyde, and ethyl acetate) were tested in mixtures. Each component was used at four different levels (giving a total of 64 experimental treatments), but just one physical sample was needed for each chemical. The experiment provided clear information about response thresholds and interactions among these host volatiles. The volatile delivery system is versatile, easy to operate, and can be constructed from inexpensive materials.
(89) Solid phase microextraction (SPME) for sample preparation during drug metabolism studies LA: German AU: Kroll_C, Borchert_HH NA: HUMBOLDT UNIVERSITAT BERLIN,INST PHARM,MATH NATURWISSENSCHAFTLICHE FAK 1,GOETHESTR 54,D-13086 BERLIN,GERMANY JN: PHARMAZIE, 1998, Vol.53, No.3, pp.172-177 IS: 0031-7144 DT: Article AB: Within the scope of the investigation of drug metabolism in keratinocytes solid phase microextraction (SPME) was investigated as a suitable method for sample preparation. The application of SPME is based on the fact, that a amount of analyte is absorbed by the polymer fiber at equilibrium, and the fiber is localized on a tip of a GC-syringe. The stable nitroxyl radical TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl) and its apolar metabolite 2,2,6,6-tetramethylpiperidine were analyzed by SPME and subsequent GC using thymol as internal standard. By means of the headspace-technique and an apolar fiber the recovery rate of TEMPO and the metabolite was nearly 100% and the precision was high. However, the results of the direct SPME were unsatisfactory. In comparison with conventional liquid/liquid extraction and solid phase extraction SPE the SPME proved the best results with regard to recovery rate and precision. Furthermore, the main advantages of SPME are the renunciation of organic solvents, the saving of time, the possibility to reuse the fiber about 100-150 times and the option for a complete automatisation of the extraction procedure.
(90) Determination of pesticide residues in wine by SPME and GC/MS for consumer risk assessment AU: Vitali_M, Guidotti_M, Giovinazzo_R, Cedrone_O NA: UNIV ROMA LA SAPIENZA,IST IGIENE G SANARELLI,CATTEDRA IGIENE AMBIENTALE,PIAZZALE ALDO MORO 5,I-00185 ROME,ITALY JN: FOOD ADDITIVES AND CONTAMINANTS, 1998, Vol.15, No.3, pp.280-287 IS: 0265-203X DT: Article AB: An analytical procedure applying solid phase microextraction (SPME) combined with gas chromatography/mass spectrometry (GC/MS) for the detection of pesticide residues in wine was performed for the determination of 14 of the pesticides most frequently used on grapes (insecticides, fungicides, herbicides). As SPME combines the possibility of a single-step extraction with other advantages (shout sampling times, solvent-free procedure, speedy extraction, low cost and simplicity) it could be successfully used either for screening or routine analysis for detecting pesticides of different chemical classes in wines, even at trace levels. The analytical procedure performed showed minimum detectable quantities ranging from 0.10 mu g/l to 6.0 mu g/l and precision from 9.7% to 18% (as relative standard deviation of 1 mu g/l levels), assuring high sensitivity and precision of analysis. Twenty-one wine samples (10 white wines and 11 red wines) available on the Italian market were analysed with the procedure described and about 57% were positive for one or more pesticides. An approach for consumer risk assessment on the basis of the data obtained was proposed for further assessments of the daily dietary intake of pesticides through wine.
(91) Determination of chlorinated acetic acids in drinking water by in-situ derivatization and solid phase microextraction AU: Aikawa_B, Burk_RC NA: CARLETON UNIV,CTR ANALYT & ENVIRONM CHEM,OTTAWA,ON K1S 5B6,CANADA JN: INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY, 1997, Vol.66, No.3, pp.215-224 IS: 0306-7319 DT: Article AB: A method is described for the determination of chlorinated acetic acids in water. The method employs in situ derivatization of the acids to their methyl esters using HCl and methanol, followed by solid phase microextraction and quantitation by GC/ECD. Optimized Ones of derivatization, adsorption and desorption have been determined. Formation of chloroform from decarboxylation of trichloroacetic acid is minimized by choice of reaction time, thereby maximizing formation of the trichloroacetic acid methyl ester. Detection limits are in the low mu g/L range for the di-and trichloroacetic acids due to the efficient adsorption of their esters on the SPME fiber, and the large response of the ECD to these species. Recoveries are similar to those found using EPA method 552. WA: chlorinated acetic acids, drinking water, solid phase microextraction
(92) Determination of DCIP in vegetables using solid-phase micro extraction and capillary GC/MS LA: Japanese AU: Iwasaki_Y, Harasaki_T, Tsuru_J, Hisano_H, Ikeda_Y NA: SAGA PREFECTURAL INST PUBL HLTH,1-20,HACHOUNAWATE MACHI,SAGA 849,JAPAN JN: JOURNAL OF THE FOOD HYGIENIC SOCIETY OF JAPAN, 1997, Vol.38, No.5, pp.347-350 IS: 0015-6426 DT: Article AB: A method for the determination of DCIP in vegetables using solid-phase micro extraction (SPME) was developed. DCIP was extracted from the head space of a vegetable sample with a fused silica fiber and determined by SIM GC/MS. The coefficient of variation was 4.4% and 4.5% at concentrations of 0.2 mu g/g and 1 mu g/g, respectively, and the linearity of the calibration curve was good over a wide range of concentrations (0.01 mu g/g similar to 2 mu g/g). The recoveries of DCIP added to tomato, eggplant, onion, and spinach at levels of 0.02 similar to 0.1 mu g/g were 88 similar to 110%. The coefficients of variation were 2.0 similar to 7.8% for DCIP.
(93) Solid phase microextraction combined with HPLC for determination of metal ions using crown ether as selective extracting reagent AU: Jia_CR, Luo_YZ, Pawliszyn_J NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA JN: JOURNAL OF MICROCOLUMN SEPARATIONS, 1998, Vol.10, No.2, pp.167- 173 IS: 1040-7685 DT: Article AB: A new solid phase microextraction (SPME) method for the analysis of metal ions in aqueous samples has been developed. Fibers doped with crown ether were used to extract mercury ions from aqueous solution through the formation of a stable complex. The complex is then desorbed from the fiber using high-performance liquid chromatography (HPLC) for separation and UV detection. This newly developed SPME method for the extraction of metal ions from aqueous samples is possible to combine in-line with other more sensitive elemental detection methods such as Atomic Absorption Spectrometry (AAS), Inductively Coupled Plasma Atomic Emission Spectrometry (ICP- AES), etc. The potential of SPME as a portable field sampling tool makes it a promising solvent-free sample preparation method for environmental field analysis.
(94) Determination of five benzodiazepines in aqueous solution and biological fluids using solid-phase microextraction with Carbowax(TM)/DVB fiber coating AU: Luo_Y, Pan_L, Pawliszyn_J NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA JN: JOURNAL OF MICROCOLUMN SEPARATIONS, 1998, Vol.10, No.2, pp.193- 201 IS: 1040-7685 DT: Article AB: A method using direct solid-phase microextraction (SPME) coupled with gas chromatography (GC) and GC/mass spectrometry (GC/MS) for the determination of five benzodiazepines (diazepam, nordiazepam, oxazepam, temazepam, and lorazepam) in aqueous solution, urine, and serum was developed. The Carbowax(TM)-divinylbenzene (CAX/DVB) coated fiber extracted all five benzodiazepines in the highest amounts compared to the other fiber coatings examined: poly(arcylate) (PA), 100 mu m poly(dimethylsiloxane) (PDMS), and poly(dimethylsiloxane)/divinylbenzene (PD MS/DVB). The highest amount of all five and benzodiazepines extracted was under conditions of saturated salt with pH 7 and sampling at 45 degrees C with agitation. The method was linear over the range of 0.1-2 mu g/mL of sample using the CAX/DVB coated fiber. The limits of detection were determined as 0.02 mu g/L, 0.03 mu g/mL, and 0.1 mu g/mL of sample for diazepam and nordiazepam, oxazepam and lorazepam, and temazepam. The standard deviation values of intraday and interday measured for the five benzodiazepines were all less than 12.5%. The new method was also applied to the analysis of the above target analytes in urine and serum.
(95) Characterization of water-soluble components of slurries using solid-phase microextraction coupled to liquid chromatography mass spectrometry AU: Moder_M, Popp_P, Pawliszyn_J NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA LEIPZIG HALLE LTD,ENVIRONM RES CTR,DEPT ANALYT CHEM,D-04318 LEIPZIG,GERMANY JN: JOURNAL OF MICROCOLUMN SEPARATIONS, 1998, Vol.10, No.2, pp.225- 234 IS: 1040-7685 DT: Article AB: Water-soluble components from sludge and sediments were sampled and analyzed with solid-phase microextraction (SPME) and high- performance liquid chromatography-electro spray ionization-mass spectrometry (HPLC-ESI-MS). The extraction, desorption, and detection conditions were examined with Carbowax-coated SPME fibers for a number of selected carboxylic acids, phthalates, and surfactants. The maximum recoveries of the defined compounds were obtained for extraction times ranging from 1 to 15 h (phthalates and surfactants) with a desorption time of 2 min for a of 80:20 (v/v) methanol-ethanol mixture. The reference compounds were detected in the low-ppb range. The main components of analyzed sludge and sediment samples were identified as phthalates, fatty acids, nonionic surfactants, chlorinated phenols, and carbohydrate derivatives. Additional information for compound identification was obtained using different spray potentials for the mass spectrometric ionization. Switching from positive to negative ionization modes changed the selectivity and sensitivity of detection, thus allowing the detection of substances of different nature.
(96) Inter-laboratory validation of solid-phase microextraction for the determination of triazine herbicides and their degradation products at ng/1 level in water samples AU: Ferrari_R, Nilsson_T, Arena_R, Arlati_P, Bartolucci_C, Basla_R, Cioni_F, DelCarlo_G, Dellavedova_P, Fattore_E, Fungi_M, Grote_C, Guidotti_M, Morgillo_S, Muller_L, Volante_M NA: EUROPEAN JOINT RES CTR,INST ENVIRONM,I-21020 ISPRA,VA,ITALY SIGMA ALDRICH,I-20151 MILAN,ITALY EAAP,SERV VIGILANZA IGIENICA,BARI,ITALY PMIP,USSL N 7,UNITA OPERAT CHIM,LECCO,ITALY ARPAT,FLORENCE,ITALY INT CTR PESTICIDE SAFETY,BUSTO GAROLFO,MI,ITALY ARPA,MODENA,ITALY PMIP,USSL N 34,UNITA OPERAT CHIM,PARABIAGO,MI,ITALY MARIO NEGRI PHARMACOL RES INST,MILAN,ITALY AZIENDA ACQUEDOTTO MUNICIPALE,MONCALIERI,TO,ITALY FRAUNHOFER INST TOXICOL & AEROSOL RES,DEPT ANALYT CHEM,D-3000 HANNOVER,GERMANY PMIP,RIETI,ITALY PMIP,USSL N 5,UNITA OPERAT CHIM,CORNO,ITALY JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.795, No.2, pp.371-376 IS: 0021-9673 DT: Article AB: The accuracy and precision of solid-phase microextraction (SPME) were validated in an inter-laboratory study including ten laboratories for the analysis of triazine herbicides and their metabolites at ng/l level in aqueous samples. The SPME conditions were optimised in order to obtain maximum sensitivity. Especially, salt addition and choice of the SPME fibre coated with Carbowax-divinylbenzene increased the sensitivity. The average detection limits were in the range from 4 to 24 ng/l for the triazine herbicides, and 20 and 40 ng/l for desisopropylatrazine and desethylatrazine, respectively. The average r(2) values of the calibration curves were above 0.99 for all of the analytes. The statistical data treatment was performed in accordance with the International Standardisation Organisation (ISO) standard 5725. Relative repeatability standard deviations between 6 and 14% and relative reproducibility standard deviations between 10 and 17% were found. The determined concentrations of the reference sample compared well to the ''true'' values, thus proving the good accuracy of the method. It is concluded that SPME is a reliable technique for the quantitative analysis of water samples containing triazine herbicides in concentrations around the European limit of 100 ng/l for individual pesticides in drinking water.
(97) Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography AU: Takekawa_K, Oya_M, Kido_A, Suzuki_O NA: YAMANASHI MED UNIV,DEPT LEGAL MED,TAMAHO,YAMANASHI 40938,JAPAN YAMANASHI POLICE HEADQUARTERS,SCI CRIME DETECT LAB,ISAWA,YAMANASHI 406,JAPAN HAMAMATSU UNIV,SCH MED,DEPT LEGAL MED,HAMAMATSU,SHIZUOKA 43131,JAPAN JN: CHROMATOGRAPHIA, 1998, Vol.47, No.3-4, pp.209-214 IS: 0009-5893 DT: Article AB: Cyanide can be extracted from whole blood samples by headspace solid-phase microextraction (SPME) with a Carbowax/divinylbenzene-coated fiber. During heating a vial of a whole blood sample containing cyanide and acetonitrile as internal standard (IS) at 50 degrees C in the presence of Na2SO4, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial for 45 min to allow adsorption of cyanide and IS. The fiber needle was then injected into a capillary gas chromatography (GC) instrument equipped with nitrogen-phosphorus detection. The headspace SPME-GC with a Supel-Q PLOT fused silica capillary column gave large peaks for cyanide and IS; almost no interfering peaks appeared. Recoveries of cyanide and IS from human whole blood were 3.02- 4.06 % and 0.21 %, respectively. The calibration curve for cyanide added to human blood showed excellent linearity in the range of 0.04-4.0 mu g mL(-1); the detection limit was about 0.02 mu g mL(-1). The coefficients of intra-day and inter-day variation were not greater than 7.1 and 9.2 %. Good correlation (r(2) = 0.999) was found between the present SPME-GC method and the conventional microdiffusion colorimetric method. Data on determination of cyanide in rat blood after intraperitoneal administration are also presented.
(98) Effect of the various parameters governing solid-phase microextraction for the trace-determination of pesticides in water AU: Dugay_J, Miege_C, Hennion_MC NA: ECOLE SUPER PHYS & CHIM IND VILLE PARIS,URA CNRS 437,LAB ENVIRONM & CHIM ANALYT,10 RUE VAUQUELIN,F-75231 PARIS 05,FRANCE JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.795, No.1, pp.27-42 IS: 0021-9673 DT: Article AB: The parameters governing solid-phase microextraction (SPME) are investigated, with emphasis on the determination of the partition coefficients, K, and their use to predict the selection of a fibre, depending on the respective characteristics of the fibres and the analytes. Film thickness and stability of the compounds can interfere with the determination of K values. The time profile curves were determined for twelve pesticides having a wide range of water solubilities and polarities and using four fibres (polydimethylsiloxane, polydimethylsiloxane-divinylbenzene, Carbowax-divinylbenzene and polyacrylate). Although the affinity order was different for the four coatings, no correlation was found between the respective characteristics of the fibres and solutes. The two fibres containing divinylbenzene were shown to have the highest affinities and the polydimethylsiloxane had the lowest affinity. The polyacrylate fibre which is the more polar commercial fibre did not provide the highest affinities for the more polar and water-soluble analytes. The important parameters for quantitative analysis have been evaluated. The calibration curves were similar when one analyte of interest was present on its own in a drinking water sample, or when eleven other pesticides were present at the same concentration or when much higher concentrations of other analytes were present in the sample. Linearity was obtained over a wide range of concentrations in drinking water samples. Detection limits are in agreement with European regulatory levels in drinking water for most of the analytes using solid-phase microextraction-gas chromatography-nitrogen-phosphorus detection (SPME-GC-NPD). In contaminated surface water samples, the chromatograms are relatively clean and most of the compounds can be detected at levels lower than 0.5 mu g/l.
(99) Solid-phase microextraction and gas chromatography with mass spectrometric detection for the determination of pesticides in aqueous samples AU: Aguilar_C, Penalver_S, Pocurull_E, Borrull_F, Marce_RM NA: UNIV ROVIRA & VIRGILI,DEPT QUIM ANALIT & QUIM ORGAN,IMPERIAL TARRACO 1,TARRAGONA 43005,SPAIN JN: JOURNAL OF CHROMATOGRAPHY A, 1998, Vol.795, No.1, pp.105-115 IS: 0021-9673 DT: Article AB: Solid-phase microextraction (SPME) is a fast, alternative method for extracting organochlorine, triazine and thiocarbamate pesticides. An 85-mu m polyacrylate fiber was used to extract the analytes directly from aqueous samples and then thermal desorption was carried out in the hot injector of a gas chromatograph-mass spectrometer. To enhance the sensitivity of SPME, the temperature and the length of the extraction and desorption steps and the pH and salt concentration of the sample were optimized. The linearity of most of pesticides for real samples was found to be between 0.07 and 30 mu g 1(-1) when GC-MS under full-scan acquisition was used and between 0.005 and 10 mu g 1(-1) when selected-ion monitoring (SIM) acquisition was used. Limits of detection at the sub mu g 1(-1) level were achieved with GC and MS under the full-scan acquisition mode and at the ng 1(-1) level for MS under SIM acquisition. The repeatability of the method for tap water spiked at a level of 0.5 mu g,a 1(-1) (n=5) was below 25% (R.S.D.).
(100) Fast screening method for the profile analysis of polycyclic aromatic hydrocarbon metabolites in urine using derivatisation - solid-phase microextraction AU: Gmeiner_G, Krassnig_C, Schmid_E, Tausch_H NA: AUSTRIAN RES CTR SIEBERSDORF,DEPT ENVIRONM ANAL,A-2444 SEIBERSDORF,AUSTRIA UNIV VIENNA,INST ANALYT CHEM,A-1090 VIENNA,AUSTRIA JN: JOURNAL OF CHROMATOGRAPHY B, 1998, Vol.705, No.1, pp.132-138 IS: 0378-4347 DT: Article AB: A method for the qualitative analysis of various metabolites of naphthalane, phenanthrene and pyrene is presented. The method uses SPME with a 85-mu m polyacrylate fibre for extraction, headspace silylation with BSTFA without any catalyst for on- fibre derivatisation and GC-MS in the SIR mode for separation and detection. The suitability of the method for profile analysis of PAH metabolites is shown by analysing a smokers urine after enzymatic cleavage (and additionally after spiking with the target analytes) and spiked water. The method exhibits satisfactory separation of all investigated metabolites and no interferences due to matrix peaks. (
(101) Application of SPME/GC-MS to characterize metabolites in the biodesulfurization of organosulfur model compounds in bitumen AU: MacPherson_T, Greer_CW, Zhou_E, Jones_AM, Wisse_G, Lau_PCK, Sankey_B, Grossman_MJ, Hawari_JL NA: NATL RES COUNCIL CANADA,BIOTECHNOL RES INST,6100 ROYALMOUNT AVE,MONTREAL,PQ H4P 2R2,CANADA NATL RES COUNCIL CANADA,BIOTECHNOL RES INST,MONTREAL,PQ H4P 2R2,CANADA IMPERIAL OIL RESOURCES LTD,CALGARY,AB T2L 2K8,CANADA EXXON RES & ENGN CO,ANNANDALE,NJ,08801 JN: ENVIRONMENTAL SCIENCE & TECHNOLOGY, 1998, Vol.32, No.3, pp.421- 426 IS: 0013-936X DT: Article AB: A combined solid-phase microextraction/GC-MS analytical technique was used to monitor the formation of metabolites in the biodesulfurization of the bitumen model organosulfur compounds, dibenzothiophene (DBT) and the dialkylated derivative 4,6-diethyldibenzothiophene (DEDBT), by Rhodococcus sp. strain ECRD-1. In the case of DBT, the following metabolites were detected: DBT 5-oxide (sulfoxide), DBT 5,5- dioxide (sulfone), dibenz[c,e][1,2]oxathiin 6-oxide (sultine), dibenz[c,e][1,2]oxathiin 6,6-dioxide (sultone), and the end product, 2-hydroxybiphenyl (2-HBP), whereas, with DEDBT, 4,6- DEDBT 5-oxide, 4,6-diethyldibenz[c,el[1,2]oxathiin 6-oxide (sultine), and 2-hydroxy-3,3'-diethylbiphenyl (HDEBP) as the final product, were identified. A time course study for the formation and disappearance of DBT and DEDBT metabolites was used to construct desulfurization pathways, which in both cases, involved the formation of the corresponding sulfoxides.
(102) Solid phase microextraction with temperature-programmed desorption for the analysis of iodination disinfection byproducts AU: Frazey_PA, Barkley_RM, Sievers_RE NA: UNIV COLORADO,DEPT CHEM & BIOCHEM,COOPERAT INST RES ENVIRONM SCI,BOULDER,CO,80309 JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.3, pp.638-644 IS: 0003-2700 DT: Article AB: An analytical approach for the determination of chlorination and iodination disinfection byproducts based on solid-phase microextraction (SPME) was developed, Solid-phase microextraction presents a simple, rapid, sensitive, and solvent-free approach to sample preparation in which analytes in either air or water matrixes are extracted into the polymeric coating of an optical fiber. Analytes are subsequently thermally desorbed in the injection port of a gas chromatograph for separation, detection, and quantitation, Thermal degradation of iodoform was observed during desorption from a polyacrylate fiber in initial GC/MS and GC/ECD experiments, Experiments were designed to determine SPME conditions that would allow quantification without significant degradation of analytes. Isothermal and temperature-programmed thermal desorptions were evaluated for efficacy in transferring analytes with wide-ranging volatilities and thermal stabilities into chromatographic analysis columns, A temperature-programmed desorption (TPD) (120-200 degrees C at 5 degrees C/min with an on-column injection port or 150-200 degrees C at 25 degrees C/min with a split/splitless injection port) was able to efficiently remove analytes with wide-ranging volatilities without causing thermal degradation, The SPME-TPD method was linear over 2-3 orders of magnitude with an electron capture detector and detection limits were in the submicrogram per liter range, Precision and detection limits for selected trihalomethanes were comparable to those of EPA method 551. Extraction efficiencies were not affected by the presence of 10 mg/L soap, 15 mg/L sodium iodide, and 6000 mg/L sodium thiosulfate, The SPME-TPD technique was applied to the determination of iodination disinfection byproducts from individual precursor compounds using GC/MS and to the quantitation of iodoform at trace levels in a water recycle system using GC/ECD.
(103) Study of erythromycin A decomposition products in aqueous solution by solid-phase microextraction liquid chromatography tandem mass spectrometry AU: Volmer_DA, Hui_JPM NA: MERCK KGAA,CENT RES ANAL,FRANKFURTER STR 250,D-64271 DARMSTADT,GERMANY NATL RES COUNCIL CANADA,INST MARINE BIOSCI,HALIFAX,NS B3H 3Z1,CANADA JN: RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 1998, Vol.12, No.3, pp.123-129 IS: 0951-4198 DT: Article AB: The decomposition of erythromycin A (EA) in aqueous solution was examined in the pH range 2-13 by means of combined solid- phase microextraction (SPME) and liquid chromatography/electrospray ionization tandem mass spectrometry. Degradation of EA, especially at lower pH values (pH less than or equal to 3), was very rapid and yielded a wide variety of decomposition products. Identification of these degradation products was achieved by means of tandem mass spectrometry in the product ion and precursor ion scan modes. Anhydroerythromycin A was shown to be the major reaction product in both acidic and basic solutions, Among the different SPME fibers investigated for extraction from aqueous solutions, polydimethylsiloxane/divinylbenzene exhibited the best performance for EA and its degradation products.
(104) Evaluation of solid-phase microextraction for analysis of volatile metabolites produced by staphylococci AU: Vergnais_L, Masson_F, Montel_MC, Berdague_JL, Talon_R NA: INRA,RECH VIANDE STN,F-63122 ST GENES CHAMPANE,FRANCE JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1998, Vol.46, No.1, pp.228-234 IS: 0021-8561 DT: Article AB: The evaluation of solid-phase microextraction (SPME) for analysis of flavor compounds produced by bacteria has been studied. First, it was necessary to determine the optimal conditions to extract the different volatile compounds in dilute aqueous solutions. For this, the effects of salt, headspace, and liquid samplings and two coating phases [poly(dimethylsiloxane) (PDMS) and poly(acrylate) (PA)] were tested. The addition of salt enhanced SPME absorption of all the compounds. Ethyl ester was better extracted in liquid sampling with PDMS phase, whereas all of the other compounds were better extracted in headspace sampling at 80 degrees C with PA phase. The SPME technique was applied to the analysis of bacterial metabolites. It has been shown that Staphylococcus xylosus (16) and Staphylococcus carnosus (833) were able to produce esters and to catabolize leucine and that S. carnosus (833) limited the oxidation of free fatty acids.
(105) Water solubility and octanol/water-partitioning of hydrophobic chlorinated organic substances determined by using SPME/GC AU: Paschke_A, Popp_P, Schuurmann_G NA: UFZ,ENVIRONM RES CTR,DEPT CHEM ECOTOXICOL,PERMOSERSTR 15,D- 04318 LEIPZIG,GERMANY UFZ,ENVIRONM RES CTR,DEPT ANAL CHEM,D-04318 LEIPZIG,GERMANY JN: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY, 1998, Vol.360, No.1, pp.52-57 IS: 0937-0633 DT: Article AB: The critical step in the determination of water solubilitiy (S- W) and octanol-water partition coefficient (K-OW) of hydrophobic organic chemicals by using the generator-column technique and the slow-stirring procedure, respectively, is the exact quantification of the low water-phase concentrations of the substances under investigation. We have tested the applicability of solid-phase microextraction (SPME) and gas chromatography with seven chlorinated organic compounds, The substances cover a S-W range from 500 mg/L to 7 ng/L and a log K-OW range from 3 to 8. The results show that SPME can be a valuable alternative to common preconcentration techniques in the quantification of hydrophobic organics in pure and octanol- saturated water, The apparent SPME distribution constants K- SPME (obtained with the 100 mu m-PDMS fiber for analyte's partitioning between fiber coating and aqueous sample) do not correlate directly with octanol/water partition coefficients and thus cannot be recommended as a surrogate parameter for K- OW.
(106) Determination of aromatic amines by solid-phase microextraction and gas chromatography mass spectrometry in water samples AU: Muller_L, Fattore_E, Benfenati_E NA: MARIO NEGRI INST PHARMACOL RES,VIA ERITREA 62,I-20157 MILAN,ITALY JN: JOURNAL OF CHROMATOGRAPHY A, 1997, Vol.791, No.1-2, pp.221-230 IS: 0021-9673 DT: Article AB: Solid-phase microextraction (SPME) in gas chromatography-mass spectrometry (GC-MS) has been introduced as a rapid and sensitive quantitative method for the detection of some aniline derivatives (o-toluidine, p-chloroaniline, 2,4-dichloroaniline, 2,5-dichloroaniline, 3,4-dichloroaniline and 3,5- dichloroaniline) in environmental water samples. Many parameters for optimisation of the extractive method, such as linearity, sensitivity, equilibration time, precision, and different operating conditions (pH, salt) have been evaluated. After a comparison of the commercially available SPME fibers, a carbowax-divinylbenzene 65 mu m polymeric phase was chosen. Linearity was excellent in the concentration range 0.05-5 mu g/l, and the method showed good reproducibility (coefficient of Variation of around 5%). The detection limits differ substantially for the various compounds analysed, but all were below any other limit of detection for these compounds in the literature. The addition of salt (sodium chloride) at pH 7.6 significantly improved the amount of analytes extracted by the fiber. Operating under basic conditions (pH 11), we did not observe a better sensitivity of the method. To evaluate its applicability on a real aqueous matrix, various groundwater samples collected in an industrially polluted area north of Milan, Italy, were analysed.
(107) Strategies for the analysis of polar solvents in liquid matrixes AU: Gorecki_T, Martos_P, Pawliszyn_J NA: UNIV WATERLOO,DEPT CHEM,WATERLOO,ON N2L 3G1,CANADA UNIV WATERLOO,WATERLOO CTR GROUNDWATER RES,WATERLOO,ON N2L 3G1,CANADA JN: ANALYTICAL CHEMISTRY, 1998, Vol.70, No.1, pp.19-27 IS: 0003-2700 DT: Article AB: Various approaches to the analysis of polar compounds in different matrixes by solid-phase microextraction (SPME) were studied. The analysis of polar analytes in nonpolar matrixes was performed with custom-made SPME fibers coated with Nafion perfluorinated resin, The sensitivity of this fiber in this type of analysis was better by 1 order of magnitude on average as compared to those of any of the commercially available fibers, The fiber was the most sensitive for the most polar of the compounds studied, i.e., methanol. Determination of methanol, ethanol, and 2-propanol in unleaded gasoline was illustrated. Except for methanol, the fiber did not perform very well in the analysis of alcohols in water, The fiber was capable of extracting water from benzene, SPME analysis of polar compounds in water was studied using aqueous solutions of acetone, methyl ethyl ketone, methyl isobutyl ketone (MIBK), 2- propanol, 2-methyl-2-propanol, and tetrahydrofuran. Fibers coated with poly(dimethylsiloxane)/ divinylbenzene yielded the highest sensitivity in this type of analysis. Low-or sub-ppb detection limits were obtained for all the analytes with FID detection when the samples were saturated with NaCl. Since fibers of this type extract analytes by adsorption rather than absorption, nonlinear responses were observed when all the analytes were allowed to equilibrate because of the limited number of adsorption sites on the surface of the coating and displacement of compounds with low distribution ratios by compounds with high distribution ratios (mainly MIBK), Two approaches allowed a significant improvement in linearity: extraction of a vigorously stirred sample for a short time, or extraction under static conditions for a time much shorter than that required for equilibration of all the analytes. In both cases the amount of MIBK extracted was significantly reduced, while the remaining analytes were affected to a much lesser degree. The sensitivity of acetone determination was greatly improved by in-solution derivatization with o-(2,3,4,5,6- pentafluorobenzyl)hydroxylamine hydrochloride and extraction of the oxime formed.
(108) Inter-laboratory studies for the validation of solid-phase microextraction for the quantitative analysis of volatile organic compounds in aqueous samples AU: Nilsson_T, Ferrari_R, Facchetti_S NA: COMMISS EUROPEAN COMMUNITIES,JOINT RES CTR,INST ENVIRONM,I- 21020 ISPRA,VA,ITALY SUPELCHEM,I-20129 MILAN,ITALY JN: ANALYTICA CHIMICA ACTA, 1997, Vol.356, No.2-3, pp.113-123 IS: 0003-2670 DT: Article AB: Inter-laboratory studies were organised with the participation of twenty laboratories for the purpose of validation of a new standard method using solid-phase microextraction (SPME) for the quantitative analysis of volatile organic compounds (VOCs) in aqueous samples. The statistical evaluation of the accuracy and precision of SPME was performed in accordance with the ISO standard concerning inter-laboratory studies on the basis of reference material and by comparison with the usual purge-and- trap and static headspace techniques. Comparable repeatability, reproducibility and accuracy were found with the SPME standard and the reference methods. Better precision of SPME was obtained by extraction from a small headspace over the aqueous phase than with the fibre immersed in water. The linearity was good in all cases and detection limits were in the low ng/l range. Thus, it is concluded that SPME is a valid alternative technique for the analysis of VOCs at trace level in various aqueous samples.
(109) Trace determination of pesticides in water by coated capillary micro extraction (CCME) and reversed-phase high performance liquid chromatography AU: Hartmann_H, Burhenne_J, Spiteller_M NA: UNIV KASSEL,DEPT ECOL CHEM & ECOTOXICOL,NORDBAHNHOFSTR 1A,D- 37213 WITZENHAUSEN,GERMANY JN: FRESENIUS ENVIRONMENTAL BULLETIN, 1998, Vol.7, No.1-2, pp.96- 103 IS: 1018-4619 DT: Article AB: A method for the automated online-CCME/HPLC aqueous samples is described. The enrichment of the analyte proceeds in tailor- made fused silica capillaries coated on the inside with polysilicone acrylate. The adsorption of triazines and phenylureas was optimized by varying several parameters resulting in determination limits below 200 ng/L.
(110) Investigations on wine bouquet components by solid-phase microextraction-capillary gas chromatography (SPME-CGC) using different fibers AU: Garcia_DDC, Reichenbacher_M, Danzer_K, Hurlbeck_C, Bartzsch_C, Feller_KH NA: UNIV JENA,INST ANORGAN & ANALYT CHEM,D-6900 JENA,GERMANY FACHHSCH JENA,FACHBEREICH MED TECH,JENA,GERMANY JN: HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY, 1997, Vol.20, No.12, pp.665-668 IS: 0935-6304 DT: Article AB: The extraction of wine bouquet components with solid-phase microextraction (SPME) using different fibers was studied. Polyacrylate fibers (PA-85) achieve the most complete bouquet profiles, About ninety substances were identified by capillary gas chromatography-MS and their retention factors were calculated to allow peak identification in capillary-GC-FID chromatograms. The terpene profiles of different nines were recorded by SPME (PA-85)-CGC-FID.
(111) Characterization of roasted coffee and coffee beverages by solid phase microextraction - Gas chromatography and principal component analysis AU: Bicchi_CP, Panero_OM, Pellegrino_GM, Vanni_AC NA: DIPARTIMENTO SCI & TECNOL FARMACO,VIA P GIURIA 9,I-10125 TURIN,ITALY LAVAZZA SPA,I-10156 TURIN,ITALY JN: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1997, Vol.45, No.12, pp.4680-4686 IS: 0021-8561 DT: Article AB: A method that differentiates between different roasted coffees and coffee beverages is described. Characterization is achieved by applying principal component analysis (PCA) to the chromatographic results obtained by solid phase microextraction-gas chromatography (SPME-GC), applied to the vapor phase in equilibrium with coffee (HS-SPME), or to coffee extracts (LS-SPME). The capabilities of this method are illustrated by some examples defining the differentiation of coffee samples of different origins or in mixtures of different compositions. KP: HPLC-UV, FIBERS
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