共查询到20条相似文献,搜索用时 15 毫秒
1.
U. Ceglarek J. Efer A. Schreiber E. Zwanziger W. Engewald 《Analytical and bioanalytical chemistry》1999,365(8):674-681
The use of Solid Phase Microextraction (SPME) for the qualitative and quantitative determination of Linear Alkylbenzenesulfonates (LAS) in waste water samples was investigated. A Carbowax/Templated Resin (CW/¶TPR) coated fiber was directly immersed into influent and effluent samples of a sewage treatment plant (STP). Extraction conditions such as time, pH, ion strength were investigated. The extracted LAS were desorbed with a solvent in a specially designed SPME-LC interface for analysis with HPLC-FLD and Electrospray Ionization Mass Spectrometry (ESI-MS). The combination of SPME with ESI-MS proved to be an alternative technique for the LAS determination in waste water. Linear ranges of the external calibration were found from 0.5–100 ng/mL, with detection limits of 0.5 ng/mL for each individual LAS homologue. The reproducibility of the method is 15% (relative standard deviation). 相似文献
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SPME-GC联用测定环境水样中的酚类化合物 总被引:1,自引:0,他引:1
建立了固相微萃取与气相色谱联用技术测定环境水样中酚类化合物的方法. 探讨了pH、离子强度、萃取头类型、萃取时间以及解析时间等条件对酚类化合物萃取量的影响, 优化了GC仪器条件. 在优化的条件下, 酚类化合物的响应值与浓度有良好的线性关系, 线性范围为0.20~200 μg/L, 检出限在0.019~0.10 μg/L之间, 相对标准偏差(RSD, n=5)为4.4%~11%, 水样平均加标回收率为92.2%~101.9%, 所建立的方法可测定环境水样中的酚类化合物. 相似文献
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Summary Solid phase microextraction was coupled with gas chromatography-mass spectrometry (SPME-GC-MS) to screen for sixteen nitrogen-containing
compounds, including herbicides, in water samples. The effects of stirring, extraction time, pH, salt concentration and the
choice of fiber coating material were evaluated. The repeatability was in the range of 0.72–18.2 (CV % at 200 ng·L−1) and the reproducibility, in the range of 5.4–34 (at 500 ng·L−1). 相似文献
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Liquid-phase microextraction (LPME) coupled with gas chromatography-flame ionization detection is applied to the analysis of phenolic compounds (phenol, o-cresol, m-cresol, 2,4-dimethylphenol, 2,3- dimethylphenol, and 3,4-dimethylphenol) in water samples. Experimental parameters affecting the extraction efficiency (including extraction solvent and drop volume, stirring rate, extraction time, temperature, salt concentration, and pH) are investigated and optimized. The developed protocol yields a good linear calibration curve from 5 or 20 to 10000 microg/L for the target analytes. The limits of detection are in the range of 0.94 to 1.97 microg/L, and the relative standard deviation is below 9.37%. The established method is applied to determine the phenolic pollutants in real wastewater samples from a coking plant. The recoveries of the phenolic compounds studied are from 92% to 102%, suggesting the feasibility of the LPME method for the determination of the phenolic compounds in wastewater. 相似文献
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Anna TyburskaKrzysztof Jankowski Agnieszka Rodzik 《Spectrochimica Acta Part B: Atomic Spectroscopy》2011,66(7):517-521
A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL− 1, respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples. 相似文献
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为全面了解小米黄酒风味成分的构成和气味特征,优化了85μm聚丙烯酸酯(PA)、100μm聚二甲基硅氧烷(PDMS)、75μm碳分子筛(CAR)/PDMS、50/30μm二乙烯基苯(DVB)/CAR/PDMS萃取头提取小米黄酒风味成分的条件,采用顶空固相微萃取(headspace solid phase microextraction,HS-SPME)-气相色谱-质谱法(GC-MS)对风味成分进行定性、定量分析,并计算气味活性值(odor active value,OAV),同时利用OAV分析风味成分的气味特征和气味强度。结果显示:不同萃取头的最优萃取条件为样品量8 mL、萃取时间40 min、萃取温度60℃、NaCl添加量1.5 g。小米黄酒风味成分由醇、酯、含苯化合物、烃、酸、醛、酮、烯、酚和杂环类化合物构成,醇为主要风味成分。通过OAV确定了苯乙醇、苯乙烯、2-甲基萘、1-甲基萘、苯甲醛、苯乙醛、2-甲氧基-苯酚为小米黄酒气味特征成分,苯基乙醇、苯乙醛对气味贡献最大。PA和PDMS萃取头分别对极性和非极性化合物具有较好的吸附效果,CAR/PDMS和DVB/CAR/PDMS萃取头对中等极性化合物具有较好的吸附效果。该研究全面了解了小米黄酒风味成分的构成,为其产品开发及品质控制提供理论了依据。 相似文献
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Determination of diethylhexyl phtalate in water by solid phase microextraction coupled to high performance liquid chromatography 总被引:3,自引:0,他引:3
Difficulties detected in the determination of the diethylhexylphthalate (DEHP) at trace levels by gas chromatography–mass spectrometry (GC–MS) using SPME, due to its ubiquitous distribution in the environment has been overcome and a new method for the determination of DEHP in drinking water has been proposed. The method is based on solid phase microextraction (SPME) coupled to high-performance liquid chromatography (HPLC). Detection was carried out spectrophotometrically. Calibration graph was linear in the range 10–110 μg/L with a regression coefficient of r2 = 0.998 and a detection limit of 0.6 μg/L. The relative standard deviation was 5 and 2% (n = 4) for chromatographic areas and retention times, respectively. The usefulness of the SPME–HPLC technique was confirmed. 相似文献
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Solid phase microextraction coupled with high performance liquid chromatography with fluorescence detection has been optimized and evaluated for a simple, rapid, and selective analysis of anatoxin-a. Four kinds of fiber (100 microm polydimethylsiloxane, 60 microm polydimethylsiloxane/divinylbenzene, 50 microm Carbowax/templated resin-100, and 85 microm polyacrylate) were evaluated for an efficient extraction of the toxin. Parameters relating to the desorption step, such as desorption mode, solvent composition, time for both static and dynamic desorption, as well as carryover, have been studied and optimized. The derivatization process was investigated using NBD-F as derivatizing reagent. Anatoxin-a derivative was formed when the anatoxin-a-loaded fiber was inserted in a vial containing 5 microL of NBD-F. Variables affecting extraction such us ionic strength, temperature, and time have been also optimized. The results obtained showed linearity in the range of 10-2000 ng and a limit of detection of 0.29 ng/mL in river water. The presented method has been applied to different environmental samples. 相似文献
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The determination of carbamate and triazine pesticides from soil leachates and slurries was investigated using solid phase microextraction (SPME) coupled to high-performance liquid chromatography-electrospray/ mass spectrometry (HPLC-ESI/MS). SPME was carried out using fibres with a newly developed 50 μm Carbowax/ template coating which are suitable for relatively polar analytes. These fibers exhibit precisions better than 10% RSD, and are resistant against high contents of organic solvents during desorption. The technique shows a high sampling frequency resulting in an increasing sample throughput. 相似文献
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M. M?der P. Popp R. Eisert J. Pawliszyn 《Fresenius' Journal of Analytical Chemistry》1999,363(7):680-685
The determination of carbamate and triazine pesticides from soil leachates and slurries was investigated using solid phase
microextraction (SPME) coupled to high-performance liquid chromatography-electrospray/ mass spectrometry (HPLC-ESI/MS). SPME
was carried out using fibres with a newly developed 50 μm Carbowax/ template coating which are suitable for relatively polar
analytes. These fibers exhibit precisions better than 10% RSD, and are resistant against high contents of organic solvents
during desorption. The technique shows a high sampling frequency resulting in an increasing sample throughput.
Received: 17 December 1997 / Revised: 30 October 1998 / Accepted: 10 November 1998 相似文献
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A simple and sensitive method for the determination of amphetamine, methamphetamine and their methylenedioxy derivatives in urine and hair samples was developed by coupling automated in-tube solid phase microextraction (SPME) to high performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-ES-MS). To achieve optimum performance, the conditions for both the in-tube SPME and the ES-MS detection were investigated. ES-MS detection conditions were studied by flow injection analysis (FIA) with direct liquid injection. In-tube SPME conditions were optimized by selecting the appropriate extraction parameters, including capillary stationary phases and sample pH. For the compounds studied, a custom-made polypyrrole (PPY) coated capillary showed superior extraction efficiency as compared to commercial capillaries. Therefore, the PPY coated capillary was selected for in-tube SPME in this study. The calibration curves of stimulants were linear in the range from 0.1 to 100 ng ml(-1) with detection limits (S/N=3) of 8-56 ng l(-1). This method was successfully applied to the analysis of the stimulants in spiked human urine and hair samples. 相似文献
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N. Huppert Marion Würtele Hermann H. Hahn 《Fresenius' Journal of Analytical Chemistry》1998,362(6):529-536
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 μg/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 μg/L.
Received: 13 March 1998 / Revised: 16 June 1998 / Accepted: 19 June 1998 相似文献
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Determination of organotin compounds in-water by headspace solid phase microextraction with gas chromatography-mass spectrometry 总被引:7,自引:0,他引:7
This investigation evaluates headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) to determine trace levels of organotins in water. The organotins were derivatized in situ with sodium tetraethylborate and adsorbed on a poly(dimethysiloxane) (PDMS)-coated fused silica fiber. The SPME experimental procedures to extract organotins in water were at pH 5, with extraction and derivatization simultaneously at 45 degrees C for 30 min in a 2% sodium tetraethylborate solution and a sample solution volume in the ratio of 1:1, and desorption in the splitless injection port of the GC at 260 degrees C for 2 min. Detection limits are determined to be in the low ng/L range. According to the analysis, the linearity range is from 10 to 10,000 ng/L with R.S.D. values below 12% except triphenyltin (24%). The proposed method was tested by analyzing surface seawater from the harbors on the Taiwanese coast for organotins residues. Some organotins studied were detected in the analyzed samples. Results of this study demonstrate the adequacy of the headspace SPME-GC-MS method for analyzing organotins in sea water samples. 相似文献
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N. Huppert Marion Würtele Hermann H. Hahn 《Analytical and bioanalytical chemistry》1998,362(6):529-536
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 μg/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 μg/L. 相似文献
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Summary 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 wet 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., nornicotines, myosmine,
anabasine and anatabine) were separated with baseline resolution within 3 min. The detection limits for these alkaloids are
below 0.1 μg 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. 相似文献
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