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Results for “Solid Phase Microextraction”

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At least 325 records · Page 18Linked to original sources

PubMed2002

Hydroxyfullerene as a novel coating for solid-phase microextraction fiber with sol-gel technology.

Hydroxyfullerene (fullerol) as a novel coating for solid-phase microextraction (SPME) fiber was first prepared by a sol-gel technology. The coating procedure involving sol solution composition and conditioning process was presented. A fullerene polysiloxane surface-bonded porous coating on the fused-silica fiber surface was obtained and confirmed by IR spectra and scanning electron microscopy. The coating has stable performance at high temperature (even to 360 degrees C) and solvents (organic and inorganic) because of the properties of fullerene and the chemical binding between the coating and the fiber surface. The extraction properties of the new coatings to less volatile organic compounds, such as polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons and polar aromatic amines were investigated using headspace SPME coupled with GC-electron-capture detection and GC-flame ionization detection. In addition, compared with commercial SPME stationary phases, the new coatings showed higher sensitivity, faster velocities of mass transfer for aromatic compound, and possessed planarity molecular recognition for PCBs. Moreover, this fiber was firm, inexpensive, durable and can be prepared simply. The fiber-to-fiber reproducibility was very good.

Chromatography↗

PubMed2003

Trace analysis of technical nonylphenol, bisphenol A and 17alpha-ethinylestradiol in wastewater using solid-phase microextraction and gas chromatography-mass spectrometry.

To enable high sample throughput, an automated solid-phase microextraction (SPME) method coupled with GC-MS for the trace analysis of technical nonylphenol, bisphenol A and 17alpha-ethinylestradiol was developed. The extraction performance of different SPME fibre coatings was examined, with polyacrylate proving most suitable. Although study of the extraction time showed that the analytes have not reached equilibrium after 3 h, as a compromise an extraction time of 1 h was applied in all the experiments with detection limits between 0.04 and 1 microg l(-1) for wastewater effluent. The mean reproducibility of the technique is 8% RSD. Carry-over effects are negligible. The linearity of calibration curves ranges over three orders of magnitude. The method was tested for determining the analytes in influents and effluents of constructed wetland plants and in model wastewater used in laboratory experiments.

Benzhydryl Compounds↗

PubMed2003

Application of isotope dilution to the determination of methylmercury in fish tissue by solid-phase microextraction gas chromatography-mass spectrometry.

Species-specific isotope dilution (ID) calibration using solid-phase microextraction (SPME) in combination with gas chromatography-mass spectrometry (GC-MS) for separation and detection of methylmercury (MeHg) in fish tissue is described. Samples were digested with methanolic potassium hydroxide. Analytes were propylated and headspace sampled with a polydimethylsiloxane-coated SPME fused-silica fiber. ID analysis was performed using a laboratory-synthesized 198Hg-enriched methylmercury (Me 198Hg) spike. Using selective ion monitoring (SIM) mode, the intensities of Me 202HgPr+ at m/z 260 and Me 198HgPr+ at m/z 256 were used to calculate the m/z ratio at 260/256, which was used to quantify MeHg in NRCC CRM DORM-2 fish tissue. A MeHg concentration of 4.336 +/- 0.091 microg g(-1) (one standard deviation, n = 4) as Hg was obtained in DORM-2, in good agreement with the certified value of 4.47 +/- 0.32 microg g(-1) (95% confidence interval). A concentration of 4.58 +/- 0.31 microg g(-1) was determined by standard additions calibration using ethylmercury (EtHg) as an internal standard. The three-fold improvement in the precision of measured MeHg concentrations using ID highlights its superiority in providing more precise results compared to the method of standard additions. A method detection limit (3 S.D.) of 0.037 microg g(-1) was estimated based on a 0.25 g subsample of DORM-2.

Animals↗

PubMed2000

Analysis of biogenic amines by solid-phase microextraction and high-performance liquid chromatography with electrochemical detection.

We investigated the new solid-phase microextraction method by high-performance liquid chromatography with electrochemical detection for the analysis of biogenic amines. The Carbowax-Templated Resin 50 microm (purple) fibre coating offers good performances for dopamine and serotonin separation, i.e., good selectivity and high sensibility (0.1 microg l(-1)). We also tested this fibre for biogenic amines quantification of rat striatum. The coating seems to be selective towards the amines and has low affinity for the metabolites, allowing a good separation and preventing drawbacks from the biological matrix. These first results obtained using this original separation method offer large perspectives of application to many biological samples.

Animals↗

PubMed2001

A rapid and sensitive method for methyl tert-butyl ether analysis in water samples by use of solid phase microextraction and gas chromatography-mass spectrometry.

This work describes a rapid and sensitive solid-phase microextraction (SPME) method for the isolation and analysis of methyl tert-butyl ether in water samples. Methyl tert-butyl ether was extracted from aqueous solutions using SPME fibre coated with Divinylbenzene/Carboxen/polydimethylsiloxane (30 microm film thickness) and analysed by GC-MS with a Hewlett Packard 6890/5973 system equipped with a capillary column coated with Vocol (30 m x 0.25 mm, 1.5 microm film thickness). Extraction parameters and chromatographic separation conditions were optimised. The developed method showed good analytical performance in terms of precision (RSD between 2% and 8%) and accuracy (mean recovery from 96% to 104%) with a detection limit of 14 ppt. Finally the method was applied to surface, tap and commercial mineral water samples, as well as snow samples collected along a busy road of Bologna town area. The median concentration of methyl tert-butyl ether in all these samples (0.05-0.4 ppb) was well below the maximum aqueous contamination levels in water adopted in the United States (13 ppb).

Carcinogens↗

PubMed1997

Aqueous alkylchloroformate derivatisation and solid-phase microextraction: determination of amphetamines in urine by capillary gas chromatography.

The alkylchloroformate derivatisation and solid-phase microextraction of amphetamine and methamphetamine directly in urine samples prior to capillary gas chromatographic analysis is described. The alkylchloroformate reagent was added to the urine sample, which was adjusted to pH 10.8, and an internal standard was added. The resulting products were water-stable carbamates that were extracted without organic solvent. The polydimethylsiloxane coated fibre was inserted into the modified sample and agitated for 14 min. The fibre with the extracted derivatisation products was injected into the capillary gas chromatograph. The extracted carbamates were evaporated at 300 degrees C in the split-splitless injection port of the gas chromatograph, separated on a methylsilicone capillary column and detected by either a nitrogen-phosphorus detector or by mass spectrometry. The method was shown to be reproducible with a detection limit of 50 ng/ml of amphetamine and methamphetamine in urine.

Amphetamine↗

PubMed2003

Solid-phase microextraction of volatile compounds from the chopped leaves of three species of Eucalyptus.

Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography and ion-trap mass spectrometry has been used to identify biogenic volatile organic compounds present in the headspace of chopped leaves of Eucalyptus (E.) dunnii, E. citriodora, and E. saligna. A simple HS-SPME method entailing 30 min of extraction at 30 degrees C was developed for this purpose. Thirty compounds were identified in the headspace of 60 juvenile chopped Eucalyptus leaves, and another 30 were tentatively identified. The presence of compounds such as (E)-4,8-dimethyl-1,3,7-nonatriene (DMNT), (E,E)-4,8,12-trimethyl-1,3,7,11-tridecatetraene (TMNT), (E,E)-alpha-farnesene, (E,E,E)-3,7,11,15-tetramethyl-1,3,6,10,14-hexadecapentaene (TMHP), beta-caryophyllene, alpha-humulene, germacrene D, and beta-cubebene in the headspace of the leaves but not in the essential oils from the same Eucalyptus trees and information about the infochemical roles of some of these compounds in other living plant systems suggest they might play a bioactive role in Eucalyptus leaves.

Eucalyptus↗

PubMed2003

Microwave-assisted headspace solid-phase microextraction for the analysis of bioemissions from Eucalyptus citriodora leaves.

Microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) was developed as a simple and effective method for fast sampling of volatile organic compounds (VOCs) from Eucalyptus citriodora Hook (E. citriodora) leaves. During microwave heating, a simple shielding device made of aluminum foil was used to protect the SPME fiber from microwave irradiation while allowing the sample to be heated. A room temperature water bath was also used to allow microwave heating to be conducted in a more controlled manner. The inner heating caused by microwave irradiation dramatically accelerated the emission of VOCs from the sample, but no marked change in headspace temperature in the sample vial was found. Under optimum conditions, the extraction efficiencies obtained with microwave heating were much higher than those obtained without microwave heating for all fibers used, namely, 7-microm polydimethylsiloxane (PDMS), 100-microm polydimethylsiloxane (PDMS), 65-microm polydimethylsiloxane/divinylbenzene (PDMS/DVB), and 75-microm carboxen/polydimethylsiloxane (CAR/PDMS). The improvement of extraction efficiency using MA-HS-SPME allowed more VOC events to be detected, with more balanced extraction of VOCs of lower and higher molecular masses. Moreover, a good linear relationship was found between sample size and GC-FID response (total peak area of VOCs), indicating the usefulness of MA-HS-SPME for quantitative analysis of individual volatile compounds in E. citriodora leaves.

Chromatography, Gas↗

PubMed2000

Direct coupling of microcolumn liquid chromatography with in-tube solid-phase microextraction for the analysis of antidepressant drugs.

The direct coupling of in-tube solid-phase microextraction (in-tube SPME) with microcolumn liquid chromatography (micro-LC) has been investigated for the analysis of antidepressants in human urine. The use of in-tube SPME has been clearly shown to be advantageous for the on-line coupling of the SPME method, as the sample pretreatment technique, with micro-LC as the separation technique. This is because much smaller amounts of the sample solutions, desorption solvents and the mobile phase are required compared with conventional SPME-LC systems. The parameters for preconcentration have been investigated for the extraction capillary with the newly developed 'wire-in-tube' configuration.

Antidepressive Agents↗

PubMed2002

A new procedure for solid-phase microextraction using a flow-through system with air segmentation.

Three different procedures for solid-phase microextraction (SPME) of trace organic compounds from liquids were evaluated: simple extraction with magnetic stirring, use of a laboratory-made flow-through extraction cell and a new system based on a laboratory-made flow-through extraction cell in which the sample stream is segmented with air bubbles. In this new procedure, the sample flows through the cell as a regular sequence of small plugs separated by air bubbles instead of in a continuous stream. This new system combines the advantages of SPME, as a simple, fast, sensitive and solvent-free sample concentration/introduction technique, with the advantages of on-line processing of aqueous sample as a less time-consuming, efficient and continuous technique. For testing the new flow-through procedure, a mixture of phthalate esters was used for direct absorption from an aqueous solution with a 100 microm polydimethylsiloxane fiber. The efficiency and precision of the procedure were compared with those of extraction with magnetic stirring and the usual flow-through cell concept. The results indicate better contact of the analytes with the extraction film when the air-segmented flow-through extraction cell is employed.

Journal Article↗

PubMed2000

Solid phase microextraction of volatile constituents from individual fresh Eucalyptus leaves of three species.

Methyl polysiloxane solid-phase microextraction fibres were used for ten minutes to adsorb volatile constituents from headspace above all or part of a single cut up fresh eucalyptus leaf kept warm at 37 degrees C. The fibres were desorbed at 200 degrees C for programmed gas chromatography (40-187 degrees C) on a methyl polysiloxane capillary. Substances were identified by mass spectra and/or authentic sample retention. Results do not correspond to published values for steam distilled oils, being richer in sesquiterpenes, of which three are common to three different species; and also in esters in two species. Five Eucalyptus citriodora leaves from the same tree over different months gave very similar analyses to a fibre in 10 min of 72.9-80.5% citronellal, 3.5-5.4% citronellol, 1.0-3.8% citronellyl acetate, 9.2-11.8% caryophyllene and 1.4-1.7% bicyclogermacrene. Six E. nicholii leaves yielded 67.2-73.7% cineole and 4.6-9.7% limonene along with 10.5-16.5% sesquiterpenes, mostly hydrocarbons, particularly bicyclogermacrene. E. globulus leaves gave only 54.0-61.3% cineole, with 19.5-24.3% alpha-pinene, 6.7-9.1% limonene and 2.1-5.4% alpha-terpinyl acetate; along with 3.6-7.7% sesquiterpenes, particularly aromadendrene, but no bicyclogermacrene.

Chromatography, Gas↗

PubMed2006

Determination of 17 kinds of banned organochlorine pesticides in water by activated carbon fiber-solid phase microextraction coupled with GC-MS.

Activated carbon fiber (ACF) as extraction fiber for solid-phase microextraction (SPME) and its application for the analysis of banned organochlorine pesticides (OCPs) were investigated. Firstly, ACF was activated by different concentration of zinc chloride, which indicated that ACF activated by 60% zinc chloride had a reasonable specific surface area, pore volume and pore distribution. Secondly, the parameters for the ACF-SPME procedure, the adsorption and desorption conditions, were also optimized when coupled with gas chromatography-mass spectrometry (GC-MS). Thirdly, the ACF-SPME was used to analyze 17 kinds of OCPs in water. The linearity of most pesticides was found to be between 0.2 and 50 microg/l with GC-MS under the selected ion monitoring (SIM) acquisition mode. The limits of detection (LOD) at the sub microg/l were obtained. The work demonstrated here shows that ACF is a promising alternative for the SPME procedure.

Carbon↗

PubMedDate not supplied

Determination of volatile residual solvents in traditional Chinese medicines by headspace solid-phase microextraction and cryogenic gas chromatography with flame ionization detection.

A method based on headspace solid-phase microextraction and cryogenic gas chromatography with flame ionization detection was developed for the determination of volatile residual solvents in traditional Chinese medicines. A laboratory-made cryogenic chromatographic system was used for the separation of 15 kinds of residual solvents. During the analysis, a 65 microm PDMS/DVB fiber was used to extract the residual solvents, the extraction time was controlled at 0 degrees C for 15 min, and the NaCl content of the sample was maintained at 30%. The limits of detection ranged from 0.08 (for octane) to 5000 microg/L (for ethanol), and the relative standard deviations were < 8%. The recoveries from spiked samples ranged from 88 to 112%. Trace levels of residual solvents in several traditional Chinese medicines were effectively identified and quantified.

Calibration↗

PubMedDate not supplied

Optimization of solid-phase microextraction for the gas chromatography/mass spectrometry analysis of persistent organic pollutants.

In this work, solid-phase microextraction (SPME) has been applied as an alternative for the selective extraction of 3 polybrominated diphenyl ethers (PBDEs), 2,2',4,4'-tetrabromodiphenyl ether (PBDE-47); 2,2',4,4',5-pentabromodiphenyl ether (PBDE-99); and 2,2',4,4',6-pentabromodiphenyl ether (PBDE-100), and 2 alkylphenols, 4-tert-OP and 4-NP, prior to their analysis by gas chromatography/mass spectrometry (GC/MS). The advantages of this technique are mainly its simplicity, cost-effectiveness, and time-saving sample preparation, as well as being a solvent-free technique. With the aim of optimizing the conditions for an efficient extraction of the studied compounds, different fiber coatings and the main parameters affecting the extraction procedure have been evaluated. The results obtained showed a good linearity in the range of concentrations investigated, and adequate relative standard deviation values were found according to the range accepted for SPME. Recovery values were in the range of 78-108%, and good detection and quantitation limits at ppt levels were obtained for both methods, allowing the determination of the selected compounds in samples at trace levels. The results obtained clearly show the potential of SPME for efficient concentration of the target compounds and also demonstrate the reliability of this extraction technique for their GC/MS analysis.

Chromatography, High Pressure Liquid↗

PubMed2005

Coupling of solid-phase microextraction and capillary isoelectric focusing with laser-induced fluorescence whole column imaging detection for protein analysis.

A coupling method of solid-phase microextraction (SPME) and capillary isoelectric focusing (CIEF) with laser-induced fluorescence (LIF) whole column imaging detection (WCID) was developed for the analysis of proteins. Unlike other liquid-phase separation methods and conventional CIEF, proteins are focused into stationary bands within a pH gradient in CIEF-WCID. Thus, CIEF-WCID is the most compatible liquid-phase separation method for coupling with SPME, which can effectively resolve the problems associated with the slow desorption kinetics of SPME in a liquid phase. By combining SPME and CIEF-WCID, the desorption time can be as long as necessary, allowing complete desorption without any band broadening and analyte carryover. By using this method, R-phycoerythrin in water can be extracted by SPME in 10 min, and subsequently analyzed by CIEF-LIF-WCID within 20 min, providing a limit of detection of 3.5 x 10(-12) M (S/N = 3). The feasibility of the SPME-CIEF-LIF-WCID method was demonstrated by extracting and analyzing extracellular phycoerythrins in cultured cyanobacteria samples. Extracellular phycoerythrins at the nanomolar level were extracted and analyzed in 30 min, while avoiding the interference of the cyanobacteria cells.

Fluorescence↗

PubMed2002

[Determination of methanol and fusel oils in alcohol beverages using headspace solid-phase microextraction and gas chromatography].

A method for the determination of methanol and fusel oils in alcohol beverages using headspace solid-phase microextraction and gas chromatography (HS-SPME-GC) is presented. The solid phase was a coated epoxy resin. The extraction and chromatography conditions were optimized. Limits of detection were 0.02 mg/L-0.04 mg/L and relative standard deviations were in the range of 1.4%-4.1%. The proposed method showed better sensitivity in comparing with direct headspace gas chromatography(HS-GC, the National Standard method). This method was applied to evaluate real samples. The spiked recoveries in beer, wine and functional alcohol samples ranged from 80.8% to 110.3% for methanol and fusel oils. The results by HS-SPME-GC and HS-GC for alcohol samples coincided very well. The proposed method is simple, fast and accurate with high reproducibility, high sensitivity and low cost. It extends the applications of SPME.

Alcoholic Beverages↗

PubMed2007

Micellar solid-phase microextraction for determining partition coefficients of substituted polycyclic aromatic hydrocarbons in micellar media: possible prediction of hydrocarbon-micelle behaviour.

Micellar solid-phase microextraction (MSPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been used to obtain partition coefficients of a group of 18 substituted aromatic hydrocarbons to ionic and nonionic micelles. Statistical and factor analyses have been utilized to establish some general equations relating molecular descriptors of non-substituted polycyclic aromatic hydrocarbons and their partition coefficients obtained by MSPME. The obtained equations have correlation coefficients higher than 0.94. They are used to predict hydrocarbon-micelle partition coefficients for a group of hydrocarbons with reported literature values giving a correlation coefficient of 0.98 and a standard deviation of the prediction of 0.182. The predictive model was also applied to substituted polycyclic aromatic hydrocarbons with partition coefficient values obtained by MSPME, with a 69% level of success.

Calibration↗

PubMed2001

Solid-phase microextraction versus single-drop microextraction for the analysis of nitroaromatic explosives in water samples.

This paper compares solid-phase microextraction (SPME) with a recently developed extraction method called single-drop microextraction (SDME) for the analysis of nitroaromatic explosives in water samples. The two techniques are examined in terms of procedure, chromatographic analysis and method performance. All practical considerations for both techniques are also reviewed. SPME requires dedicated apparatus and is relatively expensive, as the fiber's lifetime is limited. However, it has the advantages over SDME that it can be easily used for headspace analysis and has lower detection limits for all the target analytes. SDME requires more elaborate manual operations, thus affecting linearity and precision.

Gas Chromatography-Mass Spectrometry↗