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PubMed2004

New trends in sample preparation: on-line microextraction in packed syringe (MEPS) for LC and GC applications Part III: Determination and validation of local anaesthetics in human plasma samples using a cation-exchange sorbent, and MEPS-LC-MS-MS.

The need for on-line sample preparation for high-throughput applications in bioanalysis has increased during the past decade. In this paper a robust and on-line sample preparation technique, micro extraction in packed syringe (MEPS) has been developed and validated. The method is a miniaturized, fully automated, solid-phase extraction (SPE) technique that can be connected on-line to GC or LC without any modification of the chromatographs. The performance of MEPS as sample preparation method is illustrated by the determination of local anaesthetics in human plasma samples on-line with high performance liquid chromatography (HPLC) and tandem mass spectrometry. The sampling sorbent was 1mg silica based benzenesulphonic acid cation exchanger that was inserted in a 250 microl syringe. Ropicavine and two of its metabolites (PPX and 3-OH-ropivacine), lidocaine and bupivacine were used as model substances. The accuracy values of quality control samples (QC) were between 95% and 109%, and precision (relative standard deviation, R.S.D.) had a maximum deviation of 9% for the analytes.

Anesthetics↗
PubMed2006

Study of precursors responsible for off-flavor formation during storage of potato flakes.

Off-flavors frequently appear during the storage of potato flakes. Volatile profile analysis performed by solid-phase microextraction-gas chromatography-mass spectrometry revealed that hexanal is the main compound that appears during the storage period. Hexanal may be a degradation product of linoleic acid formed through linoleic acid hydroperoxide cleavage. Profiles of hexanal precursors were determined from potato flakes at different storage time points. Linoleic acid-derived oxylipins are predominant in potato flakes. The free oxylipins identified, in descending order, are as follows: hexanal, hydroxy polyunsaturated fatty (PUFAs), oxo PUFAs, divinyl ether PUFAs, and hydroperoxy PUFAs. However, the main oxylipins detected were esterified: esterified hydroxy, hydroperoxy, and oxo PUFAs. Oxylipins reveal different evolutions during the storage period. Chiral high-performance liquid chromatography analysis of the precursors of hexanal and other oxylipins revealed a racemic composition that supports the nonenzymatic formation of hexanal and most of the other oxylipins identified.

Aldehydes↗
PubMed1999

[Determination of 2,4-dinitrophenol by solid-phase microextraction coupled to GC/MS].

Solid-phase microextraction coupled GC/MS was investigated for the determination of 2,4-dinitrophenol in aqueous sample. Analytes were extracted by a 85 microns polyacrylate coated fiber. The fiber was then transferred into the injector of GC. Analytes were thermally desorbed and detected by GC/MS. The influences of several parameters on SPME procedure have been studied. The optimization condition was obtained: directly sampling in the water sample with the extraction period was 30 min and the desorption time 3 min at 270 degrees C. Acidification by hydrochloric acid (pH 2) and saturated salt were necessary for the best sensitivity. The precision of SPME is better than that of liquid-liquid extraction. This method is a fast, simple, and pre-concentration-free technique, which is suitable for detecting 2,4-dinitrophenol in water sample.

2,4-Dinitrophenol↗
PubMed1999

Solid-phase microextraction for the determination of iodinated trihalomethanes in drinking water.

A headspace solid-phase microextraction (HS-SPME) method has been developed for the determination of iodinated trihalomethanes (ITHMs) in treated water samples. Mixed THMs (bromochloroido-, bromodiiodo-, chlorodiiodo-, dibromoiodo- and dichloroiodo-) were previously synthesized since commercial standards are not available. HS-SPME has shorter equilibration times than direct SPME, a cleaner background and a longer fiber life. Experimental parameters such as the selection of SPME coatings, sample volume, extraction time and addition of salts were studied. The Carbowax-divinylbenzene fiber appears to be the most suitable for the determination of ITHMs. Analytical parameters such as linearity, limit of detection and precision were also evaluated. HS-SPME was compared to liquid-liquid microextraction for the analyses of spiked treated water samples, obtaining a good agreement. It is concluded that HS-SPME has a great potential for drinking water analysis.

Adsorption↗
PubMed2006

Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection. Very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water.

A new method was used for the extraction of organophosphorus pesticides (OPPs) from water samples: dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-flame photometric detection (GC-FPD). In this extraction method, a mixture of 12.0 microL chlorobenzene (extraction solvent) and 1.00 mL acetone (disperser solvent) is rapidly injected into the 5.00 mL water sample by syringe. Thereby, a cloudy solution is formed. In fact, the cloudy state is because of the formation of fine droplets of chlorobenzene, which has been dispersed among the sample solution. In this step, the OPPs in water sample are extracted into the fine droplets of chlorobenzene. After centrifuging (2 min at 5000 rpm), the fine droplets of chlorobenzene are sedimented in the bottom of the conical test tube (5.0+/-0.3 microL). Sedimented phase (0.50 microl) is injected into the GC for separation and determination of OPPs. Some important parameters, such as kind of extraction and disperser solvent and volume of them, extraction time, temperature and salt effect were investigated. Under the optimum conditions, the enrichment factors and extraction recoveries were high and ranged between 789-1070 and 78.9-107%, respectively. The linear range was wide (10-100,000 pg/mL, four orders of magnitude) and limit of detections were very low and were between 3 to 20 pg/mL for most of the analytes. The relative standard deviations (RSDs) for 2.00 microg/L of OPPs in water with internal standard were in the range of 1.2-5.6% (n=5) and without internal standard were in the range of 4.6-6.5%. The relative recoveries of OPPs from river, well and farm water at spiking levels of 50, 500 and 5000 pg/mL were 84-125, 88-123 and 93-118%, respectively. The performance of proposed method was compared with solid-phase microextraction (SPME) and single drop microextraction. DLLME is a very simple and rapid (less than 3 min) method, which requires low volume of sample (5 mL). It also has high enrichment factor and recoveries for extraction of OPPs from water.

Chromatography, Gas↗
PubMed1999

Determination of equilibrium constant of alkylbenzenes binding to bovine serum albumin by solid phase microextraction.

Solid phase microextraction (SPME) coupled with GC has been applied to study the binding properties between bovine serum albumin (BSA) and volatile organic compounds such as benzene, toluene, ethylbenzene, propylbenzene and butylbenzene. Their protein-ligand equilibrium constants have been determined. The measurement of free and bound ligand concentrations in the aqueous solution was based on the equilibrium among the analyte in the fiber coating (Cf), headspace (Ch) and aqueous solution (Cs). The work demonstrated that SPME is a simple and effective method in the study of protein binding to measure the freely dissolved analyte concentration as well as the equilibrium constant. The theoretical aspect of the SPME applied to the equilibrium constant measurement in two-phase (liquid sample-fiber coating) and three-phase (liquid sample-headspace-fiber coating) systems has been thoroughly discussed. The results demonstrated that the interpretation of the calibration data is crucial to the determination of freely dissolved analyte concentration and the equilibrium constant especially when the sample volume is small. The error in the experimental system is discussed. It is demonstrated in this study that for the three-phase system the amount of the analyte partitioned in the headspace could be ignored only in certain circumstances, where the Henry's law constant and the ratio between headspace volume and sample volume are sufficiently small.

Animals↗
PubMed2002

Microwave-assisted generation of standard gas mixtures.

Microwave heating was employed for preparation of the standard gas of volatile organic compounds (VOCs) and semivolatile organic compounds (semi-VOCs) by using a 1000 W commercial domestic microwave oven and 1 L gas-sampling bulbs. The VOCs investigated were benzene, chloroform, 1,3-dichlorobenzene, tetrachloroethylene, toluene, and 1,1,2-trichloroethane, and the semi-VOCs used were the polychlorinated biphenyls (PCBs) PCB 1016 and PCB 1248. Since these weakly or nonpolar molecules are very poor absorbers of microwave energy, an appropriate amount of water was introduced to accept microwave radiation and act as the thermal source to accelerate their evaporation. The glass bulb may also contribute thermal energy to the VOCs/semi-VOCs by accepting microwave energy to a small degree. For 0.5 microL of liquid VOCs on 10 mg of glass wool, it was shown that 15 microL of H2O and 60 s of microwave heating yielded a very efficient evaporation [97.2-106.4%, compared with a classic method (Muller, L; Gorecki, T.; Pawliszyn, J. Fresenius' J. Anal. Chem. 1999, 364, 610-616)]. For 1 microL of PCB solution (1000 microg/mL in hexane), 15 microL of H2O and 90 s of microwave heating also provided a complete evaporation. The addition of water was particularly significant for microwave-assisted evaporation of PCBs because semi-VOCs are much more difficult to evaporate than VOCs. This developed microwave technique proved to be quite simple, powerful, rapid, accurate, and safe for the preparation of VOC/semi-VOC standard gas. Solid- phase microextraction combined with gas chromatography was used for the gas analysis.

Air Pollution↗
PubMed2000

Use of solid-phase microextraction in the investigation of chemical communication in social wasps.

Solid-phase microextraction has been used to investigate chemical communication in several social wasp species. Using the technique to analyse exocrine gland secretions, we demonstrate that the results are comparable with those obtained with the more classical methods that use solvents, eliminating, in many cases, the shortcomings of these methods in insect pheromone analysis. As a result of its simplicity this technique is very suitable for research on the chemical ecology of social wasps, and on insect communication in general.

Animal Communication↗
PubMed1999

Application of solid-phase microextraction to the profiling of an illicit drug: manufacturing impurities in illicit 4-methoxyamphetamine.

This article describes the application of solid-phase microextraction (SPME) to the recovery of manufacturing by-products and impurities from an illicit drug seizure. The preparation chosen for examination using this technique contained 4-methoxyamphetamine, an hallucinogenic amphetamine that has been encountered frequently in South Australia. Compounds found in the PMA preparation included 4-methoxyphenol, 4-methoxybenzaldehyde, 4-methoxyphenyl-2-propanone, 4-methoxyphenyl-2-propanol, 4-methoxyphenyl-propene, and (tentatively) 4-methyl-5-(4'-methoxyphenyl) pyrimidine. The presence of these compounds suggests that the active drug was prepared from 4-methoxybenzaldehyde via 4-methoxyphenyl-2-propanone using a Leuckardt reductive amination. In this instance, SPME was found to be a simple, rapid, and non-destructive recovery technique that gave results complementary to those provided by conventional liquid-liquid extraction. There is an indication that SPME might find application in profiling of illicit drugs.

Amphetamines↗
PubMed2004

Determination of menthol in plasma and urine of rats and humans by headspace solid phase microextraction and gas chromatography--mass spectrometry.

A method for the determination of menthol and menthol glucuronide (M-G) after enzymatic hydrolysis in plasma and urine of rats and humans was developed using headspace solid phase microextraction and gas chromatography-mass spectrometry in the selected ion monitoring mode (HS-SPME/GC-MS). The assay linearity for plasma ranged from 5 to 1000 ng/ml. The limit of quantification (LOQ) in plasma was 5 ng/ml. The intra- and inter-day precision for menthol and M-G were < or = 18.1% R.S.D. at the LOQ and < or = 4.0% at higher concentrations. Menthol and M-G were determined in rat and human plasma and urine after administration of menthol.

Animals↗
PubMed2002

Determination of aldehydes in drinking water using pentafluorobenzylhydroxylamine derivatization and solid-phase microextraction.

A headspace solid-phase microextraction (HS-SPME) procedure followed by gas chromatography and electron capture detection (GC-ECD) has been developed for the determination of aldehydes in drinking water samples at microg/l concentrations. A previous derivatization with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was performed due to the high polarity and instability of these ozonation by-products. Several SPME coatings were tested and the divinylbenzene-polydimethylsiloxane (DVB-PDMS) coating in being the most suitable for the determination of these analytes. Experimental SPME parameters such as selection of coating, sample volume, addition of salt, extraction time and temperature of desorption were studied. Analytical parameters such as precision, linearity and detection limits were also determined. HS-SPME was compared to liquid-liquid microextraction (proposed in US Environmental Protection Agency Method 556) by analyzing spiked water samples; a good agreement between results obtained with both techniques was observed. Finally, aldehydes formed at the Barcelona water treatment plant (N.E. Spain) were determined at levels of 0.1-0.5 microg/l. As a conclusion, HS-SPME is a powerful tool for determining ozonation by-products in treated water.

Aldehydes↗
PubMed2005

Highly porous solid-phase microextraction fiber coating based on poly(ethylene glycol)-modified ormosils synthesized by sol-gel technology.

The preparation and characteristics of solid-phase microextraction (SPME) fibers coated with Carbowax 20M ormosil (organically modified silica) are described here. Raw fused silica fibers were coated with Carbowax 20M-modified silica using sol-gel process. Scanning electron micrographs of fibers revealed a highly porous, sponge-like coating with an average thickness of (8 +/- 1) microm. The sol-gel Carbowax fibers were compared to commercial fibers coated with 100 microm polydimethylsiloxane (PDMS) and 65 microm Carbowax-divinylbenzene (DVB). Shorter equilibrium times were possible with the sol-gel Carbowax fiber: for headspace extraction of the test analytes, they ranged from less than 3 min for benzene to 15 min for o-xylene. Extraction efficiencies of the sol-gel Carbowax fiber were superior to those of conventional fibers: for o-xylene, the extracted masses were 230 and 540% of that obtained with 100 microm PDMS and 65 microm Carbowax-DVB fibers, respectively.

Benzene↗
PubMed2000

Microextraction of drugs.

This review will attempt to provide an overview as well as a theoretical and practical understanding of the use of microextraction technologies for drug analysis. The majority of the published reports to date focus on the use of fibre solid-phase microextraction and so the review is significantly focused on this technology. Other areas of microextraction such as single drop and solvent film microextraction are also described. Where there are insufficient examples in the literature to illustrate important concepts, examples of non-drug analyses are presented. The review is intended for readers new to the field of microextraction or its use in drug extraction, but also provides an overview of the most recent advances in the field which may be of interest to more experienced users. Particular emphasis is placed on the effect various sample matrices have on extraction characteristics.

Adsorption↗
PubMed1996

Solid phase microextraction for quantitative headspace sampling of apple volatiles.

Solid phase microextraction (SPME) was evaluated for use in the quantification of aroma volatile production by Granny Smith apples during cool storage. Particular attention was paid to quantifying alpha-farnesene (3,7,11-trimethyldodeca-1,3(E),6(E),10-tetraene) due to its involvement in superficial scald, a disorder of cool stored apples. Comparison between SPME and solid phase extraction (SPE) showed that the SPME fiber had greater adsorption of high molecular weight (MW) volatiles such as alpha-farnesene. When sampling by SPME, these higher MW volatiles did not equilibrate between apples, headspace, and fiber within sampling times as long as 90 min, while lower MW volatiles equilibrated within 5 min. This behavior was also shown by a simple model system consisting of five selected volatiles dissolved in an involatile, lipophilic liquid (squalane). The less volatile high MW aroma compounds evaporated slowly from the surface of the apples and were depleted from the headspace because of very rapid adsorption by the SPME fiber. The amount of alpha-farnesene adsorbed by the fiber increased with air movement through the system. In a static headspace system, the amount of alpha-farnesene adsorbed by the fiber decreased nonlinearly with increasing distance from the apples, due to adsorption onto the glass walls. While SPME is ideal for rapid, qualitative determination of apple headspace volatiles, the slower equilibration of higher MW volatiles limits its use for quantification in more complex systems.

Chromatography, Gas↗
PubMed2005

Experimental determination and calculation of distribution coefficients between air and fiber with polydimethylsiloxane coating for some groups of organic compounds.

This paper reports the results of experimental determination of distribution coefficients K(fa) for five terpene hydrocarbons and five aliphatic ketones between air and polydimethylsiloxane (PDMS) coating for solid-phase microextraction. To estimate the values of K(fa) for compounds of the same classes, which did not undergo experiments, it is proposed to use an empirical two-parameter equation in which various physicochemical and structural characteristics weakly correlated with each other are used as descriptors. It is also shown that for these purposes it is possible to use distribution coefficients of compounds in any other two-phase heterogeneous system, e.g. octanol-water or hexane-acetonitrile. This approach was applied to estimate K(fa) values of 92 volatile organic compounds.

Air↗
PubMed2003

Determination of cannabinoids in hemp food products by use of headspace solid-phase microextraction and gas chromatography-mass spectrometry.

A fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME), followed by on-fiber derivatization and gas chromatographic-mass spectrometric (GC-MS) detection has been developed for determination of cannabinoids in hemp food samples. After addition of a deuterated internal standard, the sample was hydrolyzed with sodium hydroxide and submitted to direct HS-SPME. After absorption of analytes for on-fiber derivatization, the fiber was placed directly into the headspace of a second vial containing N-methyl- N-trimethylsilyltrifluoroacetamide (MSTFA), before GC-MS analysis. Linearity was good for Delta(9)-tetrahydrocannabinol (THC), cannabidiol, and cannabinol; regression coefficients were greater than 0.99. Depending on the characteristics of the matrix the detection limits obtained ranged between 0.01 and 0.17 mg kg(-1) and the precision between 0.4 and 11.8%. In comparison with conventional liquid-liquid extraction this automated HS-SPME-GC-MS procedure is substantially faster. It is easy to perform, solvent-free, and sample quantities are minimal, yet it maintains the same sensitivity and reproducibility. The applicability was demonstrated by analysis of 30 hemp food samples. Cannabinoids were detected in all of the samples and it was possible to differentiate between drug-type and fiber-type Cannabis sativa L. In comparison with other studies relatively low THC concentrations between 0.01 and 15.53 mg kg(-1) were determined.

Cannabinoids↗
PubMed2001

A comparison of headspace entrainment on Tenax with solid phase microextraction for the analysis of the aroma volatiles of cooked beef.

Headspace solid phase microextraction (SPME), using a Carboxen-polydimethylsiloxane fiber, was compared with headspace entrainment on Tenax TA, as a means of examining the aroma constituents of cooked beef. Extracts were analyzed using gas chromatography-mass spectrometry. Headspace entrainment on Tenax extracted higher amounts of most volatiles, particularly low-boiling compounds. However, polar volatiles, such as hydroxyfuranones and hydroxyketones, were present at higher levels in the SPME extracts. Some components were present only in the SPME extracts, including norfuraneol, furaneol, and cyclotene, which are key Maillard reaction intermediates.

Animals↗
PubMed2005

Determination of alkylphenols and bisphenol-A. A comparative investigation of functional polymer-coated membrane microextraction and solid-phase microextraction techniques.

A functional polymer (hydroxylated polymethacrylate) coated on porous polysulfone hollow fiber membrane (PS-HFM) was used as an adsorbent for the extraction of alkylphenols and bisphenol-A from seawater samples. Analyses of the extracts were performed using gas chromatography-mass spectrometry (GC-MS) after injection-port derivatization using bis(trimethylsilyl)trifluoroacetamide (BSTFA). We term the procedure as polymer-coated hollow fiber microextraction (PC-HFME). Owing to high porosity PS-HFM coated with hydroxylated polymer showed high extraction efficiency. Compared with solid-phase microextraction (SPME), PC-HFME showed good selectivity and sensitivity. Detection limits of alkylphenols and bisphenol-A ranged between 0.07 and 2.34 ng l(-1). The linearity range was from 0.01 to 15 microg l(-1) and the correlation coefficient (r) up to 0.997. The sensitivity and selectivity of the coated HFM could be potentially tuned by changing the characteristics of the coated hydroxylated polymer. The PC-HFME procedure was applied to the detection of alkylphenols and bisphenol-A in the coastal waters of Singapore.

Benzhydryl Compounds↗