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PubMed2001

SPME-MS-MVA as a rapid technique for assessing oxidation off-flavors in foods.

A new technique using solid-phase microextraction, mass spectrometry, and multivariate analysis (SPME-MS-MVA) was developed for the study of oxidized off-flavors in foods. The analytical column of a GC-MS system was replaced with a 1-m deactivated fused-silica column, which served as a transfer line to deliver volatiles extracted from samples with a Carboxen/PDMS SPME fiber to the mass spectrometer. Mass fragmentation data resulting from the unresolved food volatile components were subjected to MVA. The mass intensities from m/z 50 to m/z 150 were selected to perform MVA. Principal component analysis based on SPME-MS-MVA provided rapid differentiation of the following types of samples: control soybean oil from soybean oil exposed to fluorescent light for various time periods; control nondairy coffee creamer from complaint ("oxidized") nondairy coffee creamer samples; fresh boiled beef from boiled beef with various levels of warmed-over flavor (WOF); and control 2% milk samples from 2% milk samples abused by light or copper exposure. SPME-MS-MVA is rapid and offers significant advantages over commercial electronic nose instruments currently being used as quality assurance tools to differentiate normal tasting food and beverage samples and ingredients from those containing off-flavors and malodors.

Animals↗

PubMed2004

A cost of alarm pheromone production in cotton aphids, Aphis gossypii.

The sesquiterpene, (E)-beta-farnesene, is used by many aphid species as an alarm pheromone to warn related individuals of predation. Disturbed cotton aphids, Aphis gossypii Glover, released (E)-beta-farnesene into the air as detected by solid phase microextraction and gas chromatography mass spectrometry (GC-MS). Solvent extracts of cotton aphids of various life stages and weights also were analyzed by GC-MS for sums of ions 69 and 93, which discriminated (E)-beta-farnesene from coeluting compounds. Aphids of all life stages and sizes reared on cotton plants in both an environmental chamber and glasshouse contained (E)-beta-farnesene in amounts ranging from 0.1 to 1.5 ng per individual. The quantities of (E)-beta-farnesene in aphids increased in relation to increasing body weight, and variation in individual weights explained about 82% of the variation in alarm pheromone. However, the concentrations (ng/mg fresh weight) declined exponentially with increasing body weight. These findings indicate that aphid nymphs try to compensate for their smaller size by producing relatively more pheromone per weight than adults but still cannot approach an evolutionary optimal load, as assumed in adults with the greatest total amounts. This suggests that young aphids need to balance costs of growth and maturation with costs of producing the alarm pheromone.

Animals↗

PubMed2002

Cryogenic oven-trapping gas chromatography for analysis of volatile organic compounds in body fluids.

Cryogenic oven-trapping (COT) with capillary GC has been successfully applied to analysis of chloroform, dichloromethane, trichloroethylene, diethyl ether, the components of solvent thinner (ethyl acetate, benzene, n-butanol, toluene, and others), xylene isomers, cyanide, ethanol, hexanes, general anesthetics, and styrene in human body fluids. This COT-GC technique was compared with headspace solid-phase microextraction (SPME) coupled with GC for some volatile organic compounds (VOC); for all compounds compared the sensitivity achieved using COT-GC was more than ten times higher than for headspace SPME-GC. The COT-GC method is recommended for widespread use in forensic and environmental toxicology, because it is simple, requires no special GC operations, and yet enables high sensitivity and high resolution.

Body Fluids↗

PubMed2002

Sorptive sample preparation -- a review.

Most sample-enrichment procedures currently available rely on adsorption of the analytes of interest by a suitable adsorbent material. Although good performance can be obtained for many practical problems, in some cases the applicability of adsorptive sample preparation falls short, particularly for the enrichment of polar and/or high-molecular-weight compounds, especially in combination with thermal desorption. Because of the very strong retention of adsorbent materials, undesired effects such as incomplete desorption and artifact formation are observed. Polar solutes are easily adsorbed but readily undergo surface-catalyzed reactions and on desorption yield compounds different than those originally sampled. High-molecular-weight compounds cannot be desorbed because of extremely strong interactions with the adsorbent and their low volatility. To overcome some of these problems sample-preparation techniques based on polydimethylsiloxane sorption have been developed over the past 15 years. In contrast with adsorptive trapping, sorption is based on dissolution of the analytes in a liquid polymeric material. This is a much more inert means of solute retention which overcomes some of the limitations encountered when working with adsorbents. In this contribution, the basic principles of sorption, the different instrumentation used, and applications of the technique will be reviewed. The review covers the sorptive sample-preparation techniques, open-tubular trapping (OTT), solid-phase microextraction (SPME), gum-phase extraction (GPE), equilibrium gum-phase extraction (EGPE), and stir-bar-sorptive extraction (SBSE). Because of the nature of sorptive sample-preparation techniques, which perform particularly well in combination with thermal desorption, this review focuses strongly on gas chromatography as the means of chemical analysis.

Chromatography, Gas↗

PubMed2002

Miniaturized solid-phase extraction as a sample preparation technique for the determination of phthalates in water.

Miniaturized solid-phase extraction (SPE) has been developed and successfully employed for the determination of organic species in water samples by liquid chromatography (LC). The method is based on the concept of a microscale extraction technique using a fused-silica capillary column for gas chromatography (GC), so-called in-tube solid-phase microextraction (SPME). The extraction conditions, such as the extraction time and flow-rate for the extraction and desorption process, were investigated as well as the effect of the internal structure of the extraction capillary on the efficiency. By inserting a stainless steel wire into the extraction capillary to reduce the internal volume of the capillary with the same surface area of the coating, an improved extraction and pre-concentration effects were obtained. Further pre-concentration was accomplished by the extraction device with a novel fiber-in-tube configuration. The direct coupling of the extraction method with a LC system has made it possible to determine low levels of phthalates in water samples without high consumption of organic solvents. The system developed must have potential applications for the analysis of environmental and biological samples in aqueous sample matrices.

Capillary Action↗

PubMed2002

Validation of an SPME method, using PDMS, PA, PDMS-DVB, and CW-DVB SPME fiber coatings, for analysis of organophosphorus insecticides in natural waters.

Solid-phase microextraction (SPME) has been optimized and applied to the determination of the organophosphorus insecticides diazinon, dichlofenthion, parathion methyl, malathion, fenitrothion, fenthion, parathion ethyl, bromophos methyl, bromophos ethyl, and ethion in natural waters. Four types of SPME fiber coated with different stationary phases (PDMS, PA, PDMS-DVB, and CW-DVB) were used to examine their extraction efficiencies for the compounds tested. Conditions that might affect the SPME procedure, such as extraction time and salt content, were investigated to determine the analytical performance of these fiber coatings for organophosphorus insecticides. The optimized procedure was applied to natural waters - tap, sea, river, and lake water - spiked in the concentration range 0.5 to 50 micro g L(-1) to obtain the analytical characteristics. Recoveries were relatively high - >80% for all types of aqueous sample matrix - and the calibration plots were reproducible and linear (R(2)>0.982) for all analytes with all the fibers tested. The limits of detection ranged from 2 to 90 ng L(-1), depending on the detector and the compound investigated, with relative standard deviations in the range 3-15% at all the concentration levels tested. The SPME partition coefficients (K(f)) of the organophosphorus insecticides were calculated experimentally for all the polymer coatings. The effect of organic matter such as humic acids on extraction efficiency was also studied. The analytical performance of the SPME procedure using all the fibers in the tested natural waters proved effective for the compounds.

Acrylic Resins↗

PubMed2003

Optimization and application of SPME for the gas chromatographic determination of endosulfan and its major metabolites in the ng L(-1) range in aqueous solutions.

In the present study an analytical method was optimized for the determination of alpha-endosulfan, beta-endosulfan, endosulfan sulfate, endosulfan ether and endosulfan lactone in small volumes of environmental aqueous samples using solid-phase microextraction (SPME) and gas chromatography-electron capture detection (GC-ECD). A 100 micro m polydimethylsiloxane (PDMS) phase was used for the extraction. The limit of detection (LOD) for the analytes varied between 0.01 and 0.03 micro g L(-1) with a relative standard deviation of 3 to 11%. The influence of the ionic strength on the extraction efficiency was investigated for the individual compounds. alpha-Endosulfan, beta-endosulfan, endosulfan sulfate and endosulfan ether were extracted successfully without salt addition. The extraction efficiency of endosulfan lactone was improved with 30% NaCl content. A general decrease in extraction efficiency for alpha-endosulfan, beta-endosulfan, endosulfan sulfate and endosulfan ether with high NaCl content (20-30%) in the solution was observed due to glass surface adsorption. No effect of dissolved organic material (DOM) on the extraction efficiency was observed. The extraction coefficients changed between Log K=2.17 and 3.33. A sample from the Antarctic region was analyzed using the optimized GC-ECD/SPME method. To confirm the results obtained for the real sample a GC with a mass spectrometer (MS) was used. Endosulfan sulfate, the most toxic metabolite of endosulfan, was found in the sample at a concentration of 0.3 micro g L(-1).

Antarctic Regions↗

PubMed2003

Laboratory and field experiments used to identify Canis lupus var. familiaris active odor signature chemicals from drugs, explosives, and humans.

This paper describes the use of headspace solid-phase microextraction (SPME) combined with gas chromatography to identify the signature odors that law enforcement-certified detector dogs alert to when searching for drugs, explosives, and humans. Background information is provided on the many types of detector dog available and specific samples highlighted in this paper are the drugs cocaine and 3,4-methylenedioxy- N-methylamphetamine (MDMA or Ecstasy), the explosives TNT and C4, and human remains. Studies include the analysis and identification of the headspace "fingerprint" of a variety of samples, followed by completion of double-blind dog trials of the individual components in an attempt to isolate and understand the target compounds that dogs alert to. SPME-GC/MS has been demonstrated to have a unique capability for the extraction of volatiles from the headspace of forensic specimens including drugs and explosives and shows great potential to aid in the investigation and understanding of the complicated process of canine odor detection. Major variables evaluated for the headspace SPME included fiber chemistry and a variety of sampling times ranging from several hours to several seconds and the resultant effect on ratios of isolated volatile components. For the drug odor studies, the CW/DVB and PDMS SPME fibers proved to be the optimal fiber types. For explosives, the results demonstrated that the best fibers in field and laboratory applications were PDMS and CW/DVB, respectively. Gas chromatography with electron capture detector (GC/ECD) and mass spectrometry (GC/MS) was better for analysis of nitromethane and TNT odors, and C-4 odors, respectively. Field studies with detector dogs have demonstrated possible candidates for new pseudo scents as well as the potential use of controlled permeation devices as non-hazardous training aids providing consistent permeation of target odors.

Animals↗

PubMed2003

Comparative study of extraction techniques for determination of garlic flavor components by gas chromatography-mass spectrometry.

Several sampling techniques based on steam distillation (SD), simultaneous distillation and solvent extraction (SDE), solid-phase trapping solvent extraction (SPTE), and headspace solid-phase microextraction (HS-SPME) have been compared for the determination of Korean garlic flavor components by gas chromatography-mass spectrometry (GC-MS). Diallyl disulfide (57.88%), allyl sulfide (23.59%), and diallyl trisulfide (11.40%) were found to be the predominant flavor components of garlic samples extracted by SDE whereas these components were at levels of 89.77%, 2.43%, and 3.89% when the same sample was extracted by SD, 97.77%, 0.17%, and 0.10% by SPTE, and 97.85%, 0.01%, and 0.01% by HS-SPME using the 50/30-microm divinyl benzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber. Thermal degradation of components such as allyl methyl sulfide, dimethyl disulfide, and thiirane were observed for SDE and SD but not for SPTE or HS-SPME. HS-SPME had several advantages compared with SD, SDE, and SPTE-rapid solvent-free extraction, no apparent thermal degradation, less laborious manipulation, and less sample requirement. Five different fiber coatings were evaluated to select a suitable fiber for HS-SPME of garlic flavor components. DVB/CAR/PDMS was most efficient among the five types of fiber investigated.

Flavoring Agents↗

PubMed2003

Interlaboratory comparison study for the determination of methyl tert-butyl ether in water.

This is the first publication which describes the evaluation of the analytical performance and state-of-the-art of the determination of methyl tert-butyl ether (MTBE) in water at ng L(-1) concentrations. An interlaboratory comparison study for the determination of MTBE in water was carried out. Twenty-eight laboratories from seven European countries participated in the study. Twenty of those finally transmitted results to the organiser. Italian spring water, containing no detectable amounts of MTBE was fortified to yield two samples with MTBE concentrations of 0.074 +/- 0.004 microg L(-1) and 0.256 +/- 0.010 microg L(-1). The laboratories applied their regular in-house methods to analyse the water samples. Static headspace, Purge & Trap, solid-phase microextraction (SPME) or direct aqueous injection were used as sample preparation techniques. Subsequent separation and detection of MTBE were performed by gas chromatography/mass spectrometry (GC/MS) or gas chromatography/flame ionisation detection (GC/FID). After rejection of outliers, the overall arithmetic mean of laboratory results corresponded to recoveries of 78 +/- 20% (Sample A) and 88 +/- 20% (Sample B) of the reference concentrations. The between laboratory coefficients of variation (CV) were 32% and 31%, respectively. The organisation of the study and quality assurance measures at the organiser's laboratory are described. Moreover, the measurement results of the participants and the analytical methods used for the determination of MTBE are presented and the correlation between selected method parameters and data quality is discussed.

Journal Article↗

PubMed2003

Rapid analysis of aromatic contaminants in water samples by means of laser ionization mass spectrometry.

Three different approaches to laser ionization mass spectrometric analysis of aromatic compounds in water samples are described and their performances are compared. Whereas the first two methods are based on direct laser desorption and subsequent laser ionization of either frozen or adsorbed samples in a time-of-flight mass analyzer, the third performs laser ionization in a quadrupole ion-trap into which the sample is transferred from a GC injector via a short piece of capillary tubing. For the laser-desorption method a detection limit in the 100 microg L(-1) range was determined for fluorene in frozen samples. The easier to handle analysis of adsorbed samples yielded sensitivities which were lower by about two orders of magnitude. As both direct techniques do not reach the sensitivity required for ultra trace analysis in water a preconcentration step in form of solid-phase microextraction was added before measurement using the laser ionization quadrupole ion-trap mass spectrometer. Sensitivity in the desired ng L(-1) range was easily achieved.

Journal Article↗

PubMed2004

SPME analysis of volatile compounds from unfermented olives subjected to thermal treatment.

The effect of different types of thermal treatment, designed to increase the product's shelf-life, on the volatile composition of "Campo Real" unfermented table olives, has been studied by headspace solid-phase microextraction (HS-SPME) and GC-MS analysis. Different SPME fibres were evaluated to determine their selectivity for a mixture of the main components of the different spices used in "Campo Real" olive dressing. Of the different fibres investigated, the polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre was selected for analysis of the olive brines, which contained nine main aroma components. The types of thermal treatment were sterilisation (121 degrees C, 15 min) and four pasteurisation conditions (60 degrees C or 80 degrees C each for 5 or 9 min). Pasteurisation did not lead to significant changes in the amounts of these nine volatile compounds; the 2-butanol signal was reduced by treatment at 80 degrees C. On the other hand, sterilisation of the brine resulted in an decrease in the signals from these compounds and the appearance of a new, high signal for benzaldehyde; the origin of this has not yet been determined. Results suggest that the selected pasteurisation conditions do not significantly modify the typical, and valued, aroma characteristics of "Campo Real".

Benzenesulfonates↗

PubMed2004

High-throughput analysis of phthalate esters in human serum by direct immersion SPME followed by isotope dilution-fast GC/MS.

Solid-phase microextraction (SPME) coupled to gas chromatography/mass spectrometry (GC/MS) was applied to the determination of phthalate esters in human serum. The present method decreased the sample preparation time by a factor of 50 by using direct immersion SPME with an 85-microm polyacrylate fiber to extract phthalate esters from the matrix. The use of fast GC/MS further improves total analysis time when compared to other techniques. Isotope dilution was successfully applied to improve the precision, reproducibility, and repeatability of the SPME method. The linear dynamic range spans several orders of magnitude from low ppb to ppm levels, and the LOD for the method is 15 pg microL(-1) on average with RSDs less than 4% for the six phthalate esters included in this study.

Calibration↗

PubMed2004

A direct quantitative analysis method for monitoring biogenic volatile organic compounds released from leaves of Pelargonium hortorum in situ.

A direct quantitative method is presented that is based upon the use of multiple headspace solid phase microextraction (HS-SPME) to monitor biogenic volatile organic compounds (BVOCs) released from a living leaf of Pelargonium hortorum in situ. Seventeen BVOCs were detected by GC-MS after a single SPME extraction using a CAR/DVB/PDMS fibre. An internal standard was employed to determine the absolute amounts of seven terpenoid compounds released from a P. hortorum leaf. The quantitative analysis was performed over two days, with extraction preformed for 20 min every 3 h. The amount of volatiles extracted varied with the time of day, with two maxima recorded at 14:00 (day 1) and 17:00 (day 2), corresponding to 236 and 277 ng of the seven terpenoids recorded, respectively. These results indicate that multiple HS-SPME in combination with an internal standard is a simple, quick, and quantitative technique for analysising BVOC emissions from a live plant sample.

Calibration↗

PubMed2005

Stable isotope dilution analysis of wine fermentation products by HS-SPME-GC-MS.

The aim of this study was to quantify, in a single analysis, 31 volatile fermentation-derived products that contribute to the aroma of red and white wine. We developed a multi-component method based on headspace solid-phase microextraction coupled with gas chromatography mass spectrometry (HS-SPME-GC-MS). The 31 volatile compounds analysed include ethyl esters, acetates, acids and alcohols. Although these compounds have a range of functional groups, chemical properties, volatilities, affinities for the SPME fibre, and are found in wine at various concentrations, the accuracy of the analysis was achieved with the use of polydeuterated internal standards for stable isotope dilution analyses (SIDA). Nine of the labelled standards were commercially available, while 22 were synthesised. The method was validated by a series of duplicate spiked standard additions to model, white and red wine matrices over the concentration range relevant for each compound in wine. This demonstrated that the appropriate use of SIDA helped to account for matrix effects, for instance potential sources of variation such as the relative response to the MS detector, ionic strength, ethanol content and pH of different wine matrices. The resultant calibration functions had correlation coefficients (R(2)) ranging from 0.995 to 1.000. Each compound could be quantified at levels below its aroma threshold in wine. Relative standard deviations were all <5%. The method was optimised for the best compromise (over the 31 compounds) of wine dilution factor, level of sodium chloride addition, SPME fibre, SPME temperature, SPME time, GC column and MS conditions. Confirmation of identity was achieved by retention time and peak shape, and measurement of at least three ions for each analyte and internal standard with the MS operating in selected ion monitoring mode to facilitate more precise quantitation with a high sampling rate. The method is a valuable research tool with many relevant applications. A novel method for the combined chiral separation and SIDA quantification of 2- and 3-methylbutanoic acid is also demonstrated.

Butyrates↗

PubMed2005

Confirmation of the formation of dichlorodibenzo-p-dioxin in the photodegradation of triclosan by photo-SPME.

Photodegradation is a possible way to eliminate organic pollutants from the environment but, at the same time, can be a source of toxic byproducts. The photochemical conversion of triclosan, a common pollutant in continental waters, into dichlorodibenzo-p-dioxin (DCDD) has been confirmed in our preliminary experiments employing photo-SPME (photo-solid-phase microextraction) using 18-W UV irradiation at 254-nm wavelength. Under these conditions, triclosan is rapidly photodegraded (70% of triclosan was degraded in 2 min); the most important novel aspect of this work is the conversion of triclosan to DCDD directly on the polydimethylsiloxane coating of the SPME fiber. Moreover, this conversion is also confirmed in non-buffered aqueous photodegradation experiments using SPME as the extraction technique. In all the experiments of this study, analysis was carried out by gas chromatography-electronic impact mass spectrometry (GC-EI/MS).

Dioxins↗

PubMed2005

Analysis of trace levels of pesticides in rainwater using SPME and GC-tandem mass spectrometry.

A multiresidue method using gas chromatography coupled to ion trap tandem mass spectrometry (GC-ITD-MS/MS) associated with solid phase microextraction (SPME) was developed for the analysis of 20 pesticides commonly used in the Alsace region in rainwater samples. Since the pesticides were expected to be present at very low concentrations and in complex matrices, the analytical method used was both highly selective and sensitive. Therefore, fibers coated with polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB) were tested, and the parameters affecting the precision and accuracy of the SPME method were investigated and optimized. These parameters include the type of fiber, the adsorption time, the effect of salt, and the extraction temperature. The PDMS fiber was the most polyvalent for the extractions of the different pesticides studied. Detection limits of between 5 and 500 ng L(-1), depending on the compounds under study (except for those which could not be analyzed: captan and mevinphos), were obtained with this analytical procedure. This method was applied to the analysis of rainwater samples collected simultaneously on a weekly basis at one rural and one urban site between March 2002 and July 2003. While some of the 20 pesticides analyzed were constantly detected (such as lindane and atrazine), a strong temporal variability was observed for some of the others (including alachlor, metolachlor, atrazine).

Journal Article↗

PubMed2005

Determination of sterols in biological samples by SPME with on-fiber derivatization and GC/FID.

A new procedure for the determination of sterols in serum samples is proposed. The system consists of coating a Solid Phase Microextraction (SPME) microfiber in headspace mode with the derivatizing agent N,O-bis(trimethylsilyl)trifluoracetamide (BSTFA) and then applying this coated fiber to the simultaneous extraction and derivatization of three precursors in the cholesterol biosynthesis pathway (desmosterol, lathosterol and lanosterol) and two phytosterols (sitosterol and sitostanol) in serum samples. Optimization of the analytical procedure via the application of an experimental design, a study of matrix effects, and an analysis of serum pool samples are all described and discussed.

Flame Ionization↗