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PubMed2004

Quality assessment of Flos Chrysanthemi Indici from different growing areas in China by solid-phase microextraction-gas chromatography-mass spectrometry.

Flos Chrysanthemi Indici is a common traditional Chinese medicine (TCM). In this paper, headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS) was developed for quality assessment of Flos Chrysanthemi Indici from different growing areas in China. SPME parameters such as extraction fibers, extraction temperature, extraction time and sample mass were investigated to achieve identical results to those obtained by the steam distillation (SD). The selected SPME conditions were as follows: SPME fiber coated with 65-microm PDMS/DVB, extraction temperature of 60 degrees C, extraction time of 30 min and sample mass of 1.0 g. Furthermore, four active compounds (eucalyptol, camphor, borneol and bornyl acetate) presented in the TCM were applied to evaluating the quality of Flos Chrysanthemi Indici from 20 various areas. The quality assessment was successfully performed to compare the similarity value (S) between different sample vector of Flos Chrysanthemi Indici and the standard profile vector (SPV). The results showed that the proposed HS-SPME-GC-MS was an alternative technique for quality assessment of Flos Chrysanthemi Indici samples.

China↗

PubMed2006

In-tube solid-phase microextraction-capillary liquid chromatography as a solution for the screening analysis of organophosphorus pesticides in untreated environmental water samples.

This paper describes a method for the selective screening of organophosphorus pesticides in water. In-tube solid-phase microextraction (SPME) in an open capillary column coupled to capillary liquid chromatography (LC) with UV detection has been used to effect preconcentration, separation and detection of the analytes in the same assembly. For in-tube SPME two capillary columns of the same length and different internal diameters and coating thicknesses have been tested and compared, a 30 cm x 0.25 mm I.D., 0.25 micro m thickness coating column, and a 30 cm x 0.1 mm I.D., 0.1 micro m of coating thickness column. In both columns the coating was 95% dimethylpolysiloxane (PDMS)-5% diphenylpolysiloxane. The proposed methodology provided limits of detections (LODs) for the tested organophosphorus pesticides in the 0.1-10 micro g/L range, whereas the direct injection of the samples onto the capillary LC system provided LODs in the 50-1000 micro g/L range. The sensitivity of the proposed in-tube SPME-capillary LC method is adequate to monitorize the analyte levels in drinking water. Several triazines, polycyclic aromatic hydrocarbons (PAHs), nonylphenol, organochloride pesticides or polybrominated diphenyl ethers (PBDEs) have been evaluated as possible interferents. The reliability of the described method is demonstrated by analysing different real water samples.

Chromatography, Liquid↗

PubMed2002

Determination of thymol in human plasma by automated headspace solid-phase microextraction-gas chromatographic analysis.

A reliable and sensitive method was developed for determination of thymol in human plasma by automated headspace solid-phase microextraction (SPME). After enzymatic cleavage of thymol sulfate thymol was extracted by a 65 microm polydimethylsiloxane-divinylbenzene crimped fiber (Supelco) after addition of sodium chloride and phosphoric acid (85%). Desorption of the fiber was performed in the injection port of a gas chromatograph at 220 degrees C (HP 5890; 50 m x 0.2 mm I.D., 0.2 microm HP Innowax capillary column; flame ionization detection). Fibers were used repeatedly up to 40 analysis. The recovery was 5% after 35 min of extraction. The calibration curve was linear in the range of 8.1-203.5 ng ml(-1) with a limit of quantitation (LOQ) of 8.1 ng ml(-1). The within-day and between-day precision and accuracy were < or = 20% at the LOQ and <15% at higher concentrations according to international guidelines for validation of bioanalytical methods. After administration of a thymol-containing herbal extract only thymol sulfate, no free thymol, could be detected in human plasma, thus analysis of thymol was after enzymatic cleavage of thymol sulfate. It is concluded that the newly developed automated method can be used in clinical trials on bioavailability and pharmacokinetics of thymol-containing herbal medicinal products.

Calibration↗

PubMed2005

Determination of volatile compounds in whiting (Merlangius merlangus) using headspace-solid-phase microextraction-gas chromatography-mass spectrometry.

A method using headspace-solid-phase microextraction-gas chromatography-mass spectrometry to extract volatile compounds from whiting is developed. Several parameters such as sorption time, desorption time, fiber type, and matrix form are optimized to achieve better sensitivity in minimal analysis time. The efficiency of the method is determined by the linear range and repeatability; a mean relative standard deviation of approximately 7% is measured. It was possible to identify and quantitate 30 volatile compounds of interest present in spoiled whiting.

Animals↗

PubMed1998

Determination of organoarsenicals in the environment by solid-phase microextraction-gas chromatography-mass spectrometry.

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 400 x 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.

Arsenicals↗

PubMed2003

Determination of linear alkylbenzensulfonates in aqueous matrices by ion-pair solid-phase microextraction-in-port derivatization-gas chromatography-mass spectrometry.

Trace determination (low ng/ml) of linear alkylbenzensulfonates (LASs) in water was achieved by solid-phase microextraction (SPME) of ion-pairs formed with tetrabutylammonium. This ion-pairing reagent served two purposes. First, it allowed the extraction of LAS with the polydimethylsiloxane fiber by counterion association and second, the derivatization of the formed LAS ion pairs in the GC injection port at 300 degrees C to form the corresponding sulfonated butyl esters. The methodology developed allows the isomer specific determination of LAS at low detection limits (0.16-0.8 ng/ml), depending on the alkyl chain lengths of LASs with RSDs of 10-12%. Furthermore, the developed methodology was applied to urban wastewater and sea water and compared with a solid-phase extraction (SPE) method (e.g. C18 and strong anion-exchange sorbent) to obtain concordant values for urban wastewater. Moreover, the developed SPME methodology overcame the procedural blank and matrix-dependent recoveries found in the SPE methodologies at low LAS concentrations.

Alkanesulfonic Acids↗

PubMed2005

Reliable characterization of coffee bean aroma profiles by automated headspace solid phase microextraction-gas chromatography-mass spectrometry with the support of a dual-filter mass spectra library.

This investigation is based on the automated solid phase microextraction GC-MS analysis of the volatile fraction of a variety of coffee bean matrices. Volatile analytes were extracted by headspace (HS)-SPME which was achieved with the support of automated instrumentation. The research was directed towards various important aspects relating to coffee aroma analysis: monitoring of the volatile fraction formation during roasting; chromatographic differentiation of the two main coffee species (Arabica and Robusta) and of a single species from different geographical origins; evaluation of the influence of specific industrial treatments prior to roasting. Reliable peak assignment was carried out through the use of a recently laboratory-constructed "flavour and fragrance" library and a dual-filter MS spectral search procedure. Further emphasis was placed on the automated SPME instrumentation and on its ability to supply highly repeatable chromatographic data.

Coffee↗

PubMed2001

Screening for sarin in air and water by solid-phase microextraction-gas chromatography-mass spectrometry.

A method of screening air and water samples for the chemical-warfare agent Sarin is developed using solid-phase microextraction (SPME)-gas chromatography (GC)-mass spectrometry (MS). The SPME field kit sampler is ideal for collecting air and water samples in the field and transporting samples safely to the laboratory. The sampler also allows the sample to be introduced into the GC-MS system without further sample preparation. Results of the tests with Sarin using the SPME technique indicate that a sample collection time of 5 min is sufficient to detect 100 ng/L of Sarin in air. For water samples, Sarin is detected at a concentration of 12 microg/mL or higher. This method is ideal for screening samples for quick response situations.

Air↗

PubMed2003

Determination of amitraz in canine plasma by solid-phase microextraction-gas chromatography with thermionic specific detection.

A simple and rapid analytical method is presented for the determination of amitraz in canine plasma samples using solid-phase microextraction (SPME) and gas chromatography with thermionic specific detection (GC-TSD). The best conditions for the SPME procedure were: direct extraction on a polydimethlysiloxane (PDMS) fiber with 100-microm film thickness; 400 &microl of sample plasma matrix modified with 4 ml sodium borate solution (0.01 mol l(-1), pH 6.5); extraction temperature 70 degrees C, with stirring at 2500 rpm for 45 min. The method was linear between 20 and 400 ng ml(-1) with regression coefficients corresponding to 0.998 and coefficient of the variation of the points of the calibration curve lower than 15%. The lowest limit of quantification (LOQ) for amitraz in plasma was 20 ng ml(-1). This LOQ was determined as the lowest concentration on the calibration curve in which the coefficient of variation was lower than 15%. The proposed method was applied to determine amitraz concentrations in canine plasma to look for toxicity after treatment with amitraz in a dipping bath.

Animals↗

PubMed2001

Solid-phase microextraction-mass spectrometry: a new approach to the rapid characterization of cheeses.

This work describes a new method for the rapid characterization of cheeses by solid-phase microextraction coupled with mass spectrometry (SPME-MS). After four types of fiber were tested and the main extraction parameters studied, the volatile components were extracted using a Carboxen/PDMS 75-microm fiber placed for 10 min at 20 degrees C in the headspace of the cheese. The substances adsorbed were then transferred directly from the injector to the inlet of a mass spectrometer through a 1-m deactivated silica capillary column heated to 210 degrees C. The mass spectra thus obtained without prior chromatographic separation formed a "fingerprint" of the analyzed sample. For data analysis, the mass fragments of each spectrum (45 < m/z < 150 amu) were considered as potential descriptors of the composition of the headspace of the cheeses. Stepwise discriminant analysis was used to select a limited number of mass fragments that afforded an operational classification of the batches of cheeses studied. This new method offers the advantage of minimizing thermal, mechanical, and chemical modifications of the matrix, thereby reducing the risk of analytical artifacts. SPME-MS provides a simple and effective approach to rapid quality control by analysis of the volatile fraction of foods.

Cheese↗

PubMed2004

Solid-phase microextraction-gas chromatography-mass spectrometric analysis of volatile compounds in a compounded Chinese medicinal prescription, Xiao-Cheng-Qi-Tang.

In this paper, a headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS) was applied for the analysis of volatile compounds in a famous compounded Chinese medicinal prescription, Xiao-Cheng-Qi-Tang. Some parameters affecting the extraction efficiency such as stirring, extraction temperature, fiber exposure time and desorption time were optimized. The best results were obtained using a 100 microm PDMS fiber during headspace extraction at 90 degrees C with stirring at 1000 rpm for 20 min. Twenty-seven compounds were identified in Xiao-Cheng-Qi-Tang including some main compounds such as d-limonene and linalool. Inter- and intra-day relative standard deviations (R.S.Ds.) were less than 15.6%, showing that the method had a good reproducibility. The result might provide some foundation for building the convincing theory on the pharmacological activity of this prescription.

Drugs, Chinese Herbal↗

PubMed2002

Aroma analysis of fresh and preserved onions and leek by dual solid-phase microextraction-liquid extraction and gas chromatography-mass spectrometry.

The lachrymatory factor (thiopropanal-S-oxide) was directly analysed on fresh onion (Allium cepa) juice by solid-phase microextraction (polyacrylate fibre) using a fast routine GC-MS method on a 10 m x 0.32 mm I.D. (4 microm thick polydimethylsiloxane film) column with splitless mode injection. The identification and quantification of thiosulphinates and zwiebelanes were obtained on the same juice extracted by diethyl ether after 80 min maceration using the same GC-MS method. Selected ion recording enhanced the differentiation possibilities and the detection limits. This dual method was used to evaluate flavour differences between onion and shallot varieties as it provides accurate profiles of all initially formed compounds. Moreover, this method allowed us to compare qualitatively and quantitatively transformed products: frozen, freeze-dried powders and sterilised products. Excepting the lachrymatory factor, frozen onion compounds were similar compared to those of fresh onion sample. Conversely, the other transformed samples have lost most of the initially formed compounds and produced mainly di- and trisulphides corresponding to the degradation of thiosulphinates and zwiebelanes. These dramatic changes can explain the very different flavours of these manufactured products compared to fresh material.

Food Preservation↗

PubMed2002

Determination of methylmercury in human hair by ethylation followed by headspace solid-phase microextraction-gas chromatography-cold-vapour atomic fluorescence spectrometry.

An analytical procedure for the determination of methylmercury in human hair after acid digestion using aqueous ethylation, headspace solid-phase microextraction sampling and final gas chromatography-cold-vapour atomic fluorescence spectrometry detection is described. Acid digestion, extraction procedure and chromatographic conditions were optimised. An optimal linear range using standard mercury solutions was found and concentration detection limits for the mercury species, MeHg and Hg2+, were about 50 and 80 ng/g, respectively, for 100 mg of human hair. The reproducibility of the developed analytical procedure assessed for hair samples with incurred MeHg was better than 18% (n=5). A certified reference material from the National Institute of Environmental Studies (Japan) was used for validation. Analysis of human hair collected from urban inhabitants was performed and the mean value of methylmercury content in hair samples was 0.764 +/- 0.732 microg/g for the population tested. The developed analytical method is simple, fast and a suitable procedure for the monitoring and screening of human exposure to methylmercury.

Chromatography, Gas↗

PubMed2004

Determination of perfluorocarboxylic acids in aqueous matrices by ion-pair solid-phase microextraction-in-port derivatization-gas chromatography-negative ion chemical ionization mass spectrometry.

A rapid, selective and simple analytical procedure using tetrabutylammonium as ion pair in conjunction with solid-phase microextraction followed by in-port derivatization-GC-negative ion chemical ionization mass spectrometry was developed. The procedure allows an accurate determination of perfluoroalkylcarboxylic acids in aqueous samples at ng L(-1) levels (i.e. method detection limit 20 ng L(-1) forperfluorodecanoic acid) improving previous GC methods in terms of analysis time and sensitivity. Ammonia as reagent gas in the negative ion chemical ionization mass spectrometry increased the sensitivity at least 3-fold compared to methane for perfluorocarboxylic acid butyl esters. The developed procedure was successfully applied to effluents from wastewater treatment plants (i.e. 0.05-8.2 microg L(-1)) and harbor seawaters.

Carboxylic Acids↗

PubMed2001

Polydimethylsiloxane solid-phase microextraction-gas chromatography method for the analysis of volatile compounds in wines. Its application to the characterization of varietal wines.

A study was made of the validity of the solid-phase microextraction method, using a polydimethylsiloxane coated fused-silica fiber, for the extraction-desorption of the minor volatile compounds from wine before their gas chromatographic analysis. The aspects considered were the influence of ethanol on extraction, repeatability, limits of detection, linearity and recovery of compounds. This method, together with the direct injection of the major volatile compounds, was applied to 16 varietal wines. The findings indicate that the method is a highly suitable technique for the analysis of wines and that the volatile composition of wines depends, at least partly, on the grapes with which they have been made.

Chromatography, Gas↗

PubMed2002

Classification of Nebbiolo-based wines from Piedmont (Italy) by means of solid-phase microextraction-gas chromatography-mass spectrometry of volatile compounds.

Sixty-eight samples of wines from Piedmont (Italy) were analysed to determine their content of volatile compounds, using the solid-phase microextraction (SPME) technique coupled with gas chromatography-mass spectrometry (GC-MS). Samples were from five groups of wines: Barolo, Barbaresco, Nebbiolo d'Alba, Roero and Langhe Nebbiolo, all produced from the Nebbiolo grape in the Langhe and Roero areas (province of Cuneo, Piedmont) but differing in vintage (respectively, 3 years, 2 years, 1 year, 8 months and few months) and production zone. Thirty-five analytes were identified; peak area data, corrected for internal standard, were used for pattern recognition treatments. Principal components analysis, hierarchical cluster analysis, Kohonen self organising map, stepwise linear discriminant analysis and soft independent modelling of class analogy were applied to the data, revealing a good separation between the five groups. A main factor, strictly connected to wine vintage, was identified and found to be related to some analytes.

Cluster Analysis↗

PubMed2004

Further solid-phase microextraction-gas chromatography-mass spectrometry applications: "on-fibre" and aqueous photodegradation of nitro musks.

Photodegradation kinetics of four nitro musks (musk xylene, musk tibetene, musk ketone and musk moskene) in solid-phase microextraction (SPME) fibres ("photo-SPME") and in an aqueous system were studied by means of gas chromatography-mass spectrometry (MS) detection. Musks fragrances were extracted from aqueous solutions using SPME fibres that subsequently were exposed to different UV irradiation times, generating photoproducts easily characterized by their mass spectra. Aqueous photodegradation studies followed by SPME were also performed and compared to photo-SPME. The same fourteen photoproducts have been detected in both media. The potential of this approach to readily calculate apparent rate constants (from 10(-4) to 10(-3) s(-1)), half-life times (from 3 to 32 min) and reaction orders (n = 1) in both media is stated. The main photoreaction determined was photocyclization, but products of photoreduction and photorearrangement have also been detected. Tentative photodegradation pathways for musk moskene and musk tibetene are proposed for the first time.

Gas Chromatography-Mass Spectrometry↗

PubMed2006

Determination of chlorinated volatile organic compounds in water and municipal wastewater using headspace-solid phase microextraction-gas chromatography.

The aim of this work was to develop a fast and simple analytical method for the determination of 14 chlorinated volatile organic compounds (VOCs) in water and wastewater samples. Headspace-solid-phase microextraction (HS-SPME) and gas chromatography (GC) were used for the determination of the VOCs. The extraction parameters were investigated in order to optimize the HS-SPME-GC method. The quality parameters of the method were also investigated.

Chromatography, Gas↗