Headspace Gas Chromatography-mass Spectrometry Method Research Articles

Determination and Quantification of Acetaldehyde, Acetone, and Methanol in Hand Sanitizers Using Headspace GC/MS: Effect of Storage Time and Temperature.

Accurate determination of the concentration of alcohols and their metabolites is important in forensics and in several life science areas. A new headspace gas chromatography-mass spectrometry method has been developed to quantify alcohols and their oxidative products using isotope-labeled internal standards. The limit of detection (LOD) of the analytes in the developed method was 0.211 µg/mL for methanol, 0.158 µg/mL for ethanol, 0.157 µg/mL for isopropanol, 0.010 µg/mL for n-propanol, 0.157 µg/mL for acetone, and 0.209 µg/mL for acetaldehyde. The precision and accuracy of the method were evaluated, and the relative standard deviation percentages were found to be less than 3%. This work demonstrates the application of this method, specifically in quantifying the concentration of oxidative products of alcohol and other minor alcohols found in hand sanitizers, which have become an essential household item since the COVID-19 pandemic. Apart from the major components, the minor alcohols found in hand sanitizers include methanol, isopropanol, and n-propanol. The concentration range of these minor alcohols found in ethanol-based hand sanitizer samples was as follows: methanol, 0.000921-0.0151 mg/mL; isopropanol, 0.454-13.8 mg/mL; and n-propanol, 0.00474-0.152 mg/mL. In ethanol-based hand sanitizers, a significant amount of acetaldehyde (0.00623-0.231 mg/mL) was observed as an oxidation product, while in the isopropanol-based hand sanitizer, acetone (0.697 mg/mL) was observed as an oxidation product. The concentration of acetaldehyde in ethanol-based hand sanitizers significantly increased with storage time and temperature, whereas no such increase in acetone concentration was observed in isopropanol-based hand sanitizers with storage time and temperature. In two of the selected hand sanitizers, the acetaldehyde levels increased by almost 200% within a week when stored at room temperature. Additionally, exposing the hand sanitizers to a temperature of 45 °C for 24 h resulted in a 100% increase in acetaldehyde concentration. On the contrary, the acetone level remained constant upon the change in storage time and temperature.

An ex vivo headspace gas chromatography-mass spectrometry method for the determination of short-chain siloxanes in silicon oil tamponades used in ophthalmic surgery

Being able to facilitate retinal reattachment by preventing water migration into the subretinal space, silicone oils are widely used as long-term intraocular tamponade to treat cases of retinal detachment. Various commercial tamponades constituted by linear polydimethylsiloxane polymers with different molecular weights and cyclic impurities are available. In this study, for the first time, an untargeted headspace-gas-chromatography-mass spectrometry (HS-GC-MS) method was developed to identify low-molecular weight contaminants in three different types of silicone oil tamponades, namely Siluron 2000, RS-OIL ECS5000 and Densiron Xtra. Both commercial and post-operative tamponades were analysed to screen for the different classes of compounds present in the samples. The most abundant classes were short-chain siloxanes, fluorinated compounds, and hydrocarbons. To quantify the siloxanes present in the samples, a targeted HS-GS-MS was optimized using a central composite design and validated according to guidelines for bioanalytical methods. Lower limits of quantification in the low μg/L range, good precision with RSD% < 12% and accuracy with recovery rates in the 81 ( ± 7) – 96 ( ± 4) % range were achieved. Short-chain siloxanes were quantified in both commercial and post-operative tamponades, being the RS-OIL ECS5000 characterized by the highest concentration levels of the investigated analytes. By contrast, Densiron Xtra tamponades showed the lowest amount of short-chain siloxanes, observing a general decrease in their concentration levels according to the residence time in the eyes.

Application of Static Headspace GC-MS Method for Selective 1,4-Dioxane Detection in Food Additives.

Efficient detection methods must be developed for 1,4-dioxane due to its suspected status as a human carcinogen, which is highly mobile in food and environmental resources. In this regard, this experiment has been conducted to develop reliable and selective detection and measurement methods by using static headspace (SH) isolation, followed by gas chromatography-mass spectrometry (GC-MS). A new method was developed for determining the spiked 1,4-dioxane contents in a polyethylene glycol 600 (PEG 600). The optimal condition for SH-GC-MS was discussed. The representative ions of 1,4-dioxane and 1,4-dioxane-d8 in the SIM mode of MS are 88 and 96, respectively, and the peaks of the SIM mode were separated and confirmed. The linear range for the method covers 0.25 to 100 mg/L with a coefficient of determination (R2) ≥ 0.999. The method applicability was demonstrated by spike recovery across a variety of food additives (i.e., chlorine bitartrate, choline chloride, polysorbate 20 and 60, and PEG 1000). All spike recovery from the tested samples was in the range of 89.50-102.68% with a precision of 0.44-11.22%. These findings suggest a new analytical method for food safety inspection, and could be applicable for ensuring the safety of foods and environmental and public health on a broad scale.

Optimization of a static headspace GC-MS method and its application in metabolic fingerprinting of the leaf volatiles of 42 citrus cultivars.

Citrus leaves, which are a rich source of plant volatiles, have the beneficial attributes of rapid growth, large biomass, and availability throughout the year. Establishing the leaf volatile profiles of different citrus genotypes would make a valuable contribution to citrus species identification and chemotaxonomic studies. In this study, we developed an efficient and convenient static headspace (HS) sampling technique combined with gas chromatography-mass spectrometry (GC-MS) analysis and optimized the extraction conditions (a 15-min incubation at 100 ˚C without the addition of salt). Using a large set of 42 citrus cultivars, we validated the applicability of the optimized HS-GC-MS system in determining leaf volatile profiles. A total of 83 volatile metabolites, including monoterpene hydrocarbons, alcohols, sesquiterpene hydrocarbons, aldehydes, monoterpenoids, esters, and ketones were identified and quantified. Multivariate statistical analysis and hierarchical clustering revealed that mandarin (Citrus reticulata Blanco) and orange (Citrus sinensis L. Osbeck) groups exhibited notably differential volatile profiles, and that the mandarin group cultivars were characterized by the complex volatile profiles, thereby indicating the complex nature and diversity of these mandarin cultivars. We also identified those volatile compounds deemed to be the most useful in discriminating amongst citrus cultivars. This method developed in this study provides a rapid, simple, and reliable approach for the extraction and identification of citrus leaf volatile organic compound, and based on this methodology, we propose a leaf volatile profile-based classification model for citrus.

Quantitation of ethanol in UTI assay for volatile organic compound detection by electronic nose using the validated headspace GC-MS method.

Disease detection through gas analysis has long been the topic of many studies because of its potential as a rapid diagnostic technique. In particular, the pathogens that cause urinary tract infection (UTI) have been shown to generate different profiles of volatile organic compounds, thus enabling the discrimination of causative agents using an electronic nose. While past studies have performed data collection on either agar culture or jellified urine culture, this study measures the headspace volume of liquid urine culture samples. Evaporation of the liquid and the presence of background compounds during electronic nose (e-nose) device operation could introduce variability to the collected data. Therefore, a headspace gas chromatography-mass spectrometry method was developed and validated for quantitating ethanol in the headspace of the urine samples. By leveraging the new method to characterize the sample stability during e-nose measurement, it was revealed that ethanol concentration dropped more than 15% after only three measurement cycles, which equal 30 minutes for this study. It was further shown that by using only data within the first three cycles, better accuracies for between-day classification were achieved, which was 73.7% and 97.0%, compared to using data from within the first nine cycles, which resulted in 65.0% and 81.1% accuracies. Therefore, the newly developed method provides better quality control for data collection, paving ways for the future establishment of a training data library for UTI.

Brewing on an industrial and a craft scale – impact on the physicochemical properties and volatile compounds profile of the pale pilsener-style lager beer analysed with HS/GC-MS

The pale Pilsener-style lager beers produced on a massive and craft scale were taken to analyse their basic physicochemical properties (alcohol content, pH, haze, real degree of fermentation) and volatile compounds profiles. The research was carried out using a beer analyser equipment and a headspace gas chromatography-mass spectrometry method (HS/GC-MS). The findings showed that in terms of physicochemical and flavour attributes, the quality of craft beers differed to a higher degree from the standard Pilsener beer quality than in the case of industrial beers.

Ethanol Concentration of Kombucha Teas in British Columbia, Canada

Kombucha is a sweetened tea beverage fermented by bacterial and yeast cultures. Sweeteners, such as glucose, sucrose, fructose, and others are converted by yeasts into ethanol and then by Acetobacter and other bacterial species into a weak acetic acid solution that is diluted, flavored, and packaged into glass or aluminum cans for consumer consumption. Naturally, fermented kombucha contains 0 to 3% alcohol by volume (ABV). However, kombucha containing ethanol is concerning for pregnant women and young children for whom low levels of ethanol consumption (<3% ABV) create adverse medical outcomes. In the province of British Columbia (BC), Canadian beverages containing >1% ABV are regulated as liquor. This study assessed ethanol concentrations in kombucha collected from processors and purchased at retail venues in BC. Ethanol values were compared with the place of manufacture (country or province) and place of purchase (grocery stores, restaurants, farmers' markets, recreational centers, and processors). Ethanol (n = 684) levels were measured by using a headspace gas chromatography-mass spectrometry method with a detection limit of 0.0002% ABV for ethanol. Overall, teas contained mean and median ethanol of 0.77 and 0.62% ABV, respectively, ranging from nondetectable up to 3.62% ABV. Four kombucha teas (0.6%) made by BC processors tested over 3% ABV, and 31.5% of samples contained ethanol that exceeded the BC regulatory limits for nonalcoholic beverages of 1% ABV. Kombucha manufactured in BC had significantly higher mean ethanol values (1.16% ABV) in comparison to all other places of manufacture. Similarly, mean ethanol tea values obtained from BC processors (1.2% ABV) and restaurants (1.01% ABV) were significantly higher than those obtained at other retail venues. This study demonstrates the potential for alcohol harm to at-risk populations consuming kombucha teas sold in BC.

Development of a Sensitive Headspace Gas Chromatography-Mass Spectrometry Method for the Simultaneous Determination of Nitrosamines in Losartan Active Pharmaceutical Ingredients.

Nitrosamine impurities in angiotensin II receptor antagonists (sartans) containing a tetrazole group represent an urgent concern for active pharmaceutical ingredient (API) manufacturers and global regulators. Regarding safety, API manufacturers must develop methods to monitor the levels of each nitrosamine impurity before individual batch release. In this study, we developed and validated a sensitive, selective, and high-throughput method based on headspace gas chromatography–mass spectrometry (HS-GC–MS) for the simultaneous determination of four nitrosamines in losartan potassium API with simple sample preparation. N-Nitrosodimethylamine (NDMA, m/z 74), N-nitrosodiethylamine (NDEA, m/z 102), N-nitrosoethylisopropylamine (EIPNA, m/z 116), and N-nitrosodiisopropylamine (DIPNA, m/z 130) levels were quantified using an electron impact, single quadrupole mass spectrometer under a selected-ion-monitoring acquisition method. The method was validated according to the Q2(R1) ICH guidelines. The calibration curves of the assay ranged from 25 to 5000 ng/mL with limits of quantitation of 25 ppb for NDMA and NDEA and 50 ppb for DIPNA and EIPNA. The accuracy of the developed method ranged from −7.04% to 7.25%, and the precision %CV was ≤11.5. Other validation parameters, including specificity, stability, carryover, and robustness, met the validation criteria. In conclusion, the developed method was successfully applied for the determination of nitrosamines in losartan potassium APIs.

Headspace gas chromatography-mass spectrometry method for the determination of total cyanide concentration in water and postmortem blood samples

In this study, we aimed to develop a headspace gas chromatography? ?mass spectrometry method for determining the total cyanide concentration in the forensic evidences. Total cyanide content of the samples was calculated based on the hydrogen cyanide gas concentration evaporated from the liquid sample in the headspace vial. Hexacyanoferrate(II) was used for the optimization of headspace oven temperature. We have found that iron?cyanide bonds were completely degraded after 0.2 mL of the sample was treated with 1 mL of 1 M sulfuric acid under the optimized headspace conditions where the temperature and the heating time were 120 ?C and 12.5 min, respectively. Satisfactory recovery results for both aqueous and blood samples were obtained. The method was linear in the range 0.05?10 ?g mL-1 of cyanide which was a suitable range for toxicological investigations. The proposed method was validated and applied to the post-mortem blood samples, drinking waters, and the other forensic evidences. The proposed method can easily be performed not only in the forensic laboratories, but in the related laboratories where the total cyanide analysis is a critical issue.

Volatile sulfur compounds: The possible metabolite pattern to identify the sources and types of asafoetida by headspace GC/MS analysis

Volatile sulfur compounds of asafoetida, an oleo-gum-resin, obtained from different Ferula species may be considered as possible metabolites to determine the probable source. Asafoetida is widely used in Iranian and Indian traditional medicine and in food industry. Sesquiterpene coumarin, phenolic, and volatile compounds (especially sulfur compounds) can be used as evidence to find out the main asafoetida and their source(s). In this study, the volatile profiles of five Ferula species and six samples of asafoetida from eastern and southern Iran were investigated via the headspace gas chromatography-mass spectrometry method. Heat map analysis was performed for comparing the sulfur pattern in samples. The results showed at least two types of asafoetida in these regions were produced from special Ferula species. Accordingly, Ferula lutensis Rech., was determined as the main source of asafoetida from eastern Iran due to the presence of Z-1-butynyl-1-methyl propyl disulfide and E-1-butynyl-1-methyl propyl disulfide. The results of this research support the idea that types and levels of sulfur compounds could be considered as lead compounds for determination of the main source(s) of asafoetida.

Development and uncertainty estimation of cryogenic homogenization and static headspace–gas chromatography–mass spectrometry method for the simultaneous determination of twelve toxic volatiles in disposable menstrual products

Volatile organic compounds (VOCs) threaten the health of women who use disposable menstrual products (DMPs). In this study, we aimed to develop a simple and reliable analytical method using a cryogenic mill and static headspace–gas chromatography–mass spectrometry (HS-GC-MS) for the simultaneous determination of twelve toxic VOCs in DMPs, and estimate the measurement uncertainty of the method using the bottom-up approach to ensure the quality of analytical results. Static HS conditions for the direct thermal extraction of the target VOCs from the cryogenically ground sample powders were optimized in terms of extraction temperature and equilibrium time. The separation was achieved using a GC-MS equipped with a VF-624ms column. Cryogenic mill homogenized DMP into powder with 100-μm particles in scanning electron microscopy study. Sample powder was demonstrated to be homogenous as assessed by the homogeneity test. Validation studies showed that the method has reliable performance characteristics: linearity (R2 ≥ 0.9994), limit of quantification (LOQ, 8.4–50.5 ng g−1), precision (relative standard deviation ≤ 18.7%), and accuracy (recovery = 83.4–114.2%) for all the analytes. The proposed method was successfully applied to the commercial products of disposable sanitary pads and tampons. The content of styrene was the highest, followed by those of toluene, hexane, and ethylbenzene. The quantitative data exhibited acceptable precision, as evaluated using the intra-laboratory Horwitz ratio. The expanded uncertainties estimated at three concentration levels ranged from 6.4% to 77.9%. Our simple and reliable method will be useful for quality control testing or quantitative risk assessment and will contribute to resolving the safety issues associated with the risk of human exposure to trace volatile residues in DMPs.

Spatio-vertical characterization of the BTEXS group of VOCs in Chinese agricultural soils

Ubiquitous contamination of the BTEXS (benzene, toluene, ethylbenzene, xylene, and styrene) group in soils is a significant concern for ecological safety. However, comprehensive spatio-vertical survey of the BTEXS group on a national scale is rare to date. Using a static headspace gas chromatography–mass spectrometry method (HS-GCMS), this study performed a quantitative analysis of BTEXS levels in soils from Chinese rural areas in 2013 and 2016. The median ∑BTEXS concentrations in surface soils in 2013 and 2016 were 37.5 and 34.4 ng g−1 dry weight, respectively. Toluene was the dominant pollutant, accounting for approximately 41.6% and 32.1% of the total levels. BTEXS contamination was higher in Shanxi province, Northeast China, and Yunnan-Guizhou Plateau compared to the other regions. Vertically, toluene, m,p′-xylene and o′-xylene concentrations were significantly higher in the top soil layer (0–15 cm) and decreased significantly with increasing soil depth (p < 0.05). Higher soil organic matter was significantly associated with higher BTEXS concentrations of sampling site. BTEXS was also enhanced at sites with higher elevations and lower temperature due to global distillation effects. The findings of this study could help decision-makers to protect against BTEXS contamination in rural areas. These findings provide a basis for further study of the mechanism of BTEXS migration and transport in large-scale environment. CapsuleSpatio-vertical distribution, influence factors, exposure risks of BTEXS in soils from Chinese agricultural region was studied.

Effect of Fermentation Temperature on the Volatile Composition of Kimchi.

This study was conducted to evaluate the effect of fermentation temperature on the volatile composition in Kimchi. Kimchi was fermented at 2 temperature conditions (4 and 20 °C). Volatile compounds of Kimchi samples were analyzed during the fermentation periods using the dynamic headspace gas chromatography-mass spectrometry method. The optimum ripening time for the Kimchi fermented at 4 °C was 35 d, and that of 20 °C was 2 d. The pH at the optimum ripening time was 4.97 and 4.41, and the titratable acidity was 0.59% and 0.76% for the Kimchi fermented at 4 and 20 °C, respectively. Forty different types of volatile compounds, including alcohol, aldehyde, ester, and sulfur compounds, were identified. The Kimchi fermented at 20 °C produced greater amounts of volatile compounds than that at 4 °C. The amounts of most volatiles increased as the fermentation time increased, but those of aldehydes decreased rapidly during both 4 and 20 °C fermentation. Organic acids, ester, and nitriles were detected only in Kimchi fermented at 20 °C. The amounts of dimethyl disulfide, methyl-2-propenyl disulfide, and di-2-propenyl disulfide produced from the Kimchi fermented at 20 °C were more than 2-times of those at 4 °C. Therefore, it is concluded that the strong pungent odor of Kimchi fermented at 20° C is probably due to the high amount of organic acids (low pH) and sulfur compounds (dimethyl disulfide, methyl-2-propenyl disulfide, and di-2-propenyl disulfide) between the 2 Kimchi.

A comparative study of three tissue-cultured Dendrobium species and their wild correspondences by headspace gas chromatography–mass spectrometry combined with chemometric methods

Plant tissue culture technique is widely used in the conservation and utilization of rare and endangered medicinal plants and it is crucial for tissue culture stocks to obtain the ability to produce similar bioactive components as their wild correspondences. In this paper, a headspace gas chromatography–mass spectrometry method combined with chemometric methods was applied to analyze and evaluate the volatile compounds in tissue-cultured and wild Dendrobium huoshanense Cheng and Tang, Dendrobium officinale Kimura et Migo and Dendrobium moniliforme (Linn.) Sw. In total, 63 volatile compounds were separated, with 53 being identified from the three Dendrobium spp. samples. Different provenances of Dendrobiums had characteristic chemicals and showed remarkable quantity discrepancy of common compositions. The similarity evaluation disclosed that the accumulation of volatile compounds in Dendrobium samples might be affected by their provenance. Principal component analysis showed that the first three components explained 85.9% of data variance, demonstrating a good discrimination between samples. Gas chromatography–mass spectrometry techniques, combined with chemometrics, might be an effective strategy for identifying the species and their provenance, especially in the assessment of tissue-cultured Dendrobium quality for use in raw herbal medicines.

Antioxidant Compounds in Traditional Indian Pickles May Prevent the Process-Induced Formation of Benzene

Pickles in the Indian market contain ascorbic acid from the raw material used and benzoate as an added preservative that are involved in the formation of benzene in soft drinks. In this work, 24 market pickle samples were surveyed for benzene content, as well as its precursors and other constituents that influence its formation. The analysis showed that pickle samples were high in acid content (low pH) and showed significant amount of ascorbic acid, minerals (Cu and Fe), and benzoic acid present in them. Also, most samples exhibited high antioxidant activity that might be attributed to the ingredients used, such as fruits and spices. The solid-phase microextraction headspace gas chromatography-mass spectrometry method was developed in-house for benzene analysis. Eleven of 24 samples had benzene, with the highest concentration of 4.36 ± 0.82 μg of benzene per kg of pickle for a lime pickle that was also reported to have highest benzoic acid and considerably less hydroxyl radical ((•)OH) scavenging activity. However, benzene levels for all 11 samples were considerably below the World Health Organization regulatory limit of 10 μg/kg for benzene in mineral water. Studies on model systems revealed that the high antioxidant activity of Indian pickles may have had a strong inhibitory effect on benzene formation.

Magnetic solid phase extraction and static headspace gas chromatography–mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons

A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC–MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8ng/L. Good values for intra and inter-day precision were obtained (RSDs≤9.9%). The proposed method was successfully applied to drinking water samples.

Development of a dynamic headspace gas chromatography–mass spectrometry method for on-site analysis of sulfur mustard degradation products in sediments

Sampling teams performing work at sea in areas where chemical munitions may have been dumped require rapid and reliable analytical methods for verifying sulfur mustard leakage from suspected objects. Here we present such an on-site analysis method based on dynamic headspace GC–MS for analysis of five cyclic sulfur mustard degradation products that have previously been detected in sediments from chemical weapon dumping sites: 1,4-oxathiane, 1,3-dithiolane, 1,4-dithiane, 1,4,5-oxadithiephane, and 1,2,5-trithiephane. An experimental design involving authentic Baltic Sea sediments spiked with the target analytes was used to develop an optimized protocol for sample preparation, headspace extraction and analysis that afforded recoveries of up to 60–90%. The optimized method needs no organic solvents, uses only two grams of sediment on a dry weight basis and involves a unique sample presentation whereby sediment is spread uniformly as a thin layer inside the walls of a glass headspace vial. The method showed good linearity for analyte concentrations of 5–200ng/g dw, good repeatability, and acceptable carry-over. The method's limits of detection for spiked sediment samples ranged from 2.5 to 11μg/kg dw, with matrix interference being the main limiting factor. The instrumental detection limits were one to two orders of magnitude lower. Full-scan GC–MS analysis enabled the use of automated mass spectral deconvolution for rapid identification of target analytes. Using this approach, analytes could be identified in spiked sediment samples at concentrations down to 13–65μg/kg dw. On-site validation experiments conducted aboard the research vessel R/V Oceania demonstrated the method's practical applicability, enabling the successful identification of four cyclic sulfur mustard degradation products at concentrations of 15–308μg/kg in sediments immediately after being collected near a wreck at the Bornholm Deep dumpsite in the Baltic Sea.

Application of chemometric analysis based on physicochemical and chromatographic data for the differentiation origin of plant protection products containing chlorpyrifos

The aim of this study was to investigate the similarities and dissimilarities between the pesticide samples in form of emulsifiable concentrates (EC) formulation containing chlorpyrifos as active ingredient coming from different sources (i.e., shops and wholesales) and also belonging to various series. The results obtained by the Headspace Gas Chromatography–Mass Spectrometry method and also some selected physicochemical properties of examined pesticides including pH, density, stability, active ingredient and water content in pesticides tested were compared using two chemometric methods. Applicability of simple cluster analysis and also principal component analysis of obtained data in differentiation of examined plant protection products coming from different sources was confirmed. It would be advantageous in the routine control of originality and also in the detection of counterfeit pesticides, respectively, among commercially available pesticides containing chlorpyrifos as an active ingredient.

Rapid and Sensitive Headspace Gas Chromatography-Mass Spectrometry Method for the Analysis of Ethanol in the Whole Blood

For the forensic aim, a sensitive and specific method using headspace gas chromatography coupled with mass spectrometry (GC/MS) has been developed for the quantitative determination of ethanol in blood using n-propanol as internal standard. GC was performed in isothermal mode with a GC run-time of 5.0 min. The quantification was performed using selected ions monitoring mode adopting a quantitative ion and qualifier ion for ethanol and the internal standard. The method was linear (r(2) = 0.999, in the concentration range of 39.5-1,262.9 μg/ml), specific, sensitive (limit of quantification and limit of detection of 39.5 and 0.4 μg/ml, respectively), and robust. A slightly modified method was also developed for the quantification of 50 commonly abused drunken in blood. The method used an isothermal GC program with a run-time of 5.0 min. The quantification was performed using selected ions monitoring mode and integrating the area under the peak using n-propanol as an internal standard. The method was linear 40-1,263 μg/ml and sensitive. The method was proved superior in speed and selectivity to previously reported methods and was successfully applied to the pharmacokinetic study of ethanol.

Analysis of furan in heat-processed foods in China by automated headspace gas chromatography-mass spectrometry (HS-GC-MS)

In order to assess furan content in thermal processed commercial foods available in China, an optimized automated headspace gas chromatography-mass spectrometry method (HS-GC-MS) was developed and validated. Internal standard d4-furan was used with addition of salt (NaCl) into the headspace with an oven temperature 70 °C and equilibration time 30 min which was coupled with HP-PLOT/Q GC column. The proposed HS-GC-MS method was applied to furan quantization in 11 categories of foods (totally 133 kinds of food samples). Average level of furan detected in ng g−1 for various food products were: infant formula 15.0, bread 4.0, coffee 60.6, fruit juice 5.3, dairy product 1.5, nutritional drink 16.2, canned jam 30.4, spice 9.3, vinegar, 38.3, beer 4.9, and soy sauce 128.8. The results indicated soybean should be one kind of raw materials or precursor that is easier to form furan during food heat processing because soybean contains high fat and protein.