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A novel sampling device based on the partition of target analytes to the extraction medium was developed for the determination of sesquiterpenes in air samples. The extraction medium was prepared by the chemical derivatization of a specially prepared macroporous silica, with a specific surface area of 2.0 m2/g. Taking advantage of the sample extraction, which was mainly based on the partition of sesquiterpenes between air and a C18-bonded phase, the extracted analytes were rapidly and quantitatively desorbed just by passing a small amount of desorption solvent for subsequent analysis by gas chromatography with mass spectrometry. Several experimental conditions, such as the sampling volume and temperature, were systematically evaluated. Under optimized conditions, desorption of the extracted analytes was completed within 1 min with a desorption efficiency of more than 99.9%, achieved using 5 mL of acetone for all the evaluated sesquiterpenes. The applicability of the developed device was confirmed by the determination of several sesquiterpenes from coniferous trees. Although further improvements of the device are required for collecting large volumes or high-temperature air samples, the potential of the developed sampling device was confirmed by determining traces of semivolatile organic compounds in air samples. [ABSTRACT FROM AUTHOR]

Very volatile organic compounds (VVOCs), such as methanol, acetaldehyde, ethanol, acetone, acetonitrile, and dichloromethane, were extracted from water samples using a needle-type extraction device based on purge and trap analysis. The extracted analytes could then be determined by gas chromatography–mass spectrometry. By introducing carbon molecular sieves as the extraction medium, aqueous VVOCs could be successfully extracted using the extraction needle. The limit of quantification for methanol, acetaldehyde, ethanol, acetone, acetonitrile, and dichloromethane were 75, 75, 7.5, 0.5, 10 and 0.5 μg/L, respectively. This newly developed method was also successfully applied to the determination of VVOCs in commercial samples, such as fruit juice. [ABSTRACT FROM AUTHOR]

Abstract: Background: Isoprene in human breath is said to be related to cholesterol metabolism, and the possibility of the correlations with some clinical parameters has been studied. However, at this stage, no clear benefit of breath isoprene has been reported for clinical diagnosis. In this work, isoprene and acetone concentrations were measured in the breath of healthy and obese subjects using a needle-type extraction device for subsequent analysis in gas chromatography–mass spectrometry (GC-MS) to investigate the possibility of these compounds as an indicator of possible diseases. Methods: After measuring intraday and interday variations of isoprene and acetone concentrations in breath samples of healthy subjects, their concentrations were also determined in 80 healthy and 17 obese subjects. In addition, correlation between these breath concentrations and the blood tests result was studied for these healthy and obese subjects. Results: The results indicated successful determination of breath isoprene and acetone in this work, however, no clear correlation was observed between these measured values and the blood test results. Conclusions: Breath isoprene concentration may not be a useful indicator for obesity or hypercholesterolemia. [Copyright &y& Elsevier]

Abstract: A novel needle-type sample preparation device was developed for the effective preconcentration of volatile organic compounds (VOCs) in indoor air before gas chromatography–mass spectrometry (GC–MS) analysis. To develop a device for extracting a wide range of VOCs typically found in indoor air, several types of particulate sorbents were tested as the extraction medium in the needle-type extraction device. To determine the content of these VOCs, air samples were collected for 30min with the packed sorbent(s) in the extraction needle, and the extracted VOCs were thermally desorbed in a GC injection port by the direct insertion of the needle. A double-bed sorbent consisting of a needle packed with divinylbenzene and activated carbon particles exhibited excellent extraction and desorption performance and adequate extraction capacity for all the investigated VOCs. The results also clearly demonstrated that the proposed sample preparation method is a more rapid, simpler extraction/desorption technique than traditional sample preparation methods. [Copyright &y& Elsevier]

Abstract: A new approach to the determination of human breath acetone with particle-packed sample preparation needle was developed. The extraction needle was packed with a copolymer of methacrylic acid and ethylene glycol dimethacrylate as the extraction medium. For the analysis of breath sample, exhaled breath was collected in a sampling bag, and 50mL of the breath sample was extracted with the needle-type sample preparation device followed by analysis using gas chromatography–mass spectrometry (GC–MS). After the optimization of several basic extraction conditions for standard acetone samples, breath acetone concentration taken from controlled type-2 diabetic patients was determined. Furthermore, time variations of breath and urine acetone of four healthy individuals under fasting conditions were measured. Urine sample was collected in glass vial, and urine acetone concentration was also determined with the extraction needle by analyzing the corresponding headspace gas. The results demonstrated that the particle-packed extraction needle showed an excellent extraction performance for acetone in both breath and urine headspace samples, and that there is a clear correlation between the concentration of breath acetone and HbA1c level of controlled type-2 diabetic patients. The breath acetone level in controlled diabetic patients was in the range between 0.19 and 0.66ppmv, where its concentration in medically untreated type-2 patient was 0.92 and 1.20ppmv. The breath acetone concentration in healthy male was increased to 5.66ppmv under the 24h of fasting test, and a high correlation between the breath and urine acetone concentration was also observed. On the basis of the above results, the potential applications of the proposed method to the diagnosis of diabetes and/or ketoacidosis were suggested. [Copyright &y& Elsevier]