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采用毛细管气相色谱法和离子阱检测器的全蒸发顶空技术:一种定量生物样品中挥发性有机化合物的方法。

A full evaporation headspace technique with capillary GC and ITD: a means for quantitating volatile organic compounds in biological samples.

作者信息

Schuberth J

机构信息

Department of Forensic Chemistry, University Hospital, Linköping, Sweden.

出版信息

J Chromatogr Sci. 1996 Jul;34(7):314-9. doi: 10.1093/chromsci/34.7.314.

DOI:10.1093/chromsci/34.7.314
PMID:8675549
Abstract

The full evaporation technique (FET), which is a variant of headspace analysis used to overcome matrix effects, was combined with capillary gas chromatography (GC) and ion-trap detection (ITD). The aim was to enable quantitative tests of volatile organic compounds (VOCs) in blood and postmortem tissue samples. FET was applied to sample sized less than 35 mg whose VOCs were released from the matrix at an equilibration temperature of 130 degrees C. A capillary column with a nonpolar stationary phase was used for GC, and ITD was performed with the mass spectrometer run in full-scan mode. The potential of FET-GC-ITD was studied for the analysis of blood samples spiked with low concentrations of ethanol, acetone, 2-propanol, and 2-butanone and on brain tissue that contained methyl tert-butyl ether (MTBE), Benzene, toluene, ethylbenzene, o-, m-, and p-xylene, and propylbenzene. Samples were obtained from the bodies of victims who had inhaled smoke during an arson or accidental fire. There was a linear relationship between peak area and sample size, which indicates that the conditions of full evaporation were met and that the matrix effect was negated. The total analyte amount in the test sample at the limit of quantitation was in the range of 0.4-1 nmol for polar VOCs in blood and 0.03-0.1 nmol for nonpolar VOCs in brain tissue. Data on precision and accuracy of the method are reported.

摘要

全蒸发技术(FET)是顶空分析的一种变体,用于克服基质效应,它与毛细管气相色谱(GC)和离子阱检测(ITD)相结合。目的是能够对血液和死后组织样本中的挥发性有机化合物(VOCs)进行定量检测。FET应用于样本量小于35mg的情况,其VOCs在130℃的平衡温度下从基质中释放出来。GC使用具有非极性固定相的毛细管柱,ITD通过在全扫描模式下运行的质谱仪进行。研究了FET-GC-ITD在分析添加了低浓度乙醇、丙酮、2-丙醇和2-丁酮的血液样本以及含有甲基叔丁基醚(MTBE)、苯、甲苯、乙苯、邻二甲苯、间二甲苯、对二甲苯和丙苯的脑组织样本方面的潜力。样本取自纵火或意外火灾中吸入烟雾的受害者尸体。峰面积与样本量之间存在线性关系,这表明满足了全蒸发条件且基质效应被消除。对于血液中的极性VOCs,测试样品在定量限处的总分析物量在0.4 - 1 nmol范围内,对于脑组织中的非极性VOCs,在0.03 - 0.1 nmol范围内。报告了该方法的精密度和准确度数据。

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