Liu Yongzhen, Muralidhara Srinivasa, Bruckner James V, Bartlett Michael G
Department of Pharmaceutical and Biomedical Sciences, The University of Georgia, Athens, GA 30602-2352, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Feb 15;863(1):26-35. doi: 10.1016/j.jchromb.2007.12.010. Epub 2007 Dec 24.
A simple, rapid and sensitive method for determination of trichloroethylene (TCE) in rat blood, liver, lung, kidney and brain, using headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS), is presented. A 100-microm polydimethylsiloxane (PDMS) fiber was selected for sampling. The major analytical parameters including extraction and desorption temperature, extraction and desorption time, salt addition, and sample preheating time were optimized for each of the biological matrices to enhance the extraction efficiency and sensitivity of the method. The lower limits of quantitation for TCE in blood and tissues were 0.25ng/ml and 0.75ng/g, respectively. The method showed good linearity over the range of 0.25-100ng TCE/ml in blood and 0.75-300ng TCE/g in tissues, with correlation coefficient (R(2)) values higher than 0.994. The precision and accuracy for intra-day and inter-day measurements were less than 10%. The relative recoveries of TCE respect to deionized water from all matrices were greater than 55%. Stability tests including autosampler temperature and freeze and thaw of specimens were also investigated. This validated method was successfully applied to study the toxicokinetics of TCE following administration of a low oral dose.
本文介绍了一种使用顶空固相微萃取（HS-SPME）和气相色谱/质谱联用（GC/MS）测定大鼠血液、肝脏、肺、肾脏和大脑中三氯乙烯（TCE）的简单、快速且灵敏的方法。选用100微米的聚二甲基硅氧烷（PDMS）纤维进行采样。针对每种生物基质，对包括萃取和解吸温度、萃取和解吸时间、加盐量以及样品预热时间在内的主要分析参数进行了优化，以提高该方法的萃取效率和灵敏度。血液和组织中TCE的定量下限分别为0.25纳克/毫升和0.75纳克/克。该方法在血液中TCE浓度为0.25 - 100纳克/毫升、组织中TCE浓度为0.75 - 300纳克/克的范围内呈现良好的线性，相关系数（R²）值高于0.994。日内和日间测量的精密度和准确度均小于10%。所有基质中TCE相对于去离子水的相对回收率均大于55%。还研究了包括自动进样器温度以及样品冻融在内的稳定性测试。该经过验证的方法成功应用于研究低口服剂量TCE给药后的毒代动力学。
