Schmitt Thomas C
Department of Health and Human Services, FDA Division of Chemistry, HFT-230, National Center for Toxicological Research, 3900 NCTR Road, Jefferson, AR 72079-9502, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Nov 25;780(2):217-24. doi: 10.1016/s1570-0232(02)00371-9.
A sensitive, accurate, and reliable method is described for the quantitative determination of chloral hydrate (CH) and its metabolites in blood plasma of mice and rats. Metabolites of CH include trichloroacetic acid (TCA), trichloroethanol (TCE), and trichloroethanol glucuronide (TCE-Glu). This new method uses capillary gas chromatography with electron-capture detection (GC/ECD). Procedures for improving sample stability and quality assurance are also described that were not mentioned in previous literature. Rat or mouse plasma (50 microl) is acidified (or treated enzymatically for TCE-Glu determination) and extracted with peroxide free methyl t-butyl ether. Distilled diazomethane (CH(2)N(2)) is added to derivatize TCA to its methyl ester. Detection limits were estimated at 0.2 microg/ml for CH and TCE, and 0.1 microg/ml for TCA. Detector response to TCA and TCE were shown to be linear in the range of 3.125-200 microg/ml (r> or =0.9996). For CH, the response fits a second-order equation in this same range (r=0.99994)
描述了一种灵敏、准确且可靠的方法，用于定量测定小鼠和大鼠血浆中三氯乙醛（CH）及其代谢产物。CH的代谢产物包括三氯乙酸（TCA）、三氯乙醇（TCE）和三氯乙醇葡糖苷酸（TCE-Glu）。这种新方法采用带有电子捕获检测的毛细管气相色谱法（GC/ECD）。还描述了提高样品稳定性和质量保证的程序，这些程序在以前的文献中未提及。将大鼠或小鼠血浆（50微升）酸化（或为测定TCE-Glu进行酶处理），并用无过氧化物的甲基叔丁基醚萃取。加入蒸馏的重氮甲烷（CH₂N₂）将TCA衍生化为其甲酯。CH和TCE的检测限估计为0.2微克/毫升，TCA的检测限为0.1微克/毫升。检测器对TCA和TCE的响应在3.125 - 200微克/毫升范围内呈线性（r≥0.9996）。对于CH，在相同范围内响应符合二阶方程（r = 0.99994）
