Analysis of endosulfan and its metabolites in rat plasma and selected tissue samples by gas chromatography-mass spectrometry

Analysis of endosulfan and its metabolites in rat plasma and selected tissue samples by gas chromatography-mass spectrometry
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DOI:
10.1002/tox.20076
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发表时间:
2005-02-01
影响因子:
4.5
通讯作者:
Mohd, MA
Mohd, MA
中科院分区:
医学3区
文献类型:
--
作者:
Chan, MPL;Mohd, MA

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已经开发了一种方法,用于测定大鼠血浆和组织样本中的甲型硫丹、乙型硫丹、硫丹硫酸盐和硫丹二醇的痕量水平。血浆样品中的硫丹及其代谢物用固相萃取Chromabond-end-capped C18柱提取,并在Shimadzu QP-5050 A气相色谱-质谱联用仪(GCMS)上以选择离子监测模式进行分析。对肝脏和肾脏样本中硫丹及其代谢物的分析涉及溶剂萃取、弗罗里硅土固相萃取净化和气相色谱-质谱联用仪定量。分别在10-100 ng mL(-1)和100-1000 ng mL(-1)浓度范围内对血浆和组织样品进行回收率实验。该方法被用于分析从动物研究中采集的血浆和组织样本中的痕量硫丹及其代谢物。在肾脏样本中检测到的α-硫丹和β-硫丹的微量含量分别为3.11微克(-1)和1.19微克(-1),而在大鼠肝脏样本中检测到的硫丹硫酸盐的微量含量为0.02-0.22微克(-1)。在所有血浆样本中均未检测到硫丹及其代谢物。(C)2005 Wiley Periodicals,Inc.
A method has been developed for the determination of trace levels of alpha-endosulfan, beta-endosulfan, endosulfan sulfate, and endosulfan diol in rat plasma and tissue samples. Endosulfan and its metabolites in the plasma samples were extracted with solid-phase extraction Chromabond-end-capped C18 cartridges and analyzed by a Shimadzu QP-5050A gas chromatograph-mass spectrometer (GCMS) with quadrupole detector in selected-ion-monitoring mode. The analysis of endosulfan and its metabolites in liver and kidney samples involved solvent extraction, Florisil solid-phase-extraction cleanup, and quantitation by GCMS. Recovery experiments for the plasma and tissue samples were conducted over concentration ranges of 10-100 ng mL(-1) and 100-1000 ng mL(-1), respectively. The method was applied to the analysis of trace levels of endosulfan and its metabolites in plasma and tissue samples collected from an animal study. Trace levels of alpha-endosulfan and beta-endosulfan in the ranges of undetectable to 3.11 mug g(-1) and undetectable to 1.19 mug g(-1), respectively, were detected in the kidney samples, whereas trace levels of endosulfan sulfate in the range of 0.02-0.22 mug g(-1) were detected in the liver samples of rats. Neither endosulfan nor its metabolites was detected in any of the plasma samples. (C) 2005 Wiley Periodicals, Inc.