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Determination of chlorpyrifos and its metabolites in cells and culture media by liquid chromatography-electrospray ionization tandem mass spectrometry
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-08-18 , DOI: 10.1016/j.jchromb.2017.08.010
Xiangkun Yang , Xian Wu , Kyle A. Brown , Thao Le , Steven L. Stice , Michael G. Bartlett

A sensitive method to simultaneously quantitate chlorpyrifos, chlorpyrifos oxon and the detoxified product 3,5,6-trichloro-2-pyridinol (TCP) was developed using either liquid–liquid extraction for culture media samples, or protein precipitation for cell samples. Multiple reaction monitoring in positive ion mode was applied for the detection of chlorpyrifos and chlorpyrifos oxon, and selected ion recording in negative mode was applied to detect TCP. The method provided linear ranges from 5 to 500, 0.2–20 and 20–2000 ng/mL for media samples and from 0.5–50, 0.02–2 and 2–200 ng/million cells for CPF, CPO and TCP, respectively. The method was validated using selectivity, linearity, precision, accuracy, recovery, stability and dilution tests. All relative standard deviations (RSDs) and relative errors (REs) for QC samples were within 15% (except for LLOQ, within 20%). This method has been successfully applied to study the neurotoxicity and metabolism of chlorpyrifos in a human neuronal model.



中文翻译:

液相色谱-电喷雾串联质谱法测定细胞和培养基中毒死rif及其代谢产物

开发了一种同时定量毒死rif,毒死ox和解毒产物3,5,6-三氯-2-吡啶醇(TCP)的灵敏方法,方法是使用液-液萃取法分离培养基样品,或使用蛋白质沉淀法分离细胞样品。采用正离子模式的多反应监测来检测毒死and和毒死rif中的氧,并以负离子模式选择的离子记录来检测TCP。该方法对培养基样品提供的线性范围为5至500、0.2–20 ng / mL和20–2000 ng / mL,对于CPF,CPO和TCP的线性范围分别为0.5–50、0.02–2和2–200 ng / mL。该方法已使用选择性,线性,精密度,准确性,回收率,稳定性和稀释度测试进行了验证。质控样品的所有相对标准偏差(RSD)和相对误差(RE)均在15%以内(LLOQ除外,均在20%以内)。该方法已成功地用于研究毒死rif在人神经元模型中的神经毒性和代谢。

更新日期:2017-08-18
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