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液相色谱-质谱联用法测定人全血中灭多威
引用本文:张美玲,张振南,温从丛,王志翊,林丹,王贤亲.液相色谱-质谱联用法测定人全血中灭多威[J].中国法医学杂志,2016(4):367-368,372.
作者姓名:张美玲  张振南  温从丛  王志翊  林丹  王贤亲
作者单位:1. 温州医科大学司法鉴定中心法医毒物实验室,浙江 温州,325035;2. 温州医科大学附属第二医院急诊科,浙江温州,325027
摘    要:目的建立一种简便的测定人全血中灭多威的液相色谱-质谱联用法。方法样品处理采用液-液乙酸乙酯萃取方法。色谱柱为Zorbax SB-C18(2.1mm×50mm,5μm),流动相为乙腈-0.1%甲酸,梯度洗脱,流速为0.5mL/min,柱温40℃。采用ESI离子源,MRM离子方式监测。结果灭多威在0.05~2.0μg/mL浓度范围内线性良好(r0.995)。灭多威的方法回收率均在90%~108%的范围内,日内、日间RSD均小于15%。结论本方法可简单、高效地检测全血中灭多威浓度。

关 键 词:法医毒物分析  液-质联用法  灭多威  全血

Determination of methomyl in human blood by LC/MS
Zhang Meiling;Zhang Zhennan;Wen Congcong;Wang Zhiyi;Lin Dan;Wang Xianqin.Determination of methomyl in human blood by LC/MS[J].Chinese Journal of Forensic Medicine,2016(4):367-368,372.
Authors:Zhang Meiling;Zhang Zhennan;Wen Congcong;Wang Zhiyi;Lin Dan;Wang Xianqin
Institution:Zhang Meiling;Zhang Zhennan;Wen Congcong;Wang Zhiyi;Lin Dan;Wang Xianqin;Forensic Toxicology Laboratory,Wenzhou Medical University Forensic Center;Department of Emergency,the Second Affi liated Hospital of Wenzhou Medical University;
Abstract:Objective To develop a sensitive and simple LC/MS method for determination of methomyl in blood samples.Methods Methomyl was extracted from blood by liquid-liquid extraction with ethyl acetate, and then analyzed on a Zorbax SB-C18 (2.1mm×50mm, 5μm) column. The mobile phase consisted of acetonitrile-0.1% formic acid with gradient elution, at a lfow rate of 0.5 mL/min, at 40℃. LC-MS was performed in ESI source with MRM mode for quantiifcation.ResultsThe linear range of the concentration were 0.05~2.0μg/mL for methomyl (r>0.995). The relative recoveries of methomyl were in the range of 90%~108%. The RSDs of intra-days and inter-day were both less than 15%.Conclusion The method is a simple, quick, sensitive and could be used for determination of methomyl in blood samples.
Keywords:forensic toxicological analysis  LC/MS  methomyl  blood
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