Rapid simultaneous determination for organophosphorus pesticides in human serum by LC-MS

被引:74
作者
Inoue, Shigeaki [1 ]
Saito, Takeshi
Mase, Hiroyasu
Suzuki, Yosuke
Takazawa, Kensuke
Yamamoto, Isotoshi
Inokuchi, Sadaki
机构
[1] Tokai Univ, Sch Med, Dept Emergency & Crit Care Med, Kanagawa 2591193, Japan
[2] Tokai Univ, Sch Med, Dept Lab Med, Kanagawa 2591193, Japan
关键词
organophosphorus pesticide; LC-APCI-MS; simultaneous determination; human serum; validation; application;
D O I
10.1016/j.jpba.2007.01.036
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A simple and rapid method was developed for measuring 10 organophosphorus pesticides (acephate, methidathion, dichlorvos, fenthion, EPN, diazinon, phenthoate, malathion, fenitrothion, and cyanophos) in the serum of acute poisoning patients by LC/MS. Following deproteinization by acetonitrile, an aliquot of the biological sample was injected into a C-18 column using 10mM ammonium formate-methanol as the mobile phase. Extraction recoveries were satisfactory and ranged between 60.0 and 108.1% in serum. The limits of detection (LODs) in serum ranged from 0.125 to mu g/ml, and the limits of quantitation (LOQs) ranged from 0.25 to 1.25 mu g/ml. An excellent linearity was observed for these LOQs up to 8 mu g/ml. Intra- and interassay precision and accuracy were satisfactory for most of the pesticides analyzed. In terms of temperature stability, of all the organophosphorus compounds analyzed, dichlorvos and malathion exhibited the most rapid degradations over 24 h at room temperature. Methidathion and diazinon remained relatively stable at all temperatures during the entire 4-week testing period. The present method was successfully applied to one actual case of acute poisoning. In conclusion, this method is simple, accurate, and useful for the determination of organophosphorus pesticides and should benefit both clinical and forensic toxicology. (c) 2007 Elsevier B.V. All rights reserved.
引用
收藏
页码:258 / 264
页数:7
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