Rapid simultaneous determination for organophosphorus pesticides in human serum by LC–MS
- 作者：Shigeaki Inoue ; Takeshi Saito ; Hiroyasu Mase ; Yosuke Suzuki ; Kensuke Takazawa ; Isotoshi Yamamoto ; Sadaki Inokuchi
- 关键词：Organophosphorus pesticide ; LC-APCI-MS ; Simultaneous determination ; Human serum ; Validation ; Application
- 刊名：Journal of Pharmaceutical and Biomedical Analysis
- 出版年：2007
- 期刊代码：65_07317085
- 类别：ch
- 出版时间：9 May 2007
- 卷：44
- 期：1
- 页码：258-264
- 文件大小：702 K
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 C18 column using 10 mM 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 1 μg/ml, and the limits of quantitation (LOQs) ranged from 0.25 to 1.25 μg/ml. An excellent linearity was observed for these LOQs up to 8 μg/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.