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采用固相萃取结合二极管阵列检测的高效液相色谱法和气相色谱 - 质谱联用仪分析死后样本中的倍硫磷。

Analysis of fenthion in postmortem samples by HPLC with diode-array detection and GC-MS using solid-phase extraction.

作者信息

Meyer E, Borrey D, Lambert W, Van Peteghem C, Piette M, De Leenheer A

机构信息

Laboratorium voor Toxicologie, Universiteit Gent, Belgium.

出版信息

J Anal Toxicol. 1998 May-Jun;22(3):248-52. doi: 10.1093/jat/22.3.248.

Abstract

Fenthion (O,O-dimethyl-O-[3-methyl-4-(methylthio)-phenyl]-thiophos-phate ) is an organophosphate insecticide. A specific method to quantitate fenthion in postmortem matrices with solid-phase extraction combined with high-performance liquid chromatography-diode-array detection (HPLC-DAD) and gas chromatography-mass spectrometry (GC-MS) is presented. Fenitrothion (O,O-dimethyl-O-[3-methyl-4-nitrophenyl]-thiophosphate) is selected as the internal standard. For sample cleanup, a simple but selective solid-phase extraction is chosen after comparison with traditional liquid-liquid extraction procedures. Homogenized and appropriately diluted aqueous samples are applied, and the analytes are desorbed with 5 mL of dichloromethane. Aliquots of the extract are used for HPLC-DAD and GC-MS analysis, Liquid and GC conditions are as follows: gradient elution with a mixture of methanol and water (10:90 to 90:10, v/v) containing 0.0125M NaOH on an Aluspher RP-Select B column monitoring at 250 nm, and temperature programming from 60 to 300 degrees C on a dimethylpolysiloxane column in the SCAN mode, respectively. This method is applied to a suicidal case involving unsuspected acute intoxication with fenthion (concentration in blood, 3.8 micrograms/mL).

摘要

倍硫磷(O,O-二甲基-O-[3-甲基-4-(甲硫基)-苯基]-硫代磷酸酯)是一种有机磷杀虫剂。本文介绍了一种结合固相萃取、高效液相色谱-二极管阵列检测(HPLC-DAD)和气相色谱-质谱联用(GC-MS)定量死后基质中倍硫磷的特定方法。选用杀螟硫磷(O,O-二甲基-O-[3-甲基-4-硝基苯基]-硫代磷酸酯)作为内标。为了净化样品,在与传统液-液萃取方法比较后,选择了一种简单但具有选择性的固相萃取方法。将匀浆并适当稀释的水样进行处理,用5 mL二氯甲烷解吸分析物。取萃取液的等分试样用于HPLC-DAD和GC-MS分析,液相和气相条件如下:在Aluspher RP-Select B柱上,用含0.0125M NaOH的甲醇和水(10:90至90:10,v/v)混合物进行梯度洗脱,在250 nm波长处监测;在二甲基聚硅氧烷柱上,以扫描模式从60℃至300℃进行程序升温。该方法应用于一例涉及意外急性倍硫磷中毒(血液中浓度为3.8微克/毫升)的自杀案件。

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