Lacassie E, Marquet P, Gaulier J M, Dreyfuss M F, Lachâtre G
Department of Pharmacology and Toxicology, University Hospital, 2 Av. Martin Luther King, 87042 Limoges, France.
Forensic Sci Int. 2001 Sep 15;121(1-2):116-25. doi: 10.1016/s0379-0738(01)00461-3.
Original and sensitive multiresidue methods are presented for the detection and quantitation, in human biological matrices, of 61 pesticides of toxicological significance in human. These methods involved rapid solid-phase extraction using new polymeric support (HLB and MCX) OASIS cartridges. Gas chromatography-mass spectrometry (GC-MS) was used for volatile (organophosphate, organochlorine, phtalimide, uracil) pesticides and liquid chromatography-ionspray-mass spectrometry (LC-MS) for thermolabile and polar pesticides (carbamates, benzimidazoles). Acquisition was performed in the selected ion monitoring (SIM) mode. Extraction recovery varied owing to the nature of pesticides, but was satisfactory for all. Limits of detection (LODs) and limits of quantitation (LOQs) ranged, respectively, from 2.5 to 20 and from 5 to 50ng/ml. An excellent linearity was observed from LOQs up to 1000ng/ml for all the pesticides studied. The proposed procedures yielded reproducible results with good inter-assay accuracy and precision. A few cases of intoxication are presented to demonstrate the diagnostic interest of these methods: in two cases were determined lethal concentrations of endosulfan and carbofuran; in four other cases, the procedures helped diagnose intoxication with, respectively, parathion-ethyl, the association of bromacil and strychnine, bifenthrin and aldicarb.
本文介绍了用于检测和定量人体生物基质中61种对人体具有毒理学意义的农药的原始且灵敏的多残留方法。这些方法包括使用新型聚合物载体(HLB和MCX)OASIS小柱进行快速固相萃取。气相色谱 - 质谱联用(GC-MS)用于检测挥发性农药(有机磷、有机氯、邻苯二甲酰亚胺、尿嘧啶),液相色谱 - 离子喷雾 - 质谱联用(LC-MS)用于检测热不稳定和极性农药(氨基甲酸酯类、苯并咪唑类)。采用选择离子监测(SIM)模式进行数据采集。由于农药性质的不同,萃取回收率有所差异,但对所有农药而言均令人满意。检测限(LOD)和定量限(LOQ)分别为2.5至20 ng/ml和5至50 ng/ml。在所研究的所有农药中,从定量限到1000 ng/ml均观察到良好的线性关系。所提出的方法具有可重复的结果,批间准确性和精密度良好。文中列举了一些中毒案例以证明这些方法的诊断价值:在两例中测定了硫丹和克百威的致死浓度;在另外四例中,该方法分别有助于诊断对硫磷 - 乙基、溴敌隆与士的宁混合物、联苯菊酯和涕灭威的中毒情况。