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目的采用固相萃取-气相色谱/质谱分析方法检测血液、尿液和脏器组织中的百草枯。方法人血液、尿液和猪肺组织样品经三氯乙酸去除蛋白后,取上清用十二烷基三甲基溴化铵和十二烷基硫酸钠处理过的C18小柱提取,提取物用硼氢化钠在碱性条件下还原,产物用气相色谱/质谱法分析,外标法定量。结果生物检材中百草枯回收率为78%～87%,最低检出限为0.1μg/mL,在0.5～1mg/mL范围内线性关系良好,可对实际案例检材进行定量检测。结论本文固相萃取-气相色谱/质谱分析方法能满足中毒生物检材检验及临床毒物检验需要。
Objective To detect paraquat in blood, urine and visceral tissues by solid-phase extraction-gas chromatography / mass spectrometry. Methods Human blood, urine and lung tissue samples were removed by trichloroacetic acid protein, the supernatant with dodecyl trimethyl ammonium bromide and sodium dodecyl sulfate treated C18 column extract, extract Reduction with sodium borohydride in alkaline conditions, analysis of the product by gas chromatography / mass spectrometry, external standard. Results The recovery rate of paraquat in biological samples was 78% ~ 87%, the lowest detection limit was 0.1μg / mL, and the linearity was good in 0.5 ~ 1mg / mL range. Conclusion The SPE-GC / MS method can meet the needs of poisoning biopsy and clinical toxicology testing.