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目的建立人血液中毒死蜱的超高效液相色谱-串联质谱(UPLC-MS/MS)法,并验证其在中毒案例中的应用。方法样品通过乙腈沉淀蛋白法提取,经C apcell Pack C18MGII柱(250 mm×2.0 mm,5μm)分离,利用溶剂A(含2mmol/L乙酸铵及0.1%的甲酸水溶液)、溶剂B(含2mmol/L乙酸铵的甲醇)以体积比5∶95等度洗脱。结果线性范围为5~500 ng/m L(r=0.998 7)。检出限及最低定量限分别为2 ng/m L及4 ng/m L。日内及日间精密度均小于10%,准确度为97.44%~101.10%。长期冷冻稳定性试验数据良好。基质效应、提取回收率及提取效率分别为64.97%~86.81%、76.70%~85.52%及55.57%~66.58%。结论该方法可用于法医毒物分析及临床治疗中毒死蜱的快速提取及其定量分析。
Objective To establish a method for the determination of chlorpyrifos in human blood by UPLC-MS / MS and verify its application in the case of poisoning. Methods Samples were extracted by acetonitrile precipitation and separated on a C apcell Pack C18 MGII column (250 mm × 2.0 mm, 5 μm) using solvent A (containing 2 mmol / L ammonium acetate and 0.1% formic acid in water), solvent B L ammonium acetate in methanol) was eluted with a volume ratio of 5:95 isocratic. The linear range of results was 5 ~ 500 ng / m L (r = 0.998 7). The detection limit and the minimum limit of quantification were 2 ng / m L and 4 ng / m L, respectively. The intra-day and inter-day precision were less than 10%, the accuracy of 97.44% ~ 101.10%. Long-term freezing stability test data is good. The matrix effect, extraction recovery rate and extraction efficiency were 64.97% -86.81%, 76.70% -85.52% and 55.57% -66.58%, respectively. Conclusion The method can be used for the rapid extraction and quantitative analysis of chlorpyrifos in forensic toxicology analysis and clinical treatment.