UPLC-MS/MS检测人血中18种有机磷及氨基甲酸酯类农药

目的建立人血中18种有机磷及氨基甲酸酯类农药超高压液相色谱-串联质谱(UPLC-MS/MS)的检测方法。方法血液中加入乙腈沉淀蛋白,采用Waters BEH C18(1.7μm 2.1×50mm)柱子,流动相为5mmol/L乙酸铵水-甲醇,流速:0.3m L/min;进样量:2μL,电喷雾离子源(ESI),正离子检测,采用多反应监测方式进行定量分析。结果药物最小检测限(LOD)在0.1~40ng/m L之间,定量限(LOQ)在0.5~50ng/m L之间,各药物浓度在定量限到500ng/m L范围内线性良好,回收率均在64.3%~111.9%之间,相对标准偏差为3.9%~10.3%。结论该方法专属性强、灵敏、准确,可以适用于法庭与临床毒物分析。

Simultaneous determination of 18 organophosphorous and carbamate pesticides in human plasma by UPLC-MS/ MS

Objective To develop a method for determination of 18 organophosphorous and carbamate pesticides in human plasma by UPLC-MS/MS. Methods Following deproteinization by acetonitrile, an aliquot of the biological sample was injected into a C18 column(1.7μm 2.1×50mm) using 5mmol/L Ammonium acetate-methanol as the mobile phase with the flow rate of 0.3mL/min, the injection volume was 10μL. Electro spray ionization(ESI) Indicators source was applied and operated in positive ion mode, and multiple reaction monitoring(MRM) mode was used to quantify. Results The limits of detection(LODs) in human plasma ranged from 0.1 to 40ng/mL, and the limits of quantitation(LOQs) ranged from 0.5 to 50ng/mL. An excellent linearity was observed for these LOQs up to 50ng/mL. The average extraction recoveries were with in 64.3%~111.9%, relative standard deviation(RSD) is 3.9%~10.3%. Conclusion This method is specific, sensitive and accurate, and can be used to detect pesticides in forensic.