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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。
Objective To establish a method for the determination of 18 organophosphorus and carbamate pesticides in human blood by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The blood samples were separated by acetonitrile precipitation. The mobile phase was Waters BEH C18 (1.7μm 2.1 × 50mm) with a mobile phase of 5mmol / L ammonium acetate in water and methanol at a flow rate of 0.3m L / min. The injection volume was 2μL. Electrospray ionization Source (ESI), positive ion detection, quantitative analysis using multiple reaction monitoring methods. Results The limit of detection (LOD) was between 0.1 ~ 40ng / m L and the limit of quantitation (LOQ) was between 0.5 ~ 50ng / m L. The linearity of each drug concentration ranged from the limit of quantification to 500ng / Rates ranged from 64.3% to 111.9% with relative standard deviations of 3.9% -10.3%. Conclusion The method is specific, sensitive and accurate and can be applied to forensic and clinical analysis of poisons.