液相色谱串联质谱法定量检测血清中8种有机磷农药

目的建立了液相色谱串联质谱(LC-MS-MS)法测定血清中8种有机磷农药含量的方法。方法血清样品经乙酸乙酯液液萃取,以pH3.5的乙酸铵缓冲溶液,甲醇和水为流动相混合梯度洗脱,滤液经C185μm(2.1 mm#150mm柱)分离,经在线电喷雾离子源(ESI)正离子化后,采用多反应离子监测方式(MRM)选择离子对测定。结果目标化合物的线性范围为0～1000ng/ml,8种化合物相关系数均大于0.990,加标回收率为95%～129%,RSD<7.9%;日内日间相对标准偏差小于12%(n=6)。结论 LC-MS-MS方法高效、准确,特异性强,样品处理简单,可准确定量血清中有机磷农药。

Method establishment for the determination of 8 organophosphorus pesticides in serum using LC/MS/MS

Objective To establish the method to determine the presence and concentration of 8 organophosphors pesticides in serum by LC/MS/MS.Method The serum samples were extracted by ethyl acetateether and then separated on C18 5μm(2.1mm150mm)column with pH=3.5 acid-ammonium acetate buffer solution,methanol–water as mobile phase to mixed gradient elution.Electro-spray ionization source(ESI) was applied and operated in positive ion mode,and multiple reaction monitoring(MRM) mode was adopted.Result Within concentration ranging from 0-1000ng/ml the correlation coefficient for each compound was greater than 0.990,recoveries were between 95%-129%,RSD<7.9%.The RSD of intra-day and inter-day were less 12%(n=6).Conclusion The procedure of preparing serum samples is sample and the result of this method is efficient,accurate and specific.