液相色谱-质谱联用法测定人全血中灭多威

摘要

Objective To develop a sensitive and simple LC/MS method for determination of methomyl in blood samples.Methods Methomyl was extracted from blood by liquid-liquid extraction with ethyl acetate, and then analyzed on a Zorbax SB-C18 (2.1mm×50mm, 5µm) column. The mobile phase consisted of acetonitrile-0.1% formic acid with gradient elution, at a lfow rate of 0.5 mL/min, at 40℃. LC-MS was performed in ESI source with MRM mode for quantiifcation.ResultsThe linear range of the concentration were 0.05~2.0μg/mL for methomyl (r>0.995). The relative recoveries of methomyl were in the range of 90%~108%. The RSDs of intra-days and inter-day were both less than 15%.Conclusion The method is a simple, quick, sensitive and could be used for determination of methomyl in blood samples.%目的：建立一种简便的测定人全血中灭多威的液相色谱-质谱联用法。方法样品处理采用液-液乙酸乙酯萃取方法。色谱柱为Zorbax SB-C18(2.1mm×50mm，5μm)，流动相为乙腈-0.1%甲酸，梯度洗脱，流速为0.5mL/min，柱温40℃。采用ESI离子源，MRM离子方式监测。结果灭多威在0.05~2.0μg/mL浓度范围内线性良好(r>0.995)。灭多威的方法回收率均在90%~108%的范围内，日内、日间RSD均小于15%。结论本方法可简单、高效地检测全血中灭多威浓度。