快速测定豇豆中农药残留量的方法研究

摘要

建立豇豆中克百威、三羟基克百威、残杀威、灭多威、抗蚜威、仲丁威、甲萘威、异丙威、速灭威9种农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。样品通过乙腈匀浆提取，在电喷电离方式(ESI+)、多反应监测模式(MRM)下进行测定，基质配标准曲线定量。分析物在0.01～0.50 mg/L范围内呈线性，相关系数r＞0.99，空白样品中分析物在0.01 mg/kg、0.02 mg/kg、0.10 mg/kg 3个不同添加水平时，平均回收率在89.0%～110.0%之间；相对标准偏差为0.7%～9.1%，定量限为0.005～0.01 mg/kg，满足定量分析的要求。%An ultra performance liquid chromatography tandem mass spectrometric method was established for the simultaneous determining the residues of 9 pesticides in Cowpea. The samples were processed by ultrasonic extraction with acetonitrile. The analysis was detected by UPLC-MS/MS under positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The matrixmatched external standard calibration curves were used for the quantitative analysis. Under the optimum conditions, the method showed a good linearity in the range of 0.005~0.50 mg/L with correlation coefficient over 0.99. The limits of quantitation (LOQ) for the pesticide residue were 0.005~0.01 mg/kg. The average recoveries of pesticides residues were 89.0%~110.0% at the spiked levels of 0.01, 0.02 mg/kg and 0.10 mg/kg with relative standard deviation (RSDs) of 0.7%~9.1%. The method is sensitive and accurate and is suitable for the simultaneous quantitative determination of 9 pesticides in Cowpea.