凝胶色谱净化-超高效液相色谱-串联质谱法测定豇豆中9种农药残留

Determination of 9 Pesticides Residues in Cowpeas by GPC-UPLC-MS/MS

提出了同时检测豇豆中9种农药残留的凝胶色谱净化-超高效液相色谱-串联质谱法。豇豆样品用乙腈提取,经凝胶色谱(GPC)净化后,以甲醇和1.0mmol·L-1乙酸铵溶液作为流动相,经Waters BEH C18色谱柱分离后进行多离子反应监测(MRM)模式分析检测。9种农药的线性范围在0.01~0.50mg·L-1之间,相关系数均大于0.99。对豇豆样品进行加标试验,9种农药的回收率在72.2%~109%之间,相对标准偏差(n=5)在0.6%~8.9%之间。

The UPLC-MS/MS combined with gel permeation chromatography purification(GPC)was proposed to simultaneously measure 9pesticides residues in cowpeas.The sample was extracted by acetonitrile,and purified by GPC.The eluate was separated by using Waters BEH C18 column as stationary phase,methanol and1.0mmol·L-1 ammonium acetate solution as mobile phase,and then detected by multiple reactions monitoring(MRM).Linearity range of the 9pesticides was found between 0.01-0.50mg·L-1 with correlation coefficients above 0.99.Tests for recovery were made by standard addition,giving recovery rates in the range of 72.2%-109% and RSD′s(n=5)in the range of 0.6%-8.9%.