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
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摘要: 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1.0 mmol·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0.01~0.50 mg·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.Abstract: The UPLC-MS/MS combined with gel permeation chromatography purification (GPC) was proposed to simultaneously measure 9 pesticides 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 and 1.0 mmol·L-1 ammonium acetate solution as mobile phase,and then detected by multiple reactions monitoring (MRM). Linearity range of the 9 pesticides was found between 0.01-0.50 mg·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%.