凝胶渗透色谱净化高效液相色谱-串联质谱法检测辛辣蔬菜中咪鲜胺等7种农药残留

LC-MS/MS Determination of 7 Residual Pesticides in Spicy Flavor Vegetables with Purification by Gel Permeation Chromatography(GPC) Purification

建立了辛辣蔬菜基质中咪鲜胺、异菌脲、虫酰肼、噻螨酮、涕灭威、涕灭威亚砜和涕灭威砜7种农药残留量的凝胶渗透色谱-分散固相萃取技术相结合净化高效液相色谱串联质谱检测法。样品经乙腈提取,氮气吹干,环己烷-乙酸乙酯(1+1)溶液溶解后,凝胶渗透色谱与分散固相萃取法相结合进行净化,反相高效液相色谱柱分离后,采用液相色谱-串联质谱法在分时段多反应监测模式下进行测定,外标法定量。结果表明:7种农药在0.005-2.0μg/mL范围内线性关系均良好(r2在0.995-0.999),且所有农药检出限和定量限均低于国际限量要求;在定量限、5倍和10倍定量限的添加水平下,辛辣蔬菜中7种农药的平均回收率介于60%-120%,相对标准偏差不大于5.0%。该方法定性、定量准确,干扰小,能用于辛辣蔬菜基质中7种农药残留的检测,能很好的满足我国进出口辛辣蔬菜中这7种农药限量的严格要求。

A screening method was developed for the determination of Prochloraz, iprodione, Tebufenozide, Hexythiazox, Aldicard, Aldicard-sulfone and Aldicard-sulfoxide, seven pesticide residues in spicy flavor vegetables with purification by Gel Permeation Chromatography （GPC） and dispersive solid-phase extraction （DSPE）, then detection of liquid chromatography-tandem mass spectrometry （LC-MS/MS）. Samples were first extracted with acetonitrile, then dried by nitrogen. The remaining residues were dissolved with 8mL ethyl acetate-cyclohexane mixture （v：v=50：50） and followed with a GPC cleanup. Identification of seven pesticides was performed by LC-MS/MS with an external standard method. The results indicated the linearity of the method was good between 0.005μg/mL and 2.0μg/mL, and all limits of quantitation （LOQ） of this method can meet the international standard. Meanwhile, the recoveries of seven pesticides were in the range from 60%to 120%at the spiked level of LOQ, 5 in Spicy Flavor Vegetables samples, along with the small relative standard deviations （RSDS were all less than 5.0%）, which highly proved that the method was reliable and stable. The method is simple, rapid, accurate and of less interference, which is well suitable to the pesticide residues limit requirements of Spicy Flavor Vegetables exportation policy.