固相分散萃取-气相色谱-质谱联用法测定葡萄酒中43种农药残留量

摘要

目的：建立固相分散萃取结合气相色谱-质谱联用法(GC/MS)快速测定葡萄酒中敌敌畏、乐果、二嗪磷等葡萄种植过程中常用43种杀虫剂、杀螨剂及杀菌剂残留量。方法样品用乙腈快速提取、氯化钠和无水硫酸镁盐析后，经 GCB粉、NH2粉和 PSA粉组合吸附剂净化， GC/MS外标法定性定量。结果43种农药在10~500μg/L范围内线性关系良好，相关系数R2在0.9851~0.9997范围内，空白添加浓度在50~200μg/kg时，其回收率在67.43%~114.74%之间，相对标准差(n=6)小于13.6%，方法的测定下限(LOD)介于1~50μg/kg 之间。结论本法简单、准确、快速，适合于葡萄酒中对43种农药残留量的检测。%Objective A rapid analytical method was developed for the determination of 43 pesticide residues in grape wine by solid-phase dispersion with gas chromatography-mass spectrometry (GC/MS). Methods Toally 43 pesticide residues were extracted from the samples with acetonitrile, and then detected by GC/MS with external standard method after being cleaned up with three sorbents (PSA 80.0 mg、GCB 30.0 mg and NH2 30.0 mg). Results Good linearities of 10500μg/L were obtained and correlation coefficients were 0.98510.9997. The recoveries of all pesticides were in the range from 67.43%to 114.74%at the spiked levels of 50, 100, and 200μg/kg in grape wine, and the relative standard deviations (RSDs) were not more than 13.6%. The limits of detection (LOD) were 1~50μg/kg. Conclusion The method could be used for the determination of 43 pesticide residues in grape wine due to its simpleness, accuracy and rapidness.