QuEChERS法结合气相色谱-质谱法同时测定葡萄酒中16种农药残留

Determination of 16 Pesticide Residues in Wine by GC-MS Combined with QuEChERS

摘要: 采用气相色谱-质谱法(GC-MS)测定葡萄酒中有机磷类及有机氯类等16种农药残留。样品经酸化乙腈提取后,提取液采用QuEChERS前处理法,经N-丙基乙二胺-石墨化碳黑-C18粉末净化。净化液采用Agilent HP-5MS色谱柱分离,质谱中采用电子轰击离子源-选择离子监测模式。16种农药的线性范围为0.05~2.00 mg·L-1,方法的检出限(3S/N)在0.006~0.060 mg·kg-1之间。对空白样品进行加标回收试验,回收率在87.6%~105%之间,测定值的相对标准偏差(n=6)在0.77%~6.9%之间。方法可以用于葡萄酒中农药残留的进出口检测。

Abstract: A method of GC-MS coupled with QuEChERS was applied for simultaneous determination of 16 kinds of pesticide residues in wine. The sample was extracted with acidified acetonitrile. The extract was purified by QuEChERS method, using the mixture of N-propylethylenediamine, graphitized carbon black and C18 powder, and then separated on an Agilent HP-5MS column and detected by MS adopting EI-SIM. The linearity range of the mass concentration of 16 kinds of pesticides was 0.05-2.00 mg·L-1 with detection limits in the range of 0.006-0.060 mg·kg-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 87.6%-105%, and RSD (n=6) in the range of 0.77%-6.9%. The method was used for analysis of pesticide residues in wine samples for import and export inspection.