DSPE-GC/MS快速检测葡萄酒中52种农药残留

Fast Determination of 52 Pesticide Residues in Grape Wine by DSPE-GC /MS

利用分散固相萃取GC—MS分析，建立了葡萄酒中52种不同极性农药残留的快速检测方法．葡萄酒样品用酸化乙腈经振荡提取和超声辅助提取后，上清液用混合吸附填料进行分散固相萃取净化，高速离心后，再通过氮吹方式浓缩，复溶，过滤膜，用GC／MS检测．与传统前处理方法相比，分散固相萃取技术在检测成本和处理速度上有很大优势．52种农药在3个浓度添加水平上的加标回收率范围是60％～110％，RSD〈15％（n=5），定量限是0．0007～0．0323133g／kg．

A fast method was developed for determination of 52 pesticides in grape wine by using DSPE and GC-MS. The samples were first extracted using acetonitrile with the addition of vibration and ultra sound. Then mix adsorbents were used in dispersive solid phase extraction to purify the extracts. After the high speed centrifugation, nitrogen flushing concentration, and filtration, the samples were detected by GC/MS using selective ion monitoring （SIM）. Compared with traditional methods, QuEChERS had advantages in cost and pretreatment speed. The spiked recoveries at three levels of 52 pesticides were in range of 60% -110% while the relative standard deviations （n = 5） were all less 15%. Meanwhile, the limit of quantity （LOQ） were in the range of 0. 000 7 -0. 032 3 mg/kg. With features such as accuracy and easy operation, this method could be used to fast determination of 52 pesticides in grape wine without any special apparatus and also satisfied the requirement of the pesticide routine analysis.