固相微萃取-气相色谱-串联质谱法快速筛查葡萄酒中农药残留  

Rapid screening of pesticides residues in wine by solid phase microextraction-gas chromatography-tandem mass spectrometry

作　　者：崔宗岩[1] 王晶[1,2] 曹彦忠[1] 葛娜[1] 刘永明[1] 李阿丹[2] 张进杰[1] 

机构地区：[1]秦皇岛出入境检验检疫局检验检疫技术中心,秦皇岛066004 [2]燕山大学环境与化学工程学院,秦皇岛066004

出　　处：《食品安全质量检测学报》2017年第7期2705-2717,共13页Journal of Food Safety and Quality

基　　金：国家质检总局科技计划项目(2014IK091;2015IK094);质检公益性行业科研专项(201210092)~~

摘　　要：目的建立固相微萃取-气相色谱-串联质谱法快速筛查检测葡萄酒中农药残留。方法葡萄酒样品稀释后进行固相微萃取,直接进行气相色谱-串联质谱检测。优化选择了萃取纤维类型、萃取方式、萃取时间等固相微萃取的实验条件,考察了方法性能(检出限、添加回收率和精密度等)。结果确定方法可检测目标农药为94种,其检出限<10μg/L,平均回收率在60%~110%之间,且方法的重复性和再现性标准偏差分别在20%和30%之内。结论该检测方法操作简便、快速,单个样品分析时间不超过1 h,适用于葡萄酒中农药残留的快速筛查检测。Objective To eatablish a rapid method for simultaneous screening of pesticides in wine by solid phase microextraction-gas chromatography-tandem mass spectrometry（SPME-GC-MS/MS）. Methods Wine samples were diluted and subjected to SPME, and then detected by GC-MS/MS. The SPME parameters were optimized, including fiber selection, extraction type and extraction time and so on. The limits of detection（LODs）, recoveries and precisions were investigated. Results Totally 94 kinds of pesticides were selected as the detection compounds with LODs10 μg/L, average recoveries in the range of 60%~110%, and the repeatability and reproducibility less than 20% and 30%, respectively. Conclusion The proposed method is simple and rapid, with the analysis time less than 1 h, which is suitable for the rapid and high-through screening of pesticides in wine.

关 键 词：固相微萃取 气相色谱-串联质谱法 葡萄酒 农药残留 

分 类 号：O657.63[理学—分析化学] TS262.6[理学—化学]