分散液相微萃取-GC-MS/MS分析葡萄酒中12种农药残留  

Determination of 12 Pesticide Residues in Wine by DLLME-GC-MS/MS

作　　者：徐豪 钱家亮 陈伟 杨娟 张廷廷 赵峰[2] XU Hao;QIAN Jialiang;CHEN Wei;YANG Juan;ZHANG Tingting;ZHAO Feng(Comprehensive Technology Center of Linyi Entry-Exit Inspection and Quarantine Bureau,Linyi 276000;Linyi University,Linyi 276000)

机构地区：[1]临沂出入境检验检疫局综合技术服务中心,临沂276000 [2]临沂大学,临沂276000

出　　处：《食品工业》2019年第11期304-308,共5页The Food Industry

基　　金：山东出入境检验检疫局科研基金项目(SK201749)

摘　　要：试验研究了用分散液相微萃取-气相色谱串联质谱法检测葡萄酒中12种农药残留的方法。当葡萄酒样品体积为5 mL时,最佳萃取条件:30μL四氯化碳为萃取剂,0.8 mL丙酮为分散剂,超声萃取0.5 min。在最佳的试验条件下,采用气相色谱串联质谱在多反应监测模式下分析,该方法对葡萄酒样品中12种农药的富集倍数在123~196之间,各农药的检出限为0.0006~0.0051μg/L;在0.5,1.0和2.5μg/L 3个水平的添加浓度下,回收率在69.9%~120.1%之间,相对标准偏差小于14.3%(n=6)。该方法准确可靠、灵敏度高,可同时检测葡萄酒中12种农药残留。The application of the dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry on the determination of 12 pesticides in wine was studied.Several extraction parameters,such as the type of extraction and dispersive solvents and their volumes,shaking mode,and extraction time,were optimized by experiments,when the wine sample volume was 5 mL.Under optimal conditions(30μL carbon tetrachloride as the extraction solvent,0.8 mL acetone as the dispersive solvent,ultrasonic extraction for 0.5 minute)and multiple reaction monitor acquisition mode,the enrichment factors of 12 pesticides ranged from 123 to 196.The limits of detection varied from 0.0006μg/L to 0.0051μg/L.The recoveries at levels of 0.5,1.0 and 2.5μg/L were ranged from 69.9%to 120.1%.The relative standard deviations were less than 14.3%(n=6).The established method was sensitive,repeatable and reliable for simultaneous analysis of 12 pesticides in wine.

关 键 词：分散液相微萃取 气相色谱串联质谱 葡萄酒 农药残留 

分 类 号：TS2[轻工技术与工程—食品科学与工程]