固相萃取-气相色谱-串联质谱法测定葡萄酒中4种新型杀菌剂  

Determination of Four Fungicides in Grape wine by Gas Chromatograpy-Tandem Mass Spectrometry

作　　者：刘滨 陈瑶 朱振瓯 黄芙珍 韩超 胡贝贞 LIU Bin;CHEN Yao;ZHU Zhen-ou;HUANG Fu-zhen;HAN Chao;HU Bei-zhen(Wenzhou Entry-Exit Inspection and Quarantine Bureau ,Wenzhou 325027;Shaoxing Entry-Exit Inspection and Quarantine Bureau Integrated Technical Service Center, Shaoxing 312000)

机构地区：[1]温州出入境检验检疫局,浙江温州325027 [2]绍兴出入境检验检疫局综合技术服务中心,浙江绍兴312000

出　　处：《分析科学学报》2018年第6期837-840,共4页Journal of Analytical Science

基　　金：浙江省科技计划(No.2017C37058);浙江省151人才工程项目

摘　　要：建立了固相萃取-气相色谱-串联质谱法同时测定葡萄酒中硅噻菌胺、氟吡菌胺、吲哚磺菌胺和啶酰菌胺4种杀菌剂的分析方法。葡萄酒样品经HR-X固相萃取小柱提取和净化,乙酸乙酯洗脱目标物,在气相色谱-串联质谱多反应监测模式(MRM)下进行检测,外标法定量。在优化的条件下,4种杀菌剂在2.0～100.0ng·mL^(-1)范围内呈良好的线性关系,相关系数均≥0.9988,方法定量限为2.0μg·kg^(-1)。方法平均回收率为77.2%～93.9%,相对标准偏差≤7.8%。本方法前处理简单、选择性好、灵敏度高,可用于葡萄酒中以上4种杀菌剂的测定。A gas chromatography-tandem mass spectrometry(GC-MS/MS)method was developed for the simultaneous determination of four fungicides,including silthiofam,fuopicolide,amisulbrom and boscalid in grape wine.Wine samples were extracted and cleaned up with HR-X solid phase extraction column,the four fungicides were eluted with ethyl acetate and determined with GC-MS/MS in multiple reaction monitoring transitions(MRMs)mode and the quantification was performed by the external standard method.The results indicated that the calibration curves for the four fungicides were linear in the range of 2.0-100.0ng·mL^-1 ,with correlation coefficients not less than 0.9988.The limits of quantification was 2.0μg·kg^-1.The recoveries ranged from 77.2% to 93.9% with the RSDs not more than 7.8%.This method is simple,selective and sensitive,and it is suitable for the determination of the four fungicides in grape wine.

关 键 词：葡萄酒 杀菌剂 固相萃取 气相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]