顶空-固相微萃取-气相色谱串联质谱法测定葡萄酒中多种氯酚及氯代茴香醚  

Determination of Chlorophenols and Chloroanisols in Wine by Headspace Solid-Phase Microextraction and Gas Chromatography-Tandem Mass Spectrometry

作　　者：陈树兵[1] 孟原[2] 施瑛[3] 倪梅林[1] 莫燕霞[1] 贺小雨[1] 

机构地区：[1]宁波出入境检验检疫局技术中心,浙江宁波315012 [2]宁波大学海洋学院,浙江宁波315211 [3]南京农业大学理学院,江苏南京225001

出　　处：《食品科学》2012年第16期146-149,共4页Food Science

基　　金：国家质检总局科技计划项目(2009IK172)

摘　　要：样品中氯酚经乙酰化生成乙酰氯酚后,通过优化萃取头、离子强度、温度、时间等固相微萃取条件后,建立顶空-固相微萃取-气相色谱串联质谱法同时测定测定葡萄酒中的3种氯酚2,4,6-三氯酚(TCP)、2,3,4,6-四氯酚(TeCP)、五氯酚(PCP)以及两种氯代茴香醚2,4,6-三氯苯甲醚(TCA)、五氯苯甲醚(PCA)含量的方法。结果表明:该方法检出限为0.1ng/L,回收率为86.0%～105.9%,相对标准偏差小于16.5%。该方法前处理简单、高效、检测灵敏度高,可应用于进出口葡萄酒中木塞污染物的监控。A headspace solid-phase microextraction and gas chromatography-tandem mass spectrometric （HS-SPME- GC- MS/MS） method was proposed for the simultaneous determination of three chlorophenols 2,4,6-trichlorophenol （TCP）, 2,3,4, 6-tetrachlorophenol （TeCP）, pentachlorophenol （PCP） and two chloroanisols including pentachloroanisol （PCA） and 2,4,6- trichloroanisol （TCA） in wine. Chlorophenols from wine samples were acetylated and then analyzed by GC-MS/MS in a multi- reaction monitoring （MRM） mode. Four extraction parameters including extraction fiber, ion strength, extraction temperature and extraction time were optimized. The results showed that the limit of detection of this method was 0.1 ng/L. The average spike recovery rates of five analytes in a positive sample were 86.0%-- 105.9% with a RSD less than 16.5% （n = 5）. This method was simple, effective, sensitive and therefore applicable to monitor cork taint in exported and imported wine.

关 键 词：氯代茴香醚 氯酚 顶空-固相微萃取 气相色谱串联质谱 葡萄酒 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657[轻工技术与工程—食品科学与工程]