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

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。

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

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.