顶空固相微萃取联合气相色谱-质谱检测葡萄酒中2,4,6-三氯苯甲醚  

Optimization of Headspace Solid-Phase Microextraction Coupled to Gas Chromatography-Mass Spectrometry for the Determination of 2,4,6-Trichloroanisole in Wine

作　　者：赵英莲[1] 牟德华[1] 李艳[1] 

机构地区：[1]河北科技大学生物科学与工程学院,河北石家庄050018

出　　处：《食品科学》2016年第10期219-225,共7页Food Science

基　　金：河北省科技支撑计划课题(13397107D);河北科技大学2015年研究生创新资助项目(2015-12)

摘　　要：利用响应面法优化采用顶空固相微萃取联合气相色谱-质谱技术检测葡萄酒中2,4,6-三氯苯甲醚(2,4,6-trichloroanisole,TCA)。对萃取头进行了选择,并优化固相微萃取参数:样品体积、萃取温度、平衡时间和萃取时间等对TCA萃取效果的影响。结果表明,用聚二甲基硅氧烷/二乙烯基苯(65 μm)萃取头进行TCA萃取的最佳条件:样品9.8 mL、2 g NaCl、33℃平衡10 min、萃取90 min进行气相色谱-质谱分析,以TCA-d_5为内标物进行定量。该方法的相关系数R^2为0.999 9,重复性的相对标准偏差为1.03%,加标回收率范围在95.7%~106.1%之间,检出限和定量限分别为0.3 ng/L和1 ng/L。检测7种市售葡萄酒产品的TCA含量在0~7.6 ng/L之间,干白葡萄酒中TCA含量低于干红葡萄酒。该方法操作简单、可靠,适用于葡萄酒中TCA的测定。The objective of this study was to develop an analytical method for the determination of 2,4,6-trichloroanisole（TCA） in wine by headspace solid-phase microextraction combined with gas chromatography-mass spectrometry（HSSPME-GC-MS）. Important extraction parameters such as fiber type, sample volume, extraction temperature, equilibration time and extraction time were optimize using response surface method with the software Design Expert 7.0. The results indicated that when polydimethylsiloxane/divinylbenzene（PDMS/DVB, 65 μm） was selected as the extraction fiber, and optimised parameters for SPME were 9.8 m L of wine, 2 g of Na Cl, temperature 33 ℃, equilibration time 10 min and extraction time 90 min, followed by analysis by GC-MS and quantification using TCA-d5 as internal standard. The presented method was shown to be adequate for the purpose, with a correlation coefficient R-2 of 0.999 9, RSD of 1.03%, and recovery rates between 95.7% and 106.1%. The limit of detection（LOD） and the limit of quantification（LOQ） were 0.3 and 1 ng/L, respectively. This method was applied to analyze 7 commercial wine samples and the results revealed that the content of TCA varied between 0 and 7.6 ng/L, lower in dry white red than in dry red wine. This method is simple and reliable, and can be applied to the determination of TCA in wine.

关 键 词：响应面法 顶空固相微萃取 气相色谱-质谱 2 4 6-三氯苯甲醚 葡萄酒 

分 类 号：TS262.6[轻工技术与工程—发酵工程]