分散液液微萃取-气相色谱-质谱分析葡萄酒中单萜醇  

etermination of Mono-terpenols in Wine by Dispersive Liquid-Liquid Micro-extraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：周荔子 杨兆光[1,2] 刘耀驰[1] 杨远[1] 邱波[1] 

机构地区：[1]中南大学化学化工学院环境与水资源研究中心,长沙410083 [2]中南大学深圳研究院,深圳518057

出　　处：《分析化学》2015年第4期534-539,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21405180);湖南省自然科学基金(No.S2013J504B);环保部公益性科研专项(No.201309052)资助项目~~

摘　　要：采用分散液液微萃取与气相色谱-质谱（GC-MS）联用技术建立了葡萄酒中单萜醇（α-萜烯醇、芳樟醇、香叶醇、香茅醇）的分析方法。考察萃取剂与分散剂的种类和体积、超声和离心时间、盐的加入量、酒样中乙醇含量等因素对萃取效率的影响,确定最佳萃取条件为：在10 m L葡萄酒样中加入2,6-二叔丁基-4-甲基苯酚（BHT）作为内标,再加入100μL四氯化碳与500μL丙酮,超声3 min（40 MHz）,再离心10 min（5000 r/min）后吸取有机相进行GC-MS分析。用此条件检测4种单萜醇,线性范围为10-300μg/L,相关系数均大于0.996,检出限为6-8μg/L。实际葡萄酒样加标回收率为90.8%-96.1%,相对标准偏差为4.8%-5.6%（n=6）。本方法具有操作简单、快速、灵敏、低成本、环境友好等特点,非常适合大批量样品分析。A dispersive liquid-liquid micro-extraction procedure coupled with gas chromatography-mass spectrometry was proposed for the analysis of four mono-terpenols in wine. The pretreatment conditions including the kind and volume of extraction solvent and disperser solvent,the ultrasound time,the centrifuge time,salt addition and the alcoholicity in wines were studied. In the optimized method,100 μL CCl4and500 μL acetone were added to 10 m L wine sample mixed with butylated hydroxytoluene as internal standard.After ultrasonic for 3 minutes（ 40 MHz） and centrifugation for 10 minutes,more than 30 μL of organic phase was withdrawn for automatic sampling analysis. The standard curve of four mono-terpenols was linear in the concentration range of 10- 300 μg / L with correlation coefficients of more than 0. 996. The limits of detection were 6- 8 μg / L. In the real wine sample measurement,the recoveries were ranged from 90. 8% to 96. 1%,and the relative standard deviations were between 4. 8% and 5. 6%（ n = 6）. The whole proposed methodology demonstrated to be simple,rapid,sensitive,low-cost and environmentally friendly,which was quite suitable for the analysis of large quantities of wine samples.

关 键 词：分散液液微萃取 葡萄酒 单萜醇 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学] TS262.6[理学—化学]