应用多级液液微萃取结合气质联用定量白酒中的角鲨烯

将多级液液微萃取与气相色谱-质谱联用技术相结合建立了白酒中微量角鲨烯的快速定量方法。将白酒稀释后,用戊烷-乙醚混合溶剂(1∶3,体积比)进行多级微萃取,有机相浓缩后气质联用分析。结果显示,角鲨烯在0.62~159.88μg/L范围内具有良好的线性关系,相关系数为0.995 5,角鲨烯的检出限为0.17μg/L,当加标浓度为2,20,40μg/L时回收率分别为78.1%,85.0%和103.5%,相对标准偏差(RSD)分别为12.1%,8.9%和7.0%。该方法具有简便快速、准确灵敏、萃取效率高、有机溶剂消耗少等优点,适合白酒中痕量角鲨烯的定量分析。

Quantitation of Squalene in Chinese Liquor Using Multistage Liquid-Liquid Microextraction Coupled with Gas Chromatography-Mass Spectrometry

A multistage liquid-liquid microextraction (LLME) coupled with GC-MS method was developed to determine squalene in Chinese liquor.After diluting the liquor sample,a multistage microextraction was carried out using pentane-diethyl ether mixture(1 ∶ 3,by volume),then the organic phase was concentrated with nitrogen,and analyzed by GC-MS.The result indicated that squalene had a good linearity in the range of 0.62-159.88 μg/L,with a correlation coefficient of 0.995 5.The detection limit of squalene was as low as 0.17 μg/L.The average recoveries of squalene at spiked levels of 2,20,40 μg/L were 78.1％,85.0％,103.5％,respectively,with relative deviations of 12.1％,8.9％,7.0％,respectively.With the advantages of simplicity,accuracy,high extraction efficiency and low consumption of organic solvent,this method was suitable for the quantitative analysis of squalene in Chinese liquor.