GC-MS测定白酒中棕榈酸乙酯、油酸乙酯及亚油酸乙酯  

Determination of Ethyl Palmitate, Ethyl Oleate and Ethyl Linoleate in Liquor by Gas Chromatography-Mass Spectrometry(GC-MS)

作　　者：刘奕霏 廉哲[2] 梁鲁宁[2] 尹宝华[2] 邹洪[1] 

机构地区：[1]首都师范大学,北京100048 [2]公安部物证鉴定中心,北京100038

出　　处：《刑事技术》2016年第2期111-115,共5页Forensic Science and Technology

基　　金：基本科研业务费专项资金(No.2013JB001)

摘　　要：白酒的有机成分分析是白酒真伪区分和串并溯源工作的重要手段,通过有机成分分析可以得到白酒的有机物组成及含量信息,为鉴别工作提供证据支持。本文建立了白酒中棕榈酸乙酯、油酸乙酯和亚油酸乙酯的气相色谱-质谱联用检测方法。定性方法主要将未知样品与标准品总离子流色谱图及NIST谱库中色谱图进行比对。定量方法考察了3种高级脂肪酸酯的内标标准曲线及相关系数、加标回收率、检出限、定量限、日间及日内精密度。3种高级脂肪酸酯的内标标准曲线相关系数在0.99以上,以乙醇为空白的加标回收率在90%~110%之间。并将该方法运用于案件一例。结果表明该方法能够支持鉴定结论,且快速、准确、灵敏度高,能对白酒中棕榈酸乙酯、油酸乙酯和亚油酸乙酯进行有效分析,可用于白酒分析工作。Determining the organic components in liquor remains an important approach for the identification of liquor. The information about the composition and content of organic substance in liquor can provide evidence to support the relevant identification. Three substances, ethyl palmitate, ethyl oleate and ethyl linoleate, which are of widespread presence in liquor, were systematically analyzed by GC-MS in this study. We designed an experiment to select appropriate separation column from TR-5MS（medium polarity）, CP-Wax57（polarity） and DB-FFAP（polarity）, finally choosing the DB-FFAP（polarity） column for the subsequent analysis. The temperature procedure was as follows： at 50 ℃ for the sample to be pretreated for 2 min, then 120 ℃ achieved by 2 ℃ /min for 2min, and the further 170 ℃ reached by 6 ℃ /min for 2 min. The sample was continuously heated to 220 ℃ by 10 ℃ /min for 20 min. Helium was the carrier gas and the flow rate was 1 m L/min. The split ratio was 30：1. For the qualitative analysis, the total ion chromatogram（TIC） of the unknown samples was compared with that of the standard substance and the stored in the library of NIST. On the quantitative test, the three substances, ethyl palmitate, ethyl oleate and ethyl linoleate, were examined. The correlation coefficients of the standard curves are over 0.99 with the average recoveries varying from 90 % to 110 %. The LODs are in the range of 0.07~0.11 μg/m L and the LOQs are 0.7~1.0 μg/m L. The inter-day precisions are less than 5% and those of the intra-day less than 10%. We have used this method in a case, the contents of the ethyl palmitate, ethyl oleate and ethyl linoleate in the unknown samples were compared with the standard and a conclusion was obtained that the unknown samples were counterfeit. The method is efficient, reliable and sensitive, can meet the requirements for the determination of ethyl palmitate, ethyl oleate and ethyl linoleate in liquor.

关 键 词：棕榈酸乙酯 油酸乙酯 亚油酸乙酯 气相色谱-质谱联用 白酒 

分 类 号：DF794.3[政治法律—诉讼法学]