基于SPE-GC-MS对白酒中6种长链游离脂肪酸的测定及差异性分析  

Determination and differential analysis of six long-chain free fatty acids in Baijiu based on SPE-GC-MS

作　　者：胥鑫钰 吕志远 刘玉涛 张梦梦 李小杰 秦炳伟 赵巧珍 李强 邱振清 高红波 苏静[1] XU Xinyu;LV Zhiyuan;LIU Yutao;ZHANG Mengmeng;LI Xiaojie;QIN Bingwei;ZHAO Qiaozhen;LI Qiang;QIU Zhenqing;GAO Hongbo;SU Jing(College of Bioengineering,Qilu University of Technology(Shandong Academy of Sciences),Jinan 250353,China;Jinan Baotuquan Liquor-making Co.,Ltd.,Jinan 250115,China;China National Research Institute of Food&Fermentation Industries Co.,Ltd.,Beijing 100027,China)

机构地区：[1]齐鲁工业大学(山东省科学院)生物工程学院,山东济南250353 [2]济南趵突泉酿酒有限责任公司技术质量部,山东济南250115 [3]中国食品发酵工业研究院有限公司,北京100027

出　　处：《中国酿造》2023年第9期198-203,共6页China Brewing

基　　金：山东省自然科学基金(ZR2019MC010);山东省重点研发计划(2019JZZY011003,2020CXGC010603);泰山产业领军人才(scy20180103)。

摘　　要：为建立一种准确测定白酒中月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、油酸、亚油酸六种长链游离脂肪酸(FFAs)的方法,该研究基于衍生化-气相色谱-质谱(GC-MS)法,对衍生化试剂、萃取方法及色谱柱进行优化研究。结果表明,白酒中6种长链游离脂肪酸的最佳测定条件为采用BF3-甲醇为衍生试剂,采用固相萃取(SPE)法,CP-WAX色谱柱进行气相色谱-质谱(GC-MS)分析。在该分析条件下,6种长链游离脂肪酸在线性范围内相关系数R2均>0.993,方法检出限为0.002~0.009 mg/L,方法的精密度试验结果相对标准偏差(RSD)为3.9%~9.3%,回收率为92%~112%。该方法准确度和精密度良好,适合于白酒中月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、油酸、亚油酸6种长链游离脂肪酸的定量检测。To establish a method for the accurate determination of six long-chain free fatty acids(FFAs)including lauric acid,myristic acid,palmitic acid,stearic acid,oleic acid and linoleic acid in Baijiu,the derivatization reagents,extraction methods and columns were optimized based on derivatized-gas chromatography-mass spectrometry(GC-MS).The results showed that the optimal conditions for the determination of six long-chain free fatty acids in Baijiu were as follows:using BF3-methanol as the derivation reagent,solid phase extraction(SPE)method and CP-WAX column for GC-MS analysis.Under the analysis conditions,the correlation coefficient R2 of the six long-chain free fatty acids in the linear range were all>0.993,the detection limit of the method was 0.002-0.009 mg/L,relative standard deviation(RSD)of precision tests results ranged from 3.9%to 9.3%,and the adding standard recoveries were 92%-112%.The method had good accuracy and precision,and was suitable for the quantitative detection of six long-chain free fatty acids of lauric acid,myristic acid,palmitic acid,stearic acid,oleic acid and linoleic acid in Baijiu.

关 键 词：气相色谱-质谱法 白酒 游离脂肪酸 样品处理 

分 类 号：TS261.7[轻工技术与工程—发酵工程]