呈苦味三羟基十八烯酸UPLC-HRMS测定方法优化及其在白酒检测中的应用  

Optimization and Application of Ultra-high Performance Liquid Chromatography-High Resolution Mass Spectrometry for Determination of the Bitter Compound Trihydroxyoctadecenoic Acid in Chinese Baijiu

作　　者：杨军林 田栋伟 尹艳艳 蒋力力 黎露露 张二康 胡峰 程平言 YANG Junlin;TIAN Dongwei;YIN Yanyan;JIANG Lili;LI Lulu;ZHANG Erkang;HU Feng;CHENG Pingyan(Guizhou Xijiu Co.Ltd.,Zunyi 564622,China)

机构地区：[1]贵州习酒股份有限公司,贵州遵义564622

出　　处：《食品科学》2023年第8期352-359,共8页Food Science

基　　金：遵义市优秀青年科技创新人才培养项目(遵优青[2019]1号);贵州省科技计划项目(黔科合[2020]2Y042);贵州省纯粮固态酿造技术工程研究中心建设项目(黔财建[2019]303号);贵州省工业和信息化发展专项资金项目(黔财工[2021]165号)。

摘　　要：为分析白酒中呈苦味三羟基十八烯酸成分的含量,优化超高效液相色谱-高分辨率质谱测定方法。样品经直接稀释过膜后上机分析,结果显示,选择乙腈为有机相,0.1%甲酸溶液为水相,流速0.3 mL/min,进样量2μL,在Hypersic Gold色谱柱(100 mm×2.1 mm,1.9μm)经梯度洗脱程序下可有效分离待测物,同时对比二级子离子与Mass Frontier 8.0软件理论模拟待测物分子离子碎裂子离子结构图可实现定性分析,有效避免样品假阳性结果的出现,故该方法具有前处理简单、分析速度快、检出限低(0.2 ng/mL)、准确度高等优点,可实现白酒样品的检测需求;利用该方法研究酱香型白酒生产过程中呈苦味三羟基十八烯酸的含量变化,结果发现随着发酵时间的延长,酿酒原料中大量的亚油酸可能被氧化分解为三羟基十八烯酸,进而随蒸馏迁移入基酒;不同贮存时间基酒中呈苦味三羟基十八烯酸含量并无明显的变化规律,表明贮存时间对其含量影响不大;酱香型白酒3个典型体以酱香典型体基酒中呈苦味三羟基十八烯酸含量较低,可用于后续包装产品的主体基酒之一。An ultra-high performance liquid chromatography-high resolution mass spectrometric(UPLC-HRMS)method was developed,optimized and applied to analyze the bitter compound trihydroxyoctadecenoic acid in Chinese baijiu.The samples were diluted and filtered through a 0.22μm membrane before analysis.Acetonitrile was selected as the organic phase and 0.1%formic acid as the aqueous phase with a flow rate of 0.3 mL/min and an injection volume of 2μL.The analyte was separated on a Hypersic Gold(100 mm×2.1 mm,1.9μm)column by gradient elution,and qualitative analysis was achieved by comparison of secondary daughter ions and theoretical simulation of molecular ion fragment structures using the Mass Frontier 8.0 software,which could avoid false positive results.This method had the advantages of simple pretreatment,fast analysis,low detection limit(0.2 ng/mL)and high accuracy,and could meet the requirements for the detection of baijiu samples.This method was used to study the change in the content of trihydroxyoctaenoic acid during the production process of Maotai-flavor baijiu.The results showed that with the prolongation of fermentation time,a large amount of linoleic acid in the raw materials was likely to be oxidized and decomposed into trihydroxyoctadecenoic acid,and then transferred into the base liquor by distillation.The content of trihydroxyoctadecenoic acid in the base liquor did not obviously change during storage,indicating that it was affected little by storage time.The content of trihydroxyoctadecenoic acid in Maotai-flavor base liquor was lowest among the three typical bodies of Maotai-flavor baijiu,so Maotai-flavor base liquor could be used as one of the major base liquors for packaged products.

关 键 词：苦味 三羟基十八烯酸 白酒 方法优化 

分 类 号：O657.63[理学—分析化学]