超高效液相色谱-高分辨质谱法结合柱前衍生快速检测白酒中甲醛含量  

Rapid determination of formaldehyde in Baijiu by UPLC-Q/Orbitrap HRMS combined with precolumn derivatization

作　　者：蒋力力 黎露露 付嘉 尹艳艳 杨军林 田栋伟 尤小龙 程平言 JIANG Lili;LI Lulu;FU Jia;YIN Yanyan;YANG Junlin;TIAN Dongwei;YOU Xiaolong;CHENG Pingyan(Guizhou Maotai Distillery(Group)Xijiu Co.,Ltd.,Zunyi 564622,China)

机构地区：[1]贵州茅台酒厂(集团)习酒有限责任公司,贵州遵义564622

出　　处：《食品与发酵工业》2023年第11期260-266,共7页Food and Fermentation Industries

基　　金：贵州省科技计划项目(黔科合成果[2020]2Y042);遵义市优秀青年科技创新人才培养项目(遵优青[2019]1号);贵州省十大千亿级工业(优质烟酒)专项资金项目(黔财工[2019]226号);贵州省纯粮固态酿造技术工程研究中心建设(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：该研究采用超高效液相色谱-高分辨质谱(ultra performance liquid chromatography-Q/Orbitrap high resolution mass spectrometry,UPLC-Q/Orbitrap HRMS)结合柱前衍生建立了白酒样品中甲醛含量的分析方法。白酒样品经乙酰丙酮衍生,通过全扫描/数据依赖性二级扫描(Full MS-ddMS 2)模式检测,外标法定量。该方法在5.1~202.0μg/L范围内线性良好(R 2>0.99),相对标准偏差<5.0%,平均加标回收率在85.66%~116.50%,适用于白酒样品中甲醛含量的检测分析。运用该方法分析酱香型白酒酿造过程甲醛含量变化,确定酱香型白酒中甲醛主要产生于贮存过程,其中三、四、五、六轮次基酒甲醛含量最高,可能含有较高的甲醛前体物质,是白酒生产过程中甲醛产生的关键风险点。In this study,a method for the analysis of formaldehyde content in Baijiu was established by UPLC-Q/Orbitrap HRMS combined with precolumn derivatization.Baijiu were derivatized with acetylacetone,detected by Full MS-ddMS2 mode,and quantified by external standard method.The linearity of the method was good in the range of 5.1-202.0μg/L(R 2>0.99),the relative standard deviation was less than 5.0%,and the average recovery rate of standard addition was 85.66%-116.50%.It was suitable for the determination of formaldehyde content in Baijiu.This method was used to analyze the change of formaldehyde content during the brewing process of Maotai-flavored Baijiu,the analysis result showed that the formaldehyde in Maotai-flavor Baijiu was mainly produced in the storage process,among with the third,fourth,fifth and sixth rounds of base Baijiu has the highest formaldehyde content which may contain higher formaldehyde precursor substances,which is the key risk points of formaldehyde production in Bajiu production.

关 键 词：白酒 甲醛 衍生 超高效液相-高分辨质谱 发酵过程 

分 类 号：O657.63[理学—分析化学] TS262.3[理学—化学]