超高效液相色谱-高分辨质谱法同时测定白酒中19种氨基酸  

Determination of 19 Amino Acids in Baijiu by Ultra-high Performance Liquid Chromatography-High Resolution Mass Spectrometry

作　　者：尹艳艳 杨军林 田栋伟 蒋力力 尤小龙 张健 程平言 YIN Yan-yan;YANG Jun-lin;TIAN Dong-wei;JIANG Li-li;YOU Xiao-long;ZHANG Jian;CHENG Ping-yan(Guizhou Baijiu Manufacturing Industry Innovation Center,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,贵州省白酒制造业创新中心,贵州遵义564622

出　　处：《分析测试学报》2023年第3期330-336,共7页Journal of Instrumental Analysis

基　　金：贵州省基本建设(非涉农)投资专项(黔财建[2019]303号);贵州省工业和信息化发展专项资金(黔财工[2021]165号);黔质量发展项目[2022]8号。

摘　　要：建立了白酒样品中19种氨基酸的超高效液相色谱-高分辨质谱(UPLC-HRMS)检测方法。样品经烘箱干燥法除乙醇,水定容,使用水相滤膜过滤后上机检测。以甲醇-0.1%甲酸作为流动相,经Hypersil GOLD色谱柱(150 mm×2.1 mm,1.9μm)分离,在正离子扫描模式下,一级母离子全扫描采集化合物信息,外标法定量分析。结果表明,19种氨基酸在其线性范围内线性关系良好,相关系数(r^(2))不小于0.9862,方法的检出限为0.003~0.015μmol/L,定量下限为0.008~0.050μmol/L,白酒样品中19种氨基酸的加标回收率为88.2%~119%,相对标准偏差为0.23%~5.6%,适用于白酒样品中氨基酸分析。利用该方法分析了不同轮次酱香酒中氨基酸含量,检出L-丙氨酸、L-精氨酸、L-天冬氨酸、L-谷氨酸、甘氨酸、L-组氨酸、L-异亮氨酸、L-亮氨酸、L-赖氨酸、L-苯丙氨酸、L-脯氨酸、L-丝氨酸、L-苏氨酸、L-酪氨酸、L-缬氨酸和L-瓜氨酸共16种氨基酸。不同轮次酒中氨基酸含量的显著水平P值均小于0.05,表明不同轮次酒中氨基酸含量具有显著性差异。An ultra-high performance liquid chromatography-high resolution mass spectrometry(UPLC-HRMS)was established for the determination of 19 amino acids in Baijiu.The samples were firstly removed ethanol by oven-drying method,then the volume was fixed with ultrapure water,and filtered using an aqueous phase filter membrane before analysis.The samples were separated on a Hypersil GOLD column(150 mm×2.1 mm,1.9μm)with methanol-0.1%formic acid solution as mobile phase.The data were collected in full mass scan in positive ESI mode and the external standard method was used to achieve quantitative analysis.The results showed that the calibration curves for 19 amino acids showed good linear relationships within corresponding linear range,with correlation coefficients(r^(2))not less than 0.9862.The limits of detection and the limits of quantitation were in the range of 0.003-0.015μmol/L and 0.008-0.050μmol/L,respectively.The recoveries for Baijiu samples ranged from 88.2%to 119%,with relative standard deviations of 0.23%-5.6%.This method was suitable for the determination of amino acids in Baijiu samples.The contents of amino acids in different rounds base liquor of sauce-flavor Baijiu were analyzed by this method.Sixteen amino acids,i.e.L-alanine,L-arginine,L-aspartic acid,L-glutamic acid,glycine,L-histidine,L-isoleucine,L-leucine,L-lysine,L-phenylalanine,L-proline,L-serine,L-threonine,L-tyrosine,L-valine and L-citrulline were detected.The significant level P values of amino acid contents in different rounds base liquor of sauce-flavor Baijiu were all less than 0.05,indicating that amino acid contents in different rounds base liquor had significant differences.

关 键 词：氨基酸 白酒 超高效液相色谱-高分辨质谱(UPLC-HRMS) 

分 类 号：O657.63[理学—分析化学] O629.7[理学—化学]