分析与检测

超高效液相色谱质谱法测定酱香型酒曲原料中氨基酸含量

  • 乔敏莎 ,
  • 王凡 ,
  • 山其木格 ,
  • 乔晓娜 ,
  • 毕荣宇 ,
  • 张长霞 ,
  • 卢君
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  • 1(天士力医药集团股份有限公司研究院,天津,300410)
    2(贵州国台酒业集团股份有限公司,贵州 仁怀,564501)
硕士,中级工程师(卢君高级工程师为通信作者,E-mail:lujun951@tasly.com)

收稿日期: 2022-07-25

  修回日期: 2022-08-18

  网络出版日期: 2023-07-13

基金资助

贵州省科技成果应用及产业化计划项目(黔科合成果[2020]2Y045);贵州省仁怀市科技计划项目(仁科支撑[2020]04号);遵义市科技计划项目(遵市科合R&D[2020]31号;遵市科合支撑GY[2021]40号)

Direct determination of 19 amino acids in raw materials of Moutai-flavor Jiuqu by ultra performance liquid chromatography-tandem mass spectrometry

  • QIAO Minsha ,
  • WANG Fan ,
  • SHAN Qimuge ,
  • QIAO Xiaona ,
  • BI Rongyu ,
  • ZHANG Changxia ,
  • LU Jun
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  • 1(Tasly Academy, Tasly Holding Group Co.Ltd., Tianjin 300410, China)
    2(Guizhou Guotai Distillery Co.Ltd., Renhuai 564501, China)

Received date: 2022-07-25

  Revised date: 2022-08-18

  Online published: 2023-07-13

摘要

利用超高效液相色谱-质谱联用仪(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)建立了一种高效、快速测定酱香型白酒酿造大曲及制曲原料小麦中19种游离氨基酸的方法,并对酱酒制曲过程中氨基酸的变化规律进行初步探究。样品经粉碎、超声提取、离心及适当稀释后,可直接用于含量分析。结果表明,19种游离氨基酸在特定范围内线性关系良好(R2≥0.998 3),检出限为0.3~6.1 ng/mL,定量限为2.1~29.3 ng/mL,加标回收率为84.5%~118.5%,方法重复性和仪器精密度相对标准偏差均低于6.5%(n=6)。该方法具有分析速度快、灵敏度高且选择性好的优点,适用于酱香型白酒酿造大曲及原料中19种游离氨基酸的定量分析。

本文引用格式

乔敏莎 , 王凡 , 山其木格 , 乔晓娜 , 毕荣宇 , 张长霞 , 卢君 . 超高效液相色谱质谱法测定酱香型酒曲原料中氨基酸含量[J]. 食品与发酵工业, 2023 , 49(12) : 278 -284 . DOI: 10.13995/j.cnki.11-1802/ts.033093

Abstract

An efficient and rapid method was established by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of 19 free amino acids in Moutai-flavor Daqu starter and its raw material -wheat.And the variation tendency of these amino acids in the production process of Moutai-flavor Daqu starter was preliminarily analyzed.The sample was for direct content determination after crushing, ultrasonic extraction, centrifugation and appropriate dilution.The results showed that the linear relationship of these 19 free amino acids was good within a specific range (R2≥0.998 3), the limit of detection (LOD) was 0.3-6.1 ng/mL, the limit of quantitation (LOQ) was 2.1-29.3 ng/mL, and the recovery rate was 84.5%-118.5%.The relative standard deviation values of repeatability and instrument precision were both less than 6.5% (n=6).The method has the advantages of high speed, high sensitivity and good selectivity and is suitable for the quantitative analysis of 19 free amino acids in Moutai-flavor Daqu starter and its raw material.

参考文献

[1] 胡鹏刚, 邱树毅, 李继杰.酱香大曲酒生产工艺关键环节与其风格质量的关系[J].酿酒科技, 2010(8):36-39.
HU P G, QIU S Y, LI J J.Relations between key production techniques of Maotai-flavor Daqu and its quality and styles[J].Liquor-Making Science & Technology, 2010(8):36-39.
[2] 霍嘉颖, 黄明泉, 孙宝国, 等.中国白酒中功能因子研究进展[J].酿酒科技, 2017(9):17-23.
HUO J Y, HUANG M Q, SUN B G, et al.Research progress in functional factors in Baijiu[J].Liquor-Making Science & Technology, 2017(9):17-23.
[3] YIN H A, HE Y, DENG Y, et al.Application of Plackett-Burman experimental design for investigating the effect of wort amino acids on flavor-active compounds production during lager yeast fermentation[J].Journal of the Institute of Brewing, 2017, 123(3):300-311.
[4] 苟静瑜, 贾智勇, 闫宗科, 等.降低白酒中高级醇含量的研究进展[J].酿酒, 2016, 43(4):25-29.
GOU J Y, JIA Z Y, YAN Z K, et al.Research progress in decreasing the contents of higher alcohols in Baijiu (liquor)[J].Liquor Making, 2016, 43(4):25-29.
[5] 仇钰莹, 方芳, 周新虎, 等.酒醅中精氨酸利用菌株的分离筛选及其对浓香型白酒中瓜氨酸积累的影响[J].微生物学报, 2016, 56(10):1 638-1 646.
QIU Y Y, FANG F, ZHOU X H, et al.Characterization of arginine utilization strains from fermented grains and evaluation of their contribution to citrulline accumulation in Chinese Luzhou-flavor spirits[J].Acta Microbiologica Sinica, 2016, 56(10):1 638-1 646.
[6] FAN W L, SHEN H Y, XU Y.Quantification of volatile compounds in Chinese soy sauce aroma type liquor by stir bar sorptive extraction and gas chromatography-mass spectrometry[J].Journal of the Science of Food and Agriculture, 2011, 91(7):1 187-1 198.
[7] 温永柱, 范文来, 徐岩, 等.白酒中5种生物胺的HPLC定量分析[J].食品工业科技, 2013, 34(7):305-308.
WEN Y Z, FAN W L, XU Y, et al.Quantification for 5 selected biogenic amines in Chinese liquor by HPLC[J].Science and Technology of Food Industry, 2013, 34(7):305-308.
[8] 张巧玲, 吕锡斌, 秦兴, 等.酱香型白酒高温大曲游离氨基酸比较分析[J].中国酿造, 2019, 38(4):53-57.
ZHANG Q L, LV X B, QIN X, et al.Comparative analysis of free amino acids in high temperature Daqu of Moutai-flavor Baijiu[J].China Brewing, 2019, 38(4):53-57.
[9] 聂元皓, 徐岩, 吴群, 等.芳香族化合物前体物质酪氨酸和苯丙氨酸在白酒中的来源解析[J].食品与发酵工业, 2018, 44(10):1-6.
NIE Y H, XU Y, WU Q, et al.Analysis on source of tyrosine and phenylalanine as precursors of aromatic compounds in Baijiu (Chinese liquor)[J].Food and Fermentation Industries, 2018, 44(10):1-6.
[10] 柳习月, 朱琪, 杨帆, 等.蛋白组学揭示苯丙氨酸代谢对酱香大曲风味影响[J].食品科技, 2021, 46(8):1-6.
LIU X Y, ZHU Q, YANG F, et al.Proteomics reveals the effect of phenylalanine metabolism on the flavor of Daqu[J].Food Science and Technology, 2021, 46(8):1-6.
[11] 陈雪, 梁克红, 朱宏, 等.游离氨基酸检测方法及其应用[J].食品安全质量检测学报, 2021, 12(18):7 298-7 304.
CHEN X, LIANG K H, ZHU H, et al.Analysis method and application of free amino acids[J].Journal of Food Safety & Quality, 2021, 12(18):7 298-7 304.
[12] PIESTANSKY J, OLESOVA D, GALBA J, et al.Profiling of amino acids in urine samples of patients suffering from inflammatory bowel disease by capillary electrophoresis-mass spectrometry[J].Molecules, 2019, 24(18):3345.
[13] 孙洁, 李好转, 孙立臻, 等.芝麻香型白酒酒醅中游离氨基酸分析方法探讨[J].酿酒科技, 2014(4):93-95.
SUN J, LI H Z, SUN L Z, et al.Exploration on the analytical method of free amino acids in the fermented grains of sesame-flavor liquor[J].Liquor-Making Science & Technology, 2014(4):93-95.
[14] QIU X, REYNOLDS R, JOHANNINGSMEIER S, et al.Determination of free amino acids in five commercial sweetpotato cultivars by hydrophilic interaction liquid chromatography-mass spectrometry[J].Journal of Food Composition and Analysis,2020,92:103522.
[15] DESMONS A, THIOULOUSE E, HAUTEM J Y, et al.Direct liquid chromatography tandem mass spectrometry analysis of amino acids in human plasma[J].Journal of Chromatography A, 2020, 1 622:461135.
[16] 臧彬如, 周改莲, 单国顺, 等.超高效液相色谱串联三重四极杆质谱法测定梅花鹿茸中总游离氨基酸与游离氨基酸含量[J].医药导报, 2020, 39(11):1 520-1 527.
ZANG B R, ZHOU G L, SHAN G S, et al.Determination of total free amino acids and free amino acids in Sika Deer velvet antler by UPLC-QqQ-MS/MS[J]. Herald of Medicine, 2020, 39(11):1 520-1 527.
[17] VIOLI J P, BISHOP D P, PADULA M P, et al.Considerations for amino acid analysis by liquid chromatography-tandem mass spectrometry:A tutorial review[J].TrAC Trends in Analytical Chemistry, 2020, 131:116018.
[18] KRUMPOCHOVA P, BRUYNEEL B, MOLENAAR D, et al.Amino acid analysis using chromatography-mass spectrometry:An inter platform comparison study[J].Journal of Pharmaceutical and Biomedical Analysis, 2015, 114:398-407.
[19] 刘月, 丑建栋, 陈玥璋,等.小麦胚芽的营养功能成分及综合利用研究进展[J].食品工业科技, 2022, 43(12):457-467.
LIU Y, CHOU J D, CHEN Y Z, et al.Advances on nutritional functional components and comprehensive utilization of wheat germ[J].Science and Technology of Food Industry, 2022, 43(12):457-467.
[20] PEPÓ P, GYÖRI Z. Amino acid compositions in wheat species with different genomes. Cereal Research Communications, 2007, 35(4):1 685-1 699.
[21] 谢佳. 杂醇、酸、酯组成及氨基酸对白酒醉度的调节作用[D].广州:华南理工大学, 2018.
XIE J.Effects of composition of fusel alcohols, acids and esters and amino acids on intoxicating degree of liquor[D].Guangzhou:South China University of Technology, 2018.
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