食品科学 ›› 2024, Vol. 45 ›› Issue (6): 164-174.doi: 10.7506/spkx1002-6630-20230512-105

• 成分分析 • 上一篇    下一篇

UPLC-HRMS法同时直接测定白酒中多种痕量呈香呈味物质及衍生物含量

杨军林,尹艳艳,尹延顺,杨少娟,田栋伟,谢丹,尤小龙,吴成,胡建锋,张德芹   

  1. (贵州习酒股份有限公司,贵州 遵义 564622)
  • 出版日期:2024-03-25 发布日期:2024-04-03
  • 基金资助:
    遵义市优秀青年科技创新人才培养项目(遵优青[2019]1);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); 贵州省工业和信息化发展专项资金项目(黔财工[2021]165)

Simultaneous Direct Determination of Various Trace Aroma and Flavor Substances and Derivatives in Baijiu by UPLC-HRMS

YANG Junlin, YIN Yanyan, YIN Yanshun, YANG Shaojuan, TIAN Dongwei, XIE Dan, YOU Xiaolong, WU Cheng, HU Jianfeng, ZHANG Deqin   

  1. (Guizhou Xijiu Co. Ltd., Zunyi 564622, China)
  • Online:2024-03-25 Published:2024-04-03

摘要: 为建立一种快速、准确测定白酒中多种痕量呈香呈味物质及衍生物含量的定性定量方法,对白酒样品进行高速离心、过滤等简单前处理后,直接通过Hypersil Gold C18(150 mm×2.1 mm,1.9 μm)色谱柱进行待测物分离,再结合高分辨质谱仪实现白酒中多种痕量呈香呈味物质及衍生物的定性定量分析。结果表明,该方法前处理过程无需除乙醇以及有机溶剂提取,且仅需16 min便可完成白酒中多组分含量分析;配制17 种氨基酸、4 种生物胺及11 种难挥发性有机酸的混合标准品系列溶液,经线性拟合发现各待测组分的标准工作曲线线性关系良好(R2>0.990),且各待测组分的检出限、定量限值相对较低,可满足实际白酒样品相关化合物的分析需求;同时,各待测组分的平均回收率为71.92%~117.45%,且相对标准偏差为0.46%~5.48%,该方法对白酒中多种痕量呈香呈味物质及衍生物具有良好的回收率、精密度及稳定性。因此,该方法具有操作简单、灵敏度高及重复性好等优点,对于解析白酒中其他非挥发性呈香呈味物质的种类及其含量具有借鉴意义。

关键词: 呈香呈味物质;同时直接测定;白酒;超高效液相色谱-高分辨质谱法

Abstract: A rapid and accurate qualitative and quantitative method based on ultra-high performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS) was established for the determination of various trace aroma and flavor substances and their derivatives in baijiu. Samples were centrifuged at high speed, filtered and separated on a Hypersil Gold C18 (150 mm × 2.1 mm, 1.9 μm) column before analysis. The results showed that the pretreatment process allowed multi-component analysis of baijiu without extraction using ethanol or other organic solvents within 16 minutes. The calibration curves established using a mixed standard solution of 17 amino acids, 4 bioamines and 11 non-volatile organic acids exhibited good linearity (R2 > 0.990), and the detection limits and quantitation limits were relatively low for all analytes, which meet the requirements of the compositional analysis of baijiu. The average recoveries for all analytes were 71.92%–117.45%, with relative standard deviations (RSDs) of 0.46%–5.48%. The developed method had good recovery, precision, and stability for all analytes. Therefore, this method has the advantages of simple operation, high sensitivity, and good repeatability, and is of reference significance for the analysis of the types and contents of other non-volatile flavor substances in baijiu.

Key words: aroma and flavor substances; simultaneous direct determination; baijiu; ultra-high performance liquid chromatography-high-resolution mass spectrometry

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