食品与发酵工业 >

2025 , Vol. 51 >Issue 6: 306 - 310

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.040181

分析与检测

利用核磁氢谱定量白酒中的酸酯总量

  • 王寿峰 ,
  • 兰茜 ,
  • 雍登金 ,
  • 杨惠妮 ,
  • 胡敏
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  • 1(四川轻化工大学 化工学院,四川 自贡,643000)
    2(布鲁克(北京)科技有限公司,北京,100192)
第一作者：博士,助理研究员(王寿峰助理研究员为通信作者,shoufeng.wang@163.com)

收稿日期: 2024-06-13

  修回日期: 2024-08-18

  网络出版日期: 2025-04-14

基金资助

四川省科技厅应用基础研究项目(2020YJ0404);酿酒生物技术及应用四川省重点实验室开放基金项目(NJ2018-03)

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Quantitative analysis of acid ester content in Baijiu based on nuclear magnetic resonance spectroscopy

  • WANG Shoufeng ,
  • LAN Xi ,
  • YONG Dengjin ,
  • YANG Huini ,
  • HU Min
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  • 1(School of Chemical Engineering, Sichuan University of Science & Engineering, Zigong 643000, China)    2(Bruker (Beijing) Scientific Technology Co.Ltd., Beijing 100192, China)

Received date: 2024-06-13

  Revised date: 2024-08-18

  Online published: 2025-04-14

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摘要

国标白酒分析方法中使用指示剂法检测酸酯总量,该方法耗时长且难以批量操作。该研究提供了利用溶剂峰压制核磁共振氢谱检测白酒中酸酯总量的方法。基于核磁氢谱数据,建立了不同类型羰基α位氢积分值与对应类型的酸酯物质的量拟合曲线,在酸酯总量2.5~200 mmol/L范围内,3种类型酸酯拟合曲线相关系数R2≥ 0.999 8,线性良好,酸酯总量近似等于3种类型酸酯物质的量之和。对比验证白酒基酒样品,该方法具有良好的精密度和重现性,平行3次加标回收率为99.3%~101.7%。核磁法与指示剂法相比,相对偏差<0.02。将核磁方法用于12种市售白酒检测,测试结果与指示剂法一致,检测时间仅需19 min。基于核磁共振技术可以检测白酒中的酸酯总量,操作简便,为企业及监管部门批量检测提供一种快捷方法。

关键词： 核磁共振氢谱; 白酒; 定量; 酸酯总量

本文引用格式

王寿峰 , 兰茜 , 雍登金 , 杨惠妮 , 胡敏 . 利用核磁氢谱定量白酒中的酸酯总量[J]. 食品与发酵工业, 2025 , 51(6) : 306 -310 . DOI: 10.13995/j.cnki.11-1802/ts.040181

Abstract

The indicator method in the national Baijiu analysis standard is usually used for the examination of total acid esters in Baijiu, in general, the method takes a long time and is difficult to operate in batches.A novel method was developed for measuring acid ester content in Baijiu using proton nuclear magnetic resonance spectroscopy (1H NMR) with solvent peaks suppression technology.In this method, the fitting curves of acid ester content vs the integral ratio of three different type hydrogen peaks were established, and the correlation coefficients were R2 ≥ 0.999 8 in the range of 2.5-200 mmol/L, the linearity of both curves were good, the acid ester content was approximately equal to the sum of the three types of acids and esters.Through the analysis and verification of base Baijiu samples, the method had good precision and reproducibility, with a parallel triple spiking recovery rate of 99.3%-101.7%.Compared with the indicator method, the relative deviation of the nuclear magnetic method was less than 0.02.At the same time, 12 kinds of Baijiu selected from the market were tested by nuclear magnetic resonance, and satisfactory results were obtained.Based on the nuclear magnetic resonance technology, the total amount of acids and esters in Baijiu could be quickly detected, which was easy to operate and can be detected in batches, providing a reference method for Baijiu production enterprises and regulatory departments.

Key words： 1H NMR; Baijiu; quantify; acid ester content

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