食品与发酵工业 >

2021 , Vol. 47 >Issue 10: 235 - 239

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.025926

分析与检测

定量核磁共振氢谱测定发酵饮料中乙醇、乙酸的含量

  • 梁光焰 ,
  • 姜阳明 ,
  • 周美 ,
  • 夏宇 ,
  • 李春燕 ,
  • 胡恩明 ,
  • 颜秋晓 ,
  • 王道平
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  • 1(贵州医科大学,省部共建药用植物功效与利用国家重点实验室,贵州 贵阳,550014)
    2(贵州省中国科学院天然产物化学重点实验室,贵州 贵阳,550014)
硕士研究生(王道平副研究员为通讯作者,E-mail:wdp_7897@aliyun.com)

收稿日期: 2020-10-19

  修回日期: 2021-01-06

  网络出版日期: 2021-06-17

基金资助

贵州省科技计划项目(黔教合[2020]018;黔科合平台人才[2017]5713);贵阳市科技项目(筑科合同[2017]8-2号);贵州省科技支撑项目(黔科合支撑(2018)2308号;黔科合支撑[2020]1Y142号);贵州省教育厅科技人才成长项目(黔教合KY字[2018]197)

收起

Determination of ethanol and acetic acid in fermented drinks by q1H-NMR

  • LIANG Guangyan ,
  • JIANG Yangming ,
  • ZHOU Mei ,
  • XIA Yu ,
  • LI Chunyan ,
  • HU Enming ,
  • YAN Qiuxiao ,
  • WANG Daoping
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  • 1(State Key Laboratory of Functions and Applications of Medicinal Plants, Guizhou Medical University, Guiyang 550014, China)
    2(The Key laboratory of Chemistry for Natural Products of GuiZhou Province and Chinese Academy of Sciences, Guiyang 550014,China)

Received date: 2020-10-19

  Revised date: 2021-01-06

  Online published: 2021-06-17

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摘要

以乙醇、乙酸为研究对象,采用定量核磁共振氢谱技术测定发酵饮料中乙醇、乙酸的含量。使用氘代二甲基亚砜为溶剂,3-(三甲基甲硅烷基)丙酸-d4钠[sodium 3-(trimethylsilyl) propionate-2,2,3,3-d4,TMSP]为内标,90°脉冲,扫描次数(NS)为16,弛豫时间(D1)为20 s,采样时间(AQ)为4.50 s,298 K恒温测试。以乙醇(1.10 ppm)、乙酸 (1.80 ppm)及TMSP(0.00 ppm)峰为定量峰,对5种发酵饮料中乙醇、乙酸的含量进行测定。q1H-NMR测定乙醇线性范围为64.05~0.32 mg/mL,回收率99.68%~100.65%;乙酸线性范围为19.51~0.20 mg/mL,回收率98.38%~99.24%;乙醇、乙酸重复性相对标准差分别为0.11%、0.99% (n=6),48 h内测试结果准确可信。q1H-NMR技术可用于发酵饮料中乙醇、乙酸的含量测定,该方法操作高效简便、不损耗样品,检测结果准确可靠,拓宽了醇、酸类成分的检测手段。

关键词： 定量核磁共振; 乙醇、乙酸含量; 发酵饮料

本文引用格式

梁光焰 , 姜阳明 , 周美 , 夏宇 , 李春燕 , 胡恩明 , 颜秋晓 , 王道平 . 定量核磁共振氢谱测定发酵饮料中乙醇、乙酸的含量[J]. 食品与发酵工业, 2021 , 47(10) : 235 -239 . DOI: 10.13995/j.cnki.11-1802/ts.025926

Abstract

A quantitative analysis using q1H-NMR was developed for the determination of ethanol and acetic acid in fermented drinks. The NMR experimental conditions were as follows: using DMSO-d6 as solvent, TMSP as internal standard, 90° pulse, scanning times NS (16), relaxation time D1 (20 s), sampling time AQ (4.5 s), constant temperature test at 298 K. Using ethanol (1.10 ppm), acetate acid (1.80 ppm) and TMSP (0.00 ppm) peaks as quantitative peaks, the content of ethanol and acetic acid in five fermented drinks were determined. The linear range and recovery rate of ethanol was 64.05-0.32 mg/mL and 99.68%-100.65%, and those for acetate acid was 19.51-0.20 mg/mL and 98.38%-99.24%. The repeatability RSD of ethanol and acetic acid were 0.11% and 0.99% (n=6), respectively, and the test results were accurate and reliable within 48 hours. The high universality, accuracy, reproducibility, and efficiency of the q1H-NMR method demonstrated in this work suggest that this method could serve as a highly potential quantification alternative for quality assessment of alcohols and acids.

Key words： q1H-NMR; cotent of ethanol and acetic acid; fermented drinks

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