食品与发酵工业 >

2022 , Vol. 48 >Issue 21: 254 - 261

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.030478

分析与检测

低场核磁共振波谱仪快速测定饮料酒中酒精度

  • 许紫薇 ,
  • 冯翠萍 ,
  • 樊双喜 ,
  • 张柏林 ,
  • 赵宏飞 ,
  • 刘一诺 ,
  • 岳红卫 ,
  • 吉鑫 ,
  • 张松祥 ,
  • 陆玮 ,
  • 王道兵 ,
  • 卜凡 ,
  • 钟其顶
展开
  • 1(北京林业大学 生物科学与技术学院,北京,100091)
    2(中轻检验认证有限公司,北京,100015)
    3(安徽古井贡股份有限公司,安徽 亳州,236800)
    4(中国食品发酵工业研究院有限公司,北京,100015)
    5(泰科施普(北京)技术有限公司,北京,100039)
硕士研究生(钟其顶教授级高级工程师为通信作者,E-mail:zhongqiding@163.com)

收稿日期: 2021-12-22

  修回日期: 2022-03-08

  网络出版日期: 2022-12-02

基金资助

北京市朝阳区科技计划项目(CYGX2104);欧盟地平线2020计划项目(635690-OLEUM,727864-EU-China-Safe)

收起

Rapid determination of alcohol content in alcoholic beverages by low-field NMR

  • XU Ziwei ,
  • FENG Cuiping ,
  • FAN Shuangxi ,
  • ZHANG Bolin ,
  • ZHAO Hongfei ,
  • LIU Yinuo ,
  • YUE Hongwei ,
  • JI Xin ,
  • ZHANG Songxiang ,
  • LU Wei ,
  • WANG Daobing ,
  • BU Fan ,
  • ZHONG Qiding
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  • 1(College of Biological Sciences and Technology, Beijing Forestry University, Beijing 100091, China)
    2(Sinolight Inspection & Certification Co.Ltd., Beijing 100015, China)
    3(Anhui Gujing Distillery Co.Ltd., Bozhou 236800, China)
    4(China National Research Institute of Food & Fermentation Industries Co.Ltd, Beijing 100015, China)
    5(Techship (Beijing) Technology Co.Ltd., Beijing 100039, China)

Received date: 2021-12-22

  Revised date: 2022-03-08

  Online published: 2022-12-02

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摘要

基于低场台式核磁共振波谱仪,采用一维核磁共振氢谱(1H nuclear magnetic resonance,1H NMR)技术,建立了快速测定饮料酒(白酒、啤酒、葡萄酒和樱桃发酵酒)中酒精度的标曲法、内标法和外标法。方法检出限和定量限分别为0.08%和0.26%(体积分数)。在体积分数0.5%~80%时,标曲法、外标法和内标法的线性相关系数R2分别为0.996 1、0.996 1和0.999 5。3种方法的日内和日间精密度均小于5%。标曲法、外标法和内标法的加标回收率分别为88.1%~97.81%、84.61%~107.36%和81.83%~111.91%。可见此方法线性、重现性、回收率等均能达到准确定量的要求。该文所建立的1H NMR法与GB 5009.225—2016《食品安全国家标准 酒中乙醇浓度的测定》中数字密度计法的测定结果误差±5%,满足方法可行性验证要求。相比国标法,样品无需复杂前处理、样品用量少(仅需500 μL)、测样时间短(<5 min)。相对于高场核磁共振波谱仪,低场台式核磁共振波谱仪体积小、重量轻、便于移动,适合饮料酒中酒精度的快速和规模化分析。

关键词： 低场核磁共振仪; 饮料酒; 酒精度; 快速测定; 定量

本文引用格式

许紫薇 , 冯翠萍 , 樊双喜 , 张柏林 , 赵宏飞 , 刘一诺 , 岳红卫 , 吉鑫 , 张松祥 , 陆玮 , 王道兵 , 卜凡 , 钟其顶 . 低场核磁共振波谱仪快速测定饮料酒中酒精度[J]. 食品与发酵工业, 2022 , 48(21) : 254 -261 . DOI: 10.13995/j.cnki.11-1802/ts.030478

Abstract

Based on the low-field NMR, 1H NMR was used to establish the standard curve method, internal standard method, and external standard method for the rapid determination of alcohol content in Baijiu, beer, wine, and kirsch. The limits of detection and quantification were 0.08% (volume fraction) and 0.26% (volume fraction), respectively. Good linearity was observed in the alcohol content range of 0.5%-80% (volume fraction), with correlation coefficient R2 of the standard curve method, the external standard method, and the internal standard method being 0.996 1, 0.996 1, and 0.999 5, respectively. The precisions (relative standard deviation, RSD) of the three methods were less than 5%. The methods had good reproducibility and accurate results. The spiked recoveries of the standard curve method, the external standard method, and the internal standard method were 88.1%-97.81%, 84.61%-107.36%, and 81.83%-111.91%, respectively. It could be seen that the linearity, reproducibility and recovery of the methods met the requirements of accurate quantification. The errors between the methods of this study and the digital densimeter method of GB 5009.225—2016 were within ±5%, which met the requirements of feasibility comparative analysis and verification. Compared to the national standard method, the methods of this study had the advantages of simpler sample pretreatments, less sample usage (only 500 μL), and short test times (less than 5 min). Compared with the high-field NMR spectrum, the low-field NMR has the advantages of small volume, light weight and easy movement. It is suitable for the rapid and large-scale determination of alcohol content in alcoholic beverages.

Key words： low-field NMR; alcoholic beverages; alcohol content; rapid determination; quantification

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