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

  • WANG Shoufeng ,
  • LAN Xi ,
  • YONG Dengjin ,
  • YANG Huini ,
  • HU Min
Expand
  • 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

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.

Cite this article

WANG Shoufeng , LAN Xi , YONG Dengjin , YANG Huini , HU Min . Quantitative analysis of acid ester content in Baijiu based on nuclear magnetic resonance spectroscopy[J]. Food and Fermentation Industries, 2025 , 51(6) : 306 -310 . DOI: 10.13995/j.cnki.11-1802/ts.040181

References

[1] 任金玫, 陈君平, 李志健, 等.十二种香型白酒相关研究概况[J].中国酿造, 2022, 41(4):13-19.
REN J M, CHEN J P, LI Z J, et al.Research overview of twelve flavor types Baijiu[J].China Brewing, 2022, 41(4):13-19.
[2] 王玉荣, 田龙新, 张振东, 等. 基于智能感官和气相色谱-离子迁移谱分析贮藏年限对酱香型白酒的影响[J]. 食品与发酵工业, 2024, 50(14): 305-313.
WANG Y R, TIAN L X, ZHANG Z D, et al. Analysis of the influence of storage years on Maotai-flavor liquor based on intelligent senses and GC-IMS[J]. Food and Fermentation Industries, 2024, 50(14): 305-313.
[3] HONG J X, ZHAO D R, SUN B G.Research progress on the profile of trace components in Baijiu[J].Food Reviews International, 2023, 39(3):1666-1693.
[4] 王震, 叶宏, 朱婷婷, 等.清香型白酒风味成分的研究进展[J].食品科学, 2022, 43(7):232-244.
WANG Z, YE H, ZHU T T, et al.Progress in research on the flavor components of light-flavor Baijiu[J].Food Science, 2022, 43(7):232-244.
[5] 韩冰玙, 陈辉太, 李宗军.酱、浓、清香型白酒酿造过程中真菌及其功能特性研究进展[J].中国酿造, 2024, 43(3):27-32.
HAN B Y, CHEN H T, LI Z J.Research progress of fungi and their functional properties in the brewing process of sauce-, strong- and light-flavor Baijiu[J].China Brewing, 2024, 43(3):27-32.
[6] YAN Q, ZHANG K Z, ZOU W, et al.Three main flavour types of Chinese Baijiu:Characteristics, research, and perspectives[J].Journal of the Institute of Brewing, 2021, 127(4):317-326.
[7] XU Y Q, ZHAO J R, LIU X, et al.Flavor mystery of Chinese traditional fermented Baijiu:The great contribution of ester compounds[J].Food Chemistry, 2022, 369:130920.
[8] 胡景辉, 陈禹锜, 薛新新, 等.浓香型白酒发展概述[J].中国酿造, 2022, 41(6):24-30.
HU J H, CHEN Y Q, XUE X X, et al.Overview of development of strong-flavor Baijiu[J].China Brewing, 2022, 41(6):24-30.
[9] JIA W, FAN Z B, DU A, et al.Recent advances in Baijiu analysis by chromatography based technology-A review[J].Food Chemistry, 2020, 324:126899.
[10] WANG J S, CHEN H, WU Y S, et al.Uncover the flavor code of strong-aroma Baijiu:Research progress on the revelation of aroma compounds in strong-aroma Baijiu by means of modern separation technology and molecular sensory evaluation[J].Journal of Food Composition and Analysis, 2022, 109:104499.
[11] 朱开宪, 胡雪, 邓静, 等.基于GC-MS技术对不同香型白酒的判别分析[J].中国酿造, 2023, 42(1):213-218.
ZHU K X, HU X, DENG J, et al.Discriminant analysis of different flavor-type Baijiu based on GC-MS[J].China Brewing, 2023, 42(1):213-218.
[12] 熊秋萍, 谢小兰, 彭思妮, 等.白酒检测中色谱法替代常规理化法检测总酸总酯的研究[J].酿酒科技, 2016(7):124-127.
XIONG Q P, XIE X L, PENG S N, et al.Detection of total acids & total esters in Baijiu by chromatographic method instead of conventional physiochemical method[J].Liquor-Making Science & Technology, 2016(7):124-127.
[13] 黄清霞, 付国勇, 陈黎萍.成品白酒中酸酯总量的近红外检测[J].食品工业科技, 2022, 43(5):310-314.
HUANG Q X, FU G Y, CHEN L P.Detection of acid ester content in Baijiu (Chinese liquor) based on near infrared spectroscopy[J].Science and Technology of Food Industry, 2022, 43(5):310-314.
[14] 唐云容, 庞臻, 钟敏, 等.中红外光谱分析技术结合化学计量学方法快速分析酱香型白酒酸酯含量[J].中国酿造, 2024, 43(1):244-249.
TANG Y R, PANG Z, ZHONG M, et al.Rapid analysis of acid and ester content in sauce-flavor Baijiu by mid-infrared spectroscopy combined with chemometrics method[J].China Brewing, 2024, 43(1):244-249.
[15] 张瑞景, 王浩, 蔡凤娇, 等.高效液相色谱法检测白酒中四种有机酸的方法研究[J].中国酿造, 2022, 41(3):238-242.
ZHANG R J, WANG H, CAI F J, et al.Determination of four organic acids in Baijiu by HPLC[J].China Brewing, 2022, 41(3):238-242.
[16] FLÜGGE F, KERKOW T, KOWALSKI P, et al.Qualitative and quantitative food authentication of oregano using NGS and NMR with chemometrics[J].Food Control, 2023, 145:109497.
[17] BERTARELLO A, BERRUYER P, ARTELSMAIR M, et al.In-cell quantification of drugs by magic-angle spinning dynamic nuclear polarization NMR[J].Journal of the American Chemical Society, 2022, 144(15):6 734-6 741.
[18] CHEN H H, DING Z N, DAI T, et al.Quantitative comparison and rapid discrimination of Panax notoginseng powder and Caulis Clematidis armandii using NMR combined with pattern recognition[J].Journal of the Science of Food and Agriculture, 2023, 103(8):3 766-3 775.
[19] 刘恩满, 李雪玉, 宗绪岩, 等.基于核磁共振氢谱技术建立白酒乙醇浓度检测方法[J].食品与发酵工业, 2021, 47(12):231-235.
LIU E M, LI X Y, ZONG X Y, et al.Detection of alcohol content in Chinese Baijiu based on 1H nuclear magnetic resonance spectrum[J].Food and Fermentation Industries, 2021, 47(12):231-235.
[20] 王寿峰, 丁秀国, 林嘉荣, 等.白酒中乙醛和糠醛的吸附效果对比[J].食品科学, 2024,45(14):189-197.
WANG S F, DING X G, LIN J R, et al.Comparison of adsorption characteristics of different sorbents for acetaldehyde and furfural in Baijiu[J].Food Science, 2024,45(14):189-197.
[21] 冯艳春, 裴文莉, 王晨, 等.高效液相色谱法测定β-内酰胺抗生素中残留乙酸的含量[J].中国抗生素杂志, 2024, 49(4):388-393.
FENG Y C, PEI W L, WANG C, et al.Determination of residual acetic acid in the raw materials of β-lactam antibiotics using high performance liquid chromatography[J].Chinese Journal of Antibiotics, 2024, 49(4):388-393.
Outlines

/