食品与发酵工业 >

2022 , Vol. 48 >Issue 10: 226 - 233

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.028425

分析与检测

核磁共振氢谱法测定果汁中主要糖类的含量

  • 冯翠萍 ,
  • 刘一诺 ,
  • 许紫薇 ,
  • 樊双喜 ,
  • 岳红卫 ,
  • 辛刚 ,
  • 姜楠 ,
  • 钟其顶
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  • 1(中轻食品检验认证有限公司,北京,100015)
    2(北京林业大学 生物科学与技术学院,北京,100091)
    3(国投中鲁果汁股份有限公司,北京,100070)
    4(国投中鲁果汁股份有限公司乳山研发中心,山东 威海,264513)
    5(国家食品质量检验检测中心,北京,100015)
第一作者:硕士,工程师(钟其顶教授级高级工程师为通信作者,Email:zhongqiding@163.com)

收稿日期: 2021-06-23

  修回日期: 2021-09-14

  网络出版日期: 2022-06-10

基金资助

科技部国家重点研发计划(2017YFE0110800);科技部“十三五”重大科技计划(2016YFF0203903);欧盟地平线2020计划(635690-OLEUM;727864-EU-China-Safe)

收起

Determination of glucose, fructose and sucrose in fruit juice by 1H-NMR

  • FENG Cuiping ,
  • LIU Yinuo ,
  • XU Ziwei ,
  • FAN Shuangxi ,
  • YUE Hongwei ,
  • XIN Gang ,
  • JIANG Nan ,
  • ZHONG Qiding
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  • 1(Sinolight Food Inspection and Certification Co.Ltd., Beijing 100015, China)
    2(College of Biological Sciences and Biotechnology, Beijing Forestry University, Beijing 100091, China)
    3(SDIC Zhonglu Fruit Juice Co.Ltd., Beijing 100070, China)
    4(Rushan R & D Center of SDIC Zhonglu Fruit Juice Co.Ltd., Weihai 264513, China)
    5(National Food Quality Inspection and Testing Center, Beijing 100015, China)

Received date: 2021-06-23

  Revised date: 2021-09-14

  Online published: 2022-06-10

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摘要

该研究以邻苯二甲酸氢钾和柠檬酸分别作为定量内标和外标,结合水峰压制技术,建立了核磁共振氢谱法快速、同步、准确定量果汁中葡萄糖、果糖和蔗糖的含量。该方法果糖的检出限为0.005 g/L,定量限为0.018 g/L;葡萄糖的检测限为0.006 g/L,定量限为0.021 g/L;蔗糖的检出限为0.009 g/L,定量限制为0.030 g/L。葡萄糖、果糖、蔗糖在0.025~6.40 g/L线性关系良好(R2>0.999);外标法加标回收率为100.9%~104.7%,内标法加标回收率为102.1%~108.6%,测量精密度相对标准偏差<1%;测定方法重复性好。与GB 5009.8—2016《食品安全国家标准 食品中果糖、葡萄糖、蔗糖、麦芽糖、乳糖的测定》高效液相色谱法测定结果误差在±5%以内,满足方法的可行性验证要求。相比于国标方法该方法样品前处理简单,在测定结果准确的基础上,极大地节约了时间与人力,可实现果汁中葡萄糖、果糖和蔗糖同时定性定量检测,可广泛应用于果汁质量控制,同时为建立果汁核磁共振指纹图谱真实性鉴别技术奠定了良好基础。

关键词： 果汁; 葡萄糖; 果糖; 蔗糖; 核磁共振氢谱; 定量

本文引用格式

冯翠萍 , 刘一诺 , 许紫薇 , 樊双喜 , 岳红卫 , 辛刚 , 姜楠 , 钟其顶 . 核磁共振氢谱法测定果汁中主要糖类的含量[J]. 食品与发酵工业, 2022 , 48(10) : 226 -233 . DOI: 10.13995/j.cnki.11-1802/ts.028425

Abstract

In this study, potassium hydrogen phthalate and citric acid were used respectively as the internal and external standards for the quantitative determination of glucose, fructose and sucrose in juice by water signal suppressing 1H NMR. The results showed that the limit of detection and quantification of fructose were 0.005 g/L and 0.018 g/L, respectively. The limit of detection and quantification of glucose were 0.006 g/L and 0.021 g/L, respectively. Moreover, the limit of detection and quantification of sucrose were 0.009 g/L and 0.030 g/L, respectively. Good linearity was observed in the range of 0.025-6.40 g/L, with correlation coefficient R2 greater than 0.999. The spiked recoveries of the external standard method were 100.9%-104.7% and the spiked recoveries of internal standard method were 102.1%-108.6%. Besides, the precisions (relative standard deviation, RSD) were less than 1%; The method had good reproducibility and accurate results. The error between NMR and HPLC of GB 5009.8—2016 was within ±5%, which met the requirements of feasibility comparative analysis and validation. Compared with the HPLC method, the method developed here was simple and accuracy. It could save time and labor greatly, and could be used to measure glucose, fructose and sucrose content simultaneously without separation. It can also be widely used in juice quality control and laid a good foundation for the establishment of NMR fingerprint authenticity identification technology of juice.

Key words： juice; glucose; fructose; sucrose; 1H NMR; quantitation

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