食品与发酵工业 >

2023 , Vol. 49 >Issue 1: 273 - 278

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.030317

分析与检测

稳定同位素内标的液相色谱串联质谱法测定乳制品中唾液酸的含量

  • 何姝 ,
  • 曹晶
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  • (上海师范大学 化学与材料科学学院,上海,200234)
第一作者：硕士研究生(曹晶副研究员为通信作者,E-mail:caojing@shnu.edu.cn)

收稿日期: 2021-12-06

  修回日期: 2022-01-07

  网络出版日期: 2023-02-14

基金资助

上海市科委科技创新行动计划项目(20 JC1416800)

收起

Determination of sialic acid in dairy products by liquid chromatography-tandem mass spectrometry with stable isotope internal standard

  • HE Shu ,
  • CAO Jing
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  • (College of Chemistry and Material Science, Shanghai Normal University, Shanghai 200234, China)

Received date: 2021-12-06

  Revised date: 2022-01-07

  Online published: 2023-02-14

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摘要

该研究建立了基于稳定同位素内标液相色谱串联质谱法测定乳制品中唾液酸含量的分析方法。首次引入稳定同位素内标来定量乳制品中的唾液酸,采用电喷雾离子源,在负离子、多反应监测模式下进行定量分析。研究自样品前处理至质谱鉴定,均进行了方法比较优化,并测试了婴幼儿奶粉、酸奶等6种乳制品中的唾液酸含量。结果表明,唾液酸在0.012 5~5 μg/mL线性关系良好,相关系数为0.999 9,加标样品的回收率为76.5%~96.4%,相对标准偏差(n=6)为0.6%~6.35%,检出限和定量限分别为0.4、1.6 ng/mL。该方法样品前处理简单,检测结果准确,可定量不同乳制品中唾液酸的含量。

关键词： 唾液酸; 液相色谱串联质谱; 稳定同位素内标; 乳制品

本文引用格式

何姝 , 曹晶 . 稳定同位素内标的液相色谱串联质谱法测定乳制品中唾液酸的含量[J]. 食品与发酵工业, 2023 , 49(1) : 273 -278 . DOI: 10.13995/j.cnki.11-1802/ts.030317

Abstract

A quantitative method with stable isotope internal standard (SIIS) for the determination of N-acetylneuraminic acid (Neu5Ac) in dairy products by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established. In this research, for the first time, SIIS coupled with LC-MS/MS to quantify Neu5Ac was employed. LC-MS/MS was done in negative ion and multi-reaction monitoring mode. This study also optimized experimental conditions including sample preparation and LC-MS conditions. Totally 6 kinds of dairy products were detected by this method. Results showed that the linear range of sialic acid was 0.0125-5 μg/mL and the correlation coefficient was 0.999 9. The recoveries of the spiked samples were between 76.5% and 96.4%, and the relative standard deviations (n=6) were between 0.6% and 6.35%. The limit of detection and limit of quantification were 0.4 ng/mL and 1.6 ng/mL, respectively. The quantitative results of the SIIS method were accurate and reliable. Thus, the method explored here can be used for the determination of sialic acid in different dairy products.

Key words： sialic acid; LC-MS/MS; stable isotope internal standard; dairy products

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