现代食品2024,Vol.30Issue(17) :167-171.DOI:10.16736/j.cnki.cn41-1434/ts.2024.17.041

液质联用法测定小麦粉中5种非法添加物

Determination of Five Illegal Additives in Wheat Flour by Liquid Chromatography-Tandem Mass Spectrometry

程晓帆 李芸 陈玉浩 林爽 周启裕
现代食品2024,Vol.30Issue(17) :167-171.DOI:10.16736/j.cnki.cn41-1434/ts.2024.17.041

液质联用法测定小麦粉中5种非法添加物

Determination of Five Illegal Additives in Wheat Flour by Liquid Chromatography-Tandem Mass Spectrometry

程晓帆 1李芸 1陈玉浩 1林爽 1周启裕1
扫码查看

作者信息

  • 1. 深圳市计量质量检测研究院,广东 深圳 518000
  • 折叠

摘要

建立了液相色谱-串联质谱法快速测定小麦粉中 5 种非法添加物的分析方法.样品使用一级水直接提取,采用Agilent Eclipse Plus C18 色谱柱,以 0.1%甲酸+10 mmol·L-1 甲酸胺溶液和甲醇为流动相,梯度洗脱,采用电喷雾离子源的正负离子扫描模式对小麦粉中 5 种非法添加物进行定性定量检测.结果表明,5 种化合物在各自线性范围内具有良好的线性(r均大于 0.999 0),硫脲、曲酸、次磷酸盐的检出限为 25 μg·kg-1,定量限为50 μg·kg-1,三聚硫氰酸三钠盐、苯甲羟肟酸的检出限为5 μg·kg-1,定量限为10 μg·kg-1,在低、中、高3个加标水平下,其回收率为 82.1%~101.0%,RSD为 0.8%~5.8%(n=6).该方法专属性好,灵敏度高,前处理简单快速,可用于小麦粉中硫脲、曲酸、次磷酸盐、苯甲羟肟酸、三聚硫氰酸三钠盐的快速筛查和定量测定.

Abstract

A liquid chromatography-tandem mass spectrometry analytical method was established for the rapid determination of five kinds of illegal additives in wheat flour.The samples were extracted with primary water on an Agilent Eclipse Plus C18 column with 0.1%formic acid+10 mmol·L-1 formic acid amine solution and methanol as the mobile phase by gradient elution.The five illegal additives were qualitatively and quantitatively detected by electrospray ionization in positive and negative ion scanning mode.The results of the five compounds showed good linear relationship(r was greater than 0.999 0)in their respective linear ranges.The limits of detection and limits of quantitation of thiourea,kojic acid,and hypophosphite were 25 μg·kg-1 and 50 μg·kg-1 respectively.The limits of detection and limits of quantitation of trisodium thiocyanate and benzohydroxamic acid were 5 μg·kg-1 and 10 μg·kg-1 respectively.Average recoveries of three spiked levels were in the range from 82.1%to 101.0%,and the RSD were between 0.8%and 5.8%(n=6).This method has good specificity,high sensitivity,simple and fast pre-treatment,and can be used for rapid screening and quantitative determination of thiourea,kojic acid,hypophosphite,benzohydroxamic acid,and trisodium thiocyanate in wheat flour.

关键词

小麦粉/非法添加物/次磷酸盐

Key words

wheat flour/illegal additives/hypophosphite

引用本文复制引用

出版年

2024
现代食品
国家粮食储备局郑州科学研究设计院

现代食品

影响因子:0.169
ISSN:2096-5060
段落导航相关论文