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

作　　者：程晓帆 李芸[1] 陈玉浩 林爽 周启裕 CHENG Xiaofan;LI Yun;CHEN Yuhao;LIN Shuang;ZHOU Qiyu(Shenzhen Academy of Metrology and Quality Inspection,Shenzhen 518000,China)

机构地区：[1]深圳市计量质量检测研究院,广东深圳518000

出　　处：《现代食品》2024年第17期167-171,共5页Modern Food

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0.9990),硫脲、曲酸、次磷酸盐的检出限为25μg·kg^(-1),定量限为50μg·kg^(-1),三聚硫氰酸三钠盐、苯甲羟肟酸的检出限为5μg·kg^(-1),定量限为10μg·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。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 0.9990)in their respective linear ranges.The limits of detection and limits of quantitation of thiourea,kojic acid,and hypophosphite were 25μg·kg^(-1) and 50μg·kg^(-1) respectively.The limits of detection and limits of quantitation of trisodium thiocyanate and benzohydroxamic acid were 5μg·kg^(-1) and 10μg·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 

分 类 号：TS207.3[轻工技术与工程—食品科学]