液质联用检测老酸奶和牛轧糖中三聚氰胺的研究  

Determination of Melamine in Old Yogurt and Nougat by LC-MS/MS

作　　者：刘超 吕雪梅 景赞 LIU Chao;LU Xuemei;JING Zan(Leshan Institute for Food and Drug Control,Leshan 614000)

机构地区：[1]乐山市食品药品检验检测中心,乐山614000

出　　处：《食品工业》2023年第9期278-281,共4页The Food Industry

基　　金：乐山市科技局重点研究项目(基金编号:22SZD007)。

摘　　要：检测老酸奶、牛轧糖样品中三聚氰胺含量,消除其中的基质效应以提高准确度。通过GB/T 22388—2008《原料乳与乳制品中三聚氰胺检测方法》第二法液相色谱-质谱/质谱法(LC-MS/MS法)对老酸奶和牛轧糖进行样品前处理过程。对液质联用技术检测过程所产生的基质效应进行评价,并采用外标法和内标法消除基质效应。结果表明:试验测得基质效应小于50%,基质效应的干扰强烈;外标法测得的平均加标回收率小于90%;内标法方法学验证结果表明,在质量浓度为1~20 ng/mL呈线性相关, r=0.999 5;在加标浓度2、5和10μg/kg水平下,加标回收率分别为老酸奶100.7%~102.4%、牛轧糖102.6%~104.5%;方法精密度分别为老酸奶1.7%~2.9%、牛轧糖0.3%~2.6%。内标法消除液质联用产生的基质效应的效果比外标法的更好。Detect the content of melamine in old yogurt and nougat,and eliminate the matrix effect to improve the accuracy.The second method of GB/T 22388—2008 Determination of Melamine Inold Yogurt and Nougat was used for sample pretreatment of old yogurt and nougat.The matrix effect produced in the detection process of LC-MS/MS was evaluated,and the external standard method and internal standard method were used to eliminate the matrix effect.The results showed that the experimental results show that matrix effect was less than 50%,and the interference of matrix effect was strong.The average recovery rate of external standard method was less than 90%.The results of methodological verification by internal standard method showed that there was a linear correlation at the concentration of 1-20 ng/mL with r-0.9995;At the spiked concentrations of 2,5 and 10μg/kg,the recoveries were 100.7%-102.4%for old yogurt and 102.6%-104.5%for nougat,respectively.The precisions of the method were 1.7%-2.9%for old yogurt and 0.3%-2.6%for nougat.The internal standard method was better than the external standard method in eliminating the matrix effect caused by LC-MS/MS.The internal standard method had a better effect of eliminating matrix effect,and the method was reliable,with high accuracy and reproducibility.

关 键 词：液相色谱-质谱质谱法(LC-MS/MS) 三聚氰胺 老酸奶 牛轧糖 基质效应 

分 类 号：O657.63[理学—分析化学] TS252.54[理学—化学] TS247[轻工技术与工程—农产品加工及贮藏工程]