摘要
目的建立QuEChERS结合超高效液相色谱-串联质谱法(QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry,QuEChERS-UPLC-MS/MS)快速测定豆制品中二甲基黄和碱性嫩黄O的含量。方法豆制品经20 m L乙腈-水(1:1,V:V)浸泡,采用QuEChERS方法进行萃取、净化,经Shim-pack XR-ODSⅢ色谱柱分离,正离子扫描,多反应监测模式进行质谱分析,外标法定量。结果二甲基黄在添加水平为0.5、1和10μg/kg时,方法回收率为81.6%~97.2%;碱性嫩黄O在添加水平为6、10和50μg/kg时,方法回收率为89.1%~100.7%;二甲基黄和碱性嫩黄O的相对标准偏差均小于12%(n=6);二甲基黄和碱性嫩黄O的检出限分别为0.5、2μg/kg;定量限分别为1.5、6μg/kg。结论该方法操作简便、快速准确,适用于豆制品中二甲基黄、碱性嫩黄O的快速筛查和定量分析。
Objective To establish a method for simultaneous determination of dimethyl yellow and auramine O in bean products by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (QuEChERS- UPLC-MS/MS).Methods The bean products were soaked by 20 mL acetonitrile–water (1:1,V:V), extracted and purified by QuEChERS method, separated by Shim-pack XR-ODSⅢ column, and then determined by mass spectrometry with positive electrospray ionization and multiple reaction monitoring (MRM) mode. External standard method was used for quantification.Results The recoveries of dimethyl yellow were 81.6%~97.2% when spiked at 0.5, 1 and 10μg/kg, and the recoveries of auramine O were 89.1%~100.7% when spiked at 6, 10 and 50μg/kg. The relative standard deviations of the method were less than 12% (n=6). The limits of detection of dimethyl yellow and auramine O were 0.5 and 2μg/kg, respectively. The limits of quantitation were 1.5 and 6μg/kg, respectively. Conclusion This method is simple, accurate, and sensitive, which can be used for rapid screening and quantitative analysis of dimethyl yellow and auramine O in bean products.
出处
《食品安全质量检测学报》
CAS
2016年第12期4753-4758,共6页
Journal of Food Safety and Quality
基金
国家质检总局项目(2013QK284)~~
作者简介
李锦清,硕士,工程师,主要研究方向为食品检测与研发。E-mail:460661142@qq.com
通讯作者:陈满英,博士,高级工程师,主要研究方向为环境检测、食品化工检测。E-mail:103427809@qq.com