摘要
建立QuEChERS-超高效液相色谱串联质谱法(UPLC-MS/MS)快速测定婴幼儿奶粉中5种黄曲霉毒素的方法.样品采用QuEChERS法提取之后,使用分散式固相萃取管(EMR-Lipid dSPE)进行净化,选择ACQUITY BEN C18色谱柱(1.7μm,2.1 mm×100 mm)分离,多反应监测采集模式(MRM)进行定性和定量检测,外标法定量.结果显示,在优化的分析条件下,5种待测物在0~1.6 ng/mL线性关系良好,相关系数(r)在0.9964~0.9991范围内,检出限为0.04~0.20 ng/g,定量限为0.58~0.95 ng/g,低、中、高3个添加水平的回收率为81.9%~103.2%,相对标准偏差(RSD)为2.2%~4.5%.方法净化效果良好,具有前处理操作简便、快速、高效、准确等优点,可用于婴幼儿奶粉中黄曲霉毒素检测.
A QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)has been established for rapid determination of five aflatoxins in infant milk powder.After the sample was extracted by QuEChERS,and then purified by enhanced matrix removal lipid-dispersed solid phase extraction(EMR-Lipid dSPE).ACQUITY BEN C18 column(1.7μm,2.1 mm×100 mm)was selected for the separation.The qualitative and quantitative analyses were performed under the multiple reaction monitoring(MRM)acquisition mode,and an external standard method was used for the quantification.Under optimized analytical conditions,the analytes showed good linearities in concentration ranges of 0~1.6 ng/mL with their correlation coefficients(r)in ranges of 0.9964~0.9991.The limit of detection were 0.04~0.20 ng/g,the limit of quantitative were 0.58~0.95 ng/g,the spiked recoveries of low,medium and high for three concentration levels were 81.9%~103.2%,the relative standard deviations(RSD)of 2.2%~4.5%.The method has a good purification effect,and has the advantages of simple operation,accurate result,low detection limit and high sensitivity,which is suitable for the rapid detections of aflatoxin in infant milk powder.
作者
王小乔
许晓辉
张虹艳
冯翀
吴福祥
潘秀丽
李赟
李晨曦
WANG Xiao-qiao;XU Xiao-hui;ZHANG Hong-yan;FENG Chong;WU Fu-xiang;PAN Xiu-li;LI Yun;LI Chen-xi(Lanzhou Institute for Food and Drug Control,Lanzhou 730050,China;School of Life Science and Engineering,Lanzhou University of Technology,Lanzhou 730050,China)
出处
《分析测试技术与仪器》
CAS
2022年第1期96-102,共7页
Analysis and Testing Technology and Instruments
基金
甘肃省市场监督管理局技术计划项目(SSCJG-SP-202108)。