超高效液相色谱-串联质谱法测定牛乳中21种β-兴奋剂  

Quantitative Determination of 21 β-Agonists in Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张立佳 胡雪 莫楠 白艳梅 张悦 刘丽君 李翠枝 ZHANG Lijia;HU Xue;MO Nan;BAI Yanmei;ZHANG Yue;LIU Lijun;LI Cuizhi(Inner Mongolia Yili Industrial Group Co.Ltd.,Hohhot 010110,China)

机构地区：[1]内蒙古伊利实业集团股份有限公司,内蒙古呼和浩特010110

出　　处：《乳业科学与技术》2020年第3期17-22,共6页JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY

基　　金：“十三五”国家重点研发计划重点专项(2017YFE0110800,2018YFF0215206)。

摘　　要：建立超高效液相色谱-串联质谱法同时测定牛乳中21种β-兴奋剂残留量。样品经酶解、固相萃取柱净化,采用Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,以0.1%甲酸-10%甲醇水溶液为流动相梯度洗脱,在电喷雾离子源正离子模式下,采用多反应监测模式,对21种β-兴奋剂进行定性和定量分析。结果表明:该方法的定量限为0.05μg/kg,在0.05、0.10、0.50μg/kg 3个不同添加水平下,平均回收率为61.0%~124.3%,相对标准偏差为2.39%~10.66%;该方法稳定、准确、灵敏度高,可用于牛乳中21种β-兴奋剂残留量检测。An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous quantitative determination of 21 β-agonists in milk.The samples were hydrolyzed and cleaned up a solid-phase extraction column.The analytes were separated by UPLC with an Acquity UPLC BEH C18 column(50 mm×2.1 mm,1.7μm)using a gradient mobile phase consisting of 0.1%formic acid aqueous solution and methanol(10:90,V/V).Identification and quantification were achieved by UPLC-MS/MS with multiple reaction monitoring(MRM)under the positive ion mode The limit of quantitation of all β-agonists was 0.05μg/kg.The average recovery varied from 61.0%to 124.3%at spiked concentration levels of 0.05,0.10 and 0.50μg/kg with relative standard deviations(RSDs)of 2.39%–10.66%.Our results demonstrate that the method is stable,accurate and sensitive,and can be used for the determination of the 21β-agonists residues in milk.

关 键 词：超高效液相色谱-串联质谱 Β-兴奋剂 牛乳 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]