超高效液相色谱-串联质谱法测定饲料中9种氨基糖苷类抗生素  

Determination of 9 kinds of aminoglycosides in feed by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：肖志明[1] 王钦钦 尤艳莉[2] 李彦伸[2] 杨建中 贾铮[1] 王石[1] 樊霞[1] XIAO Zhi-Ming;WANG Qin-Qin;YOU Yan-Li;LI Yan-Shen;YANG Jian-Zhong;JIA Zheng;WANG Shi;FAN Xia(Institute of Quality Standard and Testing Technology for Agro-products,Chinese Academy of Agricultural Sciences,Beijing 100081,China;College of Life Science,Yantai University,Yantai 264005,China;SGS-CSTC Standards Technical Services Co.,Ltd.,Qingdao Branch,Qingdao 266101,China;Veterinary Medicine and Feed Supervision Institute of Xinjiang Uygur Autonomous Region,Urumqi 830063,China)

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,北京100081 [2]烟台大学生命科学学院,烟台264005 [3]通标标准技术服务(青岛)有限公司,青岛266101 [4]新疆维吾尔自治区兽药饲料监察所,乌鲁木齐830063

出　　处：《食品安全质量检测学报》2021年第19期7563-7571,共9页Journal of Food Safety and Quality

基　　金：“十三五”国家重点研发计划项目(2019YFE0103800);中国农业科学院创新工程项目。

摘　　要：目的建立超高效液相色谱-串联质谱法测定饲料中9种氨基糖苷类抗生素(aminoglycosides,AGs)的分析方法。方法样品采用10 mmol/L磷酸二氢钾缓冲液作为提取液,酶探针超声提取1min,通过阳离子交换固相萃取柱净化,在电喷雾电离正离子模式下使用超高效液相色谱-串联质谱仪进行检测,外标法定量。结果经方法学验证,在5-1000 μg/L范围内,9种AGs均呈现良好的线性关系,方法的检出限为5-20 μg/kg,定量限为20-80 μg/kg。在20-400 μg/kg添加浓度范围内,饲料中9种AGs的平均回收率为76.2%-113.2%;日内变异系数为1.1%-8.4%,日间变异系数为1.1%-11.6%。结论该方法稳定、灵敏,可同时实现饲料中9种AGs的检测,满足饲料中AGs日常监测应用需求。Objective To establish an analytical method for the determination of 9 kinds of aminoglycosides(AGs) in feed by ultra performance liquid chromatography-tandem mass spectrometry.Methods The samples were extracted with 10 mmol/L potassium phosphate buffer solution using enzyme probe ultrasound for 1 min,and purified by cation exchange solid phase extraction column.The samples were detected by ultra performance liquid chromatography-tandem mass spectrometry in electrospray ionization positive ion mode,and quantified by external standard method.Results Verified by square law,the linear relationships of the 9 kinds of AGs were good in the range of 5-1000 μg/L,with the detection limits of 5-20 μg/kg and the quantitation limits of 20-80 μg/kg.The average recoveries of 9 kinds of AGs in feed ranged from 76.2% to 113.2% at the concentration of 20-400 μg/kg;the intra-day coefficients of variation were 1.1%-8.4%,and the intra-day coefficients of variation were 1.1%-11.6%.Conclusion This method is stable and sensitive,and can simultaneously detect 9 kinds of AGs in feed,thus meeting the daily monitoring application requirements of AGs in feed.

关 键 词：饲料 氨基糖苷类抗生素 超高效液相色谱-串联质谱法 

分 类 号：S816.17[农业科学—饲料科学] O657.63[农业科学—畜牧学]