超高效液相色谱-串联质谱测定预混合饲料中11种蛋白同化激素  

Determination of 11 anabolic steroids hormones in mixed feed additives by ultra performance liquid chromatography tandem-mass spectrometry

作　　者：王博 张婧 吴剑平 严凤 WANG BO;ZHANG Jing;WU Jian-ping;YAN Feng

机构地区：[1]上海市兽药饲料检测所,上海201103

出　　处：《饲料研究》2023年第14期119-124,共6页Feed Research

摘　　要：试验旨在建立预混合饲料中11种蛋白同化激素的超高效液相色谱-串联质谱测定方法。饲料样品经乙腈提取后,使用乙二胺-N-丙基硅烷(PSA)净化,以Phenomenex C18色谱柱(100 mm×2.1 mm,2.6μm)作为分析柱,乙腈和0.01%甲酸溶液作为流动相进行梯度洗脱。在电喷雾正电离模式下进行定性及内标法定量分析。结果显示,11种蛋白同化激素在1~100μg/L范围内线性关系良好,相关系数大于0.993 9。甲基睾酮、司坦唑醇和醋酸美伦孕酮的方法检出限为5μg/kg,定量限为10μg/kg,其余8种蛋白同化激素的方法检出限为20μg/kg,定量限为50μg/kg。11种蛋白同化激素的加标回收率为85.38%~115.72%,相对标准偏差(RSD)为0.5%~14.8%。研究表明,试验所用方法操作简单、灵敏度高且定量准确,适用于测定预混合饲料中11种蛋白同化激素含量,可为预混合饲料中的蛋白同化激素类药物非法添加监管提供一定参考。The study was to establish a method for the determination of 1l anabolic steroids hormones in premix feed by ultra performance liquid chromatography tandem-mass spectrometry.The feed samples were extracted with acetonitrile and cleaned using ethylenediamine-N-propylsilane(PSA).The target analytes were separated on Phenomex C18 chromatographic column(100 mm×2.1 mm,2.6μm),eluted with acetonitrile and 0.01%formic acid in acetonitrilein gradient.Qualitative analysis and quantitative analysis by internal standard method were carried out in electrospray positive ionization mode.The results showed that in the range of 1~100μg/L,1l target analytes exhibited good linearity with correlation coefficients above 0.9939.The detection limit of methyltestosterone,stanazol and melengestrol acetate was 5μg/kg,the quantitative limit was 10μg/kg,the detection limit of the other eight anabolic steroids hormones was 20μg/kg,the quantitative limit was 50μg/kg.The recoveries of 11 kinds of protein anabolic hormones were 85.38%~115.72%,RSD was 0.5%~14.8%.The study indicates that the established method has the advantages of simple operation,high sensitivity and accurate quantification,which is suitable for the detection of 1l anabolic steroids hormones in premix feed,and can provide reference for the supervision of illegal drug addition in premix feed.

关 键 词：超高效液相色谱-串联质谱 预混合饲料 蛋白同化激素 

分 类 号：S816.17[农业科学—饲料科学]