超高效液相色谱-静电场轨道离子阱高分辨质谱联用筛查分析饲料中抗菌类药物  

Screening analysis of antibiotics drugs in animal feed using UPLC-Orbitrap HRMS

作　　者：王国庆[1] 刘云[1] 柯玮[2] 孙雨安[1] 李振兴[1] 

机构地区：[1]郑州轻工业学院材料与化学工程学院,河南郑州450001 [2]国家烟草质量监督检验中心,河南郑州450000

出　　处：《轻工学报》2016年第4期15-22,共8页Journal of Light Industry

基　　金：国家自然科学基金项目(21171150);国家质量监督检验检疫总局科技计划项目(2015IK114)

摘　　要：将73种抗菌药物标准品混合物经超高效液相色谱－静电场轨道离子阱高分辨质谱（UPLC-Orbitrap HRMS）分离和离子化，确定抗菌药物的离子化模式，建立抗菌药物实测精确分子量和保留时间标准数据库．饲料样品匀质后采用50％（v／v）乙腈水溶液一次提取和乙腈二次提取，经氨基固相萃取小柱净化，氮气吹干浓缩、过滤等处理后进行检测．结果表明，本法在测定饲料中抗菌药物时，回收率34．51％～129．64％，相对标准偏差0．1％～24．4％；在添加量为5μg·g －1时，均可检出．73 kinds of mixed antibacterial drug standards were separated and ionized by ultra high performance liquid chromatography-Orbtrap high resolution mass spectrometry （UPLC-Orbitrap HRMS）,the retention times and ionization mode of the the antimicrobial drugs were determined,and the antimicrobial drug accurate meas-urement of molecular weight and the retention time of the standard database were established.Feed samples were homogenized,first extracted with acetonitrile water solution 50% （v/v）,second extracted with acetoni-trile,purified by amino solid phase extraction cartridge,dried with nitrogen concentration and filtered for detection.The results showed that the recovery rate of this method was 34.51 % ~1 29.64%,the relative standard deviation was 0.1 % ~24.4%,and add amount of 5 μg·g -1 could be detected.

关 键 词：超高效液相色谱 静电场轨道离子阱高分辨质谱 饲料 抗菌药物 

分 类 号：TS201.6[轻工技术与工程—食品科学]