高分辨质谱筛查复合预混合饲料中 非法添加药物  

Screening of illegal additives in compound premix feed by high resolution mass spectrometry

作　　者：霍宁宁 李研东 霍惠玲 韩雪[1] 苗玉涛 HUO Ningning;LI Yandong;HUO Huiling;HAN Xue;MIAO Yutao(College of Food and Biology,Hebei University of Science and Technology,Shijiazhuang,Hebei Province 050018,China;Hebei Provincial Station of Veterinary Drug and Feed,Shijiazhuang,Hebei Province 050035,China)

机构地区：[1]河北科技大学食品与生物学院,河北石家庄050018 [2]河北省兽药饲料工作总站,河北石家庄050035

出　　处：《中国饲料》2023年第1期105-113,共9页China Feed

基　　金：河北省农业高质量发展关键共性技术攻关专项(20327502D);河北省生猪产业创新团队专项。

摘　　要：本实验旨在建立复合预混合饲料中超高效液相色谱-四极杆静电场轨道阱质谱(HPLC-Q-Exactive Focus/MS)测定157种非法添加药物的高通量筛查方法。通过构建非法添加药物筛查数据库并与样品中未知物信息进行比对,从而快速确定未知药物种类和含量。数据库包括磺胺类、喹诺酮类、β-受体激动剂类、硝基咪唑类、苯并咪唑类、蛋白同化激素类、糖皮质激素类、喹噁啉类、四环素类、抗病毒类、氯霉素类和真菌毒素类等12类157种药物的液相色谱条件及相关筛查参数。饲料样品使用50%乙腈水溶液超声提取,净化后过膜上机,正负模式扫描,TraceFinder软件进行定性筛查。结果表明:该方法可适用于复合预混合饲料中多种兽药非法添加的快速筛查,当药物添加浓度为50 ng/g时药物检出率为98.7%,药物添加浓度为100 ng/g时药物检出率100%。该方法可基本满足预混合饲料中非法添加药物的高通量快速检测需求,为实现多种药物高通量筛查提供数据支撑。A high-throughput screening method for the determination of 157 illegally added drugs in compound premix feed by ultra performance liquid chromatography-quadrupole electrostatic field orbitrap mass spectrometry(HPLC-Q-Exactive Focus/MS)was established.By building a database of illegal drug addition screening and comparing with the unknown information in the sample,the type and content of unknown drugs was quickly determined.The database included sulfonamides,quinolones,β-agonists,nitroimidazoles,benzimi-dazoles,protein assimilation hormones,glucocorticoids,quinolines,tetracyclines,antivirals,chloramphenicols and mycotoxins.The liquid chromatography conditions and related screening parameters of 157 common illegally added drugs in 12 categories were included.Feed samples were ultrasonically extracted with 50%acetonitrile aqueous solution.After purification,positive and negative mode scanning was performed,and TraceFinder software was used for qualitative screening.The results showed that this method could be applied to the rapid screening of illegal addition of multiple veterinary drugs in compound premix feed.When the drug concentration was higher than 50 ng/g,the drug detection rate was 98.7%,and when the drug concentration was higher than 100 ng/g,the drug detection rate was 100%.This method could basically meet the needs of high-throughput rapid detection of illegal addition of drugs in premix feed,and provide data support for further realization of high-throughput screening methods for more drugs.

关 键 词：复合预混合饲料 非法添加 筛查 高分辨质谱 

分 类 号：S816.17[农业科学—饲料科学]