盐析辅助液液萃取-超高效液相色谱串联质谱法测定山羊角中53种禁用兽药残留  

Determination of 53 prohibited veterinary drug residues in goat horn by salting-out assisted liquid-liquid extraction combined with UHPLC-MS/MS

作　　者：劳柏豪 孙健 张静娴 于泓 冉莹瑛 黄帆 季申 胡青 LAO Bai-hao;SUN Jian;ZHANG Jing-xian;YU Hong;RAN Ying-ying;HUANG Fan;JI Shen;HU Qing(School of Pharmacy,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;National Medical Products Administration Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海中医药大学中药学院,上海201203 [2]上海市食品药品检验研究院,国家药品监督管理局中药质量控制重点实验室,上海201203

出　　处：《药学学报》2025年第3期791-800,共10页Acta Pharmaceutica Sinica

基　　金：上海市科委研发平台专项(21DZ2290200)。

摘　　要：建立了UHPLC-MS/MS测定山羊角中53种禁用兽药残留的检测方法,包括16种镇静剂类、14种β-受体激动剂类、氯霉素、4种氟喹诺酮类、7种硝基咪唑类、3种喹噁啉类化合物、8种其他类化合物。采用盐析辅助液液萃取样品,Zorbax Eclipse Plus C18色谱柱(1.8μm,3.0 mm×150 mm,Agilent),以0.1%甲酸溶液-乙腈为流动相,梯度洗脱,在电喷雾离子化正负离子模式下,以多反应监测方式(MRM)检测。53种待测物在各自浓度范围内均成良好线性关系,相关系数均在0.99以上;三水平平均加样回收率为70.4%~118.7%,相对标准偏差(RSD)为0.69%~12.07%,检出限为0.1~50μg·kg^(-1),定量限为0.2~100μg·kg^(-1)。本方法已应用于实际样品的测定。A detection method using UHPLC-MS/MS was established for the determination of 53 prohibited veterinary drug residues in goat horns,including 16 tranquilizers,14β-agonists,chloramphenicol,4 fluoroquinolones,7 nitroimidazoles,3 quinoxalines,and 8 other compounds.Samples were extracted using salting-out assisted liquidliquid extraction(SALLE).A Zorbax Eclipse Plus C18 column(1.8μm,3.0 mm×150 mm,Agilent)was used with 0.1%formic acid solution-acetonitrile as the mobile phase for gradient elution.Detection was performed in positive and negative electrospray ionization modes using multiple reaction monitoring(MRM).All 53 analytes showed good linearity within their respective concentration ranges,with correlation coefficients above 0.99.The average recoveries at three spiked levels ranged from 70.4%to 118.7%,with relative standard deviations(RSDs)ranging from 0.69%to 12.07%.The limits of detection(LODs)ranged from 0.1 to 50μg·kg^(-1),and the limits of quantitation(LOQs)ranged from 0.2 to 100μg·kg^(-1).This method has been applied to the determination of real samples.

关 键 词：山羊角 禁用兽药残留 盐析辅助液液萃取 超高效液相色谱串联三重四极杆质谱 

分 类 号：R917[医药卫生—药物分析学]