UPLC-MS/MS高通量测定鸡粪中81种抗菌药物残留方法的建立  

UPLC-MS/MS sample pretreatment methods for high-throughput determination of four groups of 81 antimicrobial residues in chicken manure

作　　者：刘田 赵芮敏 李木子 李泽慧 孙瑞 杨智和 孙晓亮[2] 赵思俊[2] 宋翠平[2] 霍乃蕊[1] LIU Tian;ZHAO Ruimin;LI Muzi;LI Zehui;SUN Rui;YANG Zhihe;SUN Xiaoliang;ZHAO Sijun;SONG Cuiping;HUO Nairui(College of Veterinary Medicine,Shanxi Agricultural University,Jinzhong 030031,China;Chinese Center for Animal Health and Epidemiology,Qingdao 266032,China;College of Veterinary Medicine,Beijing College of Agriculture,Beijing 102206,China;College of Veterinary Medicine,Tianjin Agricultural College,Tianjin 300384,China)

机构地区：[1]山西农业大学动物医学学院,山西晋中030031 [2]中国动物卫生与流行病学中心,山东青岛266032 [3]北京农学院动物医学学院,北京102206 [4]天津农学院动物医学学院,天津300384

出　　处：《农业环境科学学报》2025年第1期260-268,共9页Journal of Agro-Environment Science

基　　金：中国动物卫生与流行病学中心创新基金项目(2021221200)。

摘　　要：通过比较、优化样品前处理方法,建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)高通量、快速测定鸡粪中磺胺类、大环内酯类、喹诺酮类、四环素类等4类81种抗菌药物残留检测方法。样品经EDTA-Mcllvaine与10%乙腈/乙酸(5∶15,V/V)混合溶液提取,HLB固相萃取柱净化过柱后,在UPLC-MS/MS多反应监测模式下进行定性及定量分析。加标回收试验结果显示,鸡粪中81种药物在1.0~100.0μg·kg^(-1)范围内线性关系良好(R^(2)>0.99),检出限为1.0~2.5μg·kg^(-1),待测药物的回收率为60.24%~118.70%。该方法简单可靠,提取效果好,适用于鸡粪中多类抗菌药物残留的大批样品筛查和确证。An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the highthroughput and rapid determination of 81 antimicrobial drug residues in chicken manure of four classes,including sulfonamides,macrolides,quinolones and tetracyclines,by comparing and optimising sample pretreatment methods.The samples were extracted with a mixture of EDTA-Mcllvaine and 10% acetonitrile/acetic acid(5∶15 V/V),cleaned up and passed through the HLB solid phase extraction column,and then analyzed qualitatively and quantitatively in UPLC-MS/MS multiple reaction monitoring mode.The standard recovery test showed that the linear relationship of 81 drugs in chicken feces was good in the range of 1.0-100.0μg·kg^(-1)(R^(2)>0.99),the detection limit was 1.0-2.5μg·kg^(-1),and the recovery rate was 60.24%-118.70%.The method is simple and reliable,has good extraction effect,and is suitable for screening and confirming the residues of many kinds of antibiotics in chicken manure.

关 键 词：鸡粪 超高效液相色谱-串联质谱法 抗菌药物 残留 

分 类 号：O657.63[理学—分析化学] X839.2[理学—化学]