超高效液相色谱 串联质谱法同时测定畜禽排泄物中15种喹诺酮类药物  

Simultaneous determination of 15 quinolones in livestock and poultry excrement by UPLC-MS/MS

作　　者：裘丞军 侯轩 陈凯 吴望君 周炜 段友刚 QIU Chengjun;HOU Xuan;CHEN Kai;WU Wangjun;ZHOU Wei;DUAN Yougang(Zhejiang Center of Animal Disease Control,Hangzhou 311199,China;Kaihua County Center of Agricultural Affairs Management,Kaihua 324300,Zhejiang,China)

机构地区：[1]浙江省动物疫病预防控制中心,浙江杭州311199 [2]开化县农业事务管理中心,浙江开化324300

出　　处：《浙江农业学报》2024年第7期1519-1529,共11页Acta Agriculturae Zhejiangensis

基　　金：浙江省重点研发计划项目(2020C02032);浙江省农业重大技术协同推广计划(2021XTTGXM03)。

摘　　要：建立了应用超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定畜禽排泄物中15种喹诺酮类药物残留量的分析方法。样品经冷冻干燥后粉碎过筛,N,N-二甲基甲酰胺(DMF)和0.1 mol·L^(-1)盐酸溶液混合提取,HLB固相萃取柱净化,UPLC-MS/MS检测,基质匹配校准外标法定量。结果表明:15种喹诺酮在2~50 ng·mL^(-1)浓度范围内线性良好,决定系数(R^(2))>0.99,检出限为5μg·kg^(-1),定量限为10μg·kg^(-1),添加量为10、20、500μg·kg^(-1)浓度时,平均回收率为76.2%~109.0%,相对标准偏差(RSD)为1.3%~12.4%(n=6)。该方法实现了较低的检测限、定量限,较高回收率和稳定性,可应用于畜禽排泄物中喹诺酮类药物残留量的监测,为畜禽排泄物在种植业中的科学施用提供准确指导,为间接监测养殖过程中各喹诺酮类药物的含量提供技术方法,指导养殖企业合理使用抗菌药物。An analytical method for the simultaneous determination of 15 quinolones residues in livestock and poultry excrement by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The sample was crushed and sieved after freeze-drying,extracted by mixing N,N-dimethylformamide(DMF)and 0.1 mol·L^(-1) hydrochloric acid solution,purified by HLB solid phase extraction column,detected by UPLC-MS/MS,and quantified by matrix matching calibration external standard method.The results showed that the linearity of 15 quinolones was good in the concentration range of 2-50 ng·mL^(-1),the coefficient of determination(R^(2))>0.99,and the detection limit was 5μg·kg^(-1),limit of quantitation was 10μg·kg^(-1),the average recovery rate was 76.2%-109.0%,relative standard derivation(RSD)was 1.3%-12.4%(n=6)at the concentration of 10,20 and 500μg·kg^(-1).This method has achieved lower detection limit,quantitative limit,higher recovery rate and stability.It can be applied to the monitoring of quinolones residues in livestock and poultry excrement,provide accurate guidance for the scientific application of livestock and poultry excrement in the planting industry,provide technical methods for indirect monitoring of the content of quinolones in the breeding process,and guide the rational use of antibiotics by breeding enterprises.

关 键 词：超高效液相色谱串联质谱(UPLC-MS/MS) 喹诺酮类 畜禽排泄物 

分 类 号：S859.8[农业科学—临床兽医学]