超高效液相色谱-串联质谱法同时测定畜禽排泄物中20种磺胺类药物的残留  

Simultaneous Determination of 20 Sulfonamides in Livestock and Poultry Excrement by UPLC-MS/MS

作　　者：裘丞军 薛银 邱鑫磊 黄娟 陈晓林 陈洁 QIU Chengjun;XUE Yin;QIU Xinlei;HUANG Juan;CHEN Xiaolin;CHEN Jie(Zhejiang Center of Animal Disease Control,Hangzhou 311199;Zhejiang Huanmao Automatic Control Technology Co.Ltd,Hangzhou 311100)

机构地区：[1]浙江省动物疫病预防控制中心,浙江杭州311199 [2]浙江环茂自控科技有限公司,浙江杭州311100

出　　处：《分析科学学报》2024年第1期57-64,共8页Journal of Analytical Science

基　　金：浙江省重点研发计划项目(2021C02007);浙江省农业重大技术协同推广计划(2021XTTGXM03)。

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定畜禽排泄物中20种磺胺类药物残留量的分析方法。样品经冷冻干燥后粉碎过筛,90%酸化乙腈提取,HLB固相萃取柱净化,UPLC-MS/MS检测,基质匹配校准外标法定量。结果显示,20种磺胺类药物在2~250 ng/mL浓度范围内,线性良好,相关系数均>0.99,检出限为2μg/kg,定量限为5μg/kg。在添加浓度分别为5、10、500μg/kg时,平均回收率为78.0%~117%,相对标准偏差(n=6)为1.1%~14.2%。该方法具有较低的检出限、定量限及较高的回收率和稳定性,可应用于畜禽排泄物中20种磺胺类药物残留量的监测。A method for the simultaneous determination of 20 sulfonamides residues in livestock and poultry excreta by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was established.After freeze-drying,the sample was crushed and sieved,extracted with 90% acidified acetonitrile,purified with 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 20 sulfonamides was good at the concentration of 2-250 μg/mL,the correlation coefficient r>0.99,the detection limit was 2 μg/kg and the limit of quantitation was 5 μg/kg.The average recovery was 78.0%-117% and RSD was 1.1%-14.2%(n=6) at the concentration of 5,10 and 500 μg/kg.This method has achieved a low detection limit and quantitative limit,high recovery rate and stability,and can be used to monitor the residues of 20 sulfonamides in livestock and poultry excreta,providing accurate guidance for the scientific application of livestock and poultry excreta in the planting industry.On the other hand,it can indirectly monitor the content of sulfonamides in the breeding process,and guide the breeding enterprises to reasonably use antibacterial drugs.

关 键 词：超高效液相色谱-串联质谱(UPLC-MS/MS) 磺胺类 畜禽排泄物 

分 类 号：O657.63[理学—分析化学]