超高效液相色谱-串联质谱法测定淡水鱼中18种喹诺酮类和氯霉素类抗生素  

Determination of 18 quinolones and chloramphenicols in freshwater fish by ultra - performance liquid chromatography tandem mass spectrometry

作　　者：刘少颖[1] 王兴龙 任韧[1] 金铨[1] 郑颖莹 LIU Shao-ying;WANG Xing-long;REN Ren;JIN Quan;ZHENG Ying-ying(Hangzhou Municipal Center for Disease Control and Prevention,Zhejiang 310021,China)

机构地区：[1]浙江省杭州市疾病预防控制中心,浙江310021 [2]杭州医学院

出　　处：《中国卫生检验杂志》2023年第9期1049-1052,1066,共5页Chinese Journal of Health Laboratory Technology

基　　金：浙江省分析测试科技计划项目(2018C37031)。

摘　　要：目的 建立淡水鱼中18种喹诺酮类和氯霉素类抗生素的超高效液相色谱-串联质谱快速测定方法。方法 样品经EDTA-Mcllvaine缓冲溶液超声提取,HLB固相萃取柱净化,HSS T3柱色谱分离,流动相为0.1%甲酸水溶液-0.1%甲酸乙腈,梯度洗脱,超高效液相色谱-串联质谱仪分离检测,内标法定量。结果 氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、环丙沙星、达氟沙星、二氟沙星、恩诺沙星、氟甲喹、恶喹酸、沙拉沙星、依诺沙星、西诺沙星、吡哌酸、萘啶酸、氯霉素、甲砜霉素、氟甲砜霉素18种抗生素在0.1 ng/ml~200 ng/ml浓度内线性良好,检出限(LODs)和定量限(LOQs)分别为0.01μg/kg~0.15μg/kg和0.02μg/kg~0.49μg/kg,回收率为67.7%~116.1%,相对标准偏差(RSDs)为2.64%~19.93%。结论 该方法简便、灵敏、可靠,适合于淡水鱼中18种喹诺酮类和氯霉素类抗生素的测定。Objective A method was developed and validated for the determination of 18 quinolones and chloramphenicols in freshwater fish by ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Methods The target analytes in samples were ultrasonically extracted with EDTA-Mcllvaine buffer solution and purified with HLB solid phase extraction column.Separation and detection were completed by UPLC-MS/MS with dynamic multiple reaction monitoring mode,and quantitative analysis was based on internal standard curves.Results The linear ranges of the method were within 0.1 ng/ml-200 ng/ml.The limits of detection(LODs)and limits of quantification(LOQs)of 18 antibiotics(ofloxacin,pefloxacin,norfloxacin,lomefloxacin,ciprofloxacin,danofloxacin,difloxacin,enrofloxacin,flumequine,oxolinic acid,sarafloxacin,enoxacin,cinoxacin,pipemidic acid,nalidixic acid,chloramphenicol,thiamphenicol and florfenicol)were within 0.01μg/kg-0.15μg/kg and 0.02μg/kg-0.49μg/kg,respectively.The recovery was within 67.7%-116.1%,and the relative standard deviation(RSD)was within 2.64%-19.93%.Conclusion The method is simple,sensitive and accurate and is suitable for the determination of 18 quinolones and chloramphenicols in freshwater fish.

关 键 词：超高效液相色谱-串联质谱法 淡水鱼 喹诺酮 氯霉素 

分 类 号：O657.63[理学—分析化学]