UPLC-MS/MS固相萃取法检测鸡肝、鸡胗中11种喹诺酮、4种四环素、氯霉素残留  

UPLC-MS/MS and solid phase extraction determination of 11 quinolones,4 tetracyclines and chloramphenicol residues in chicken liver and gizzard

作　　者：李堃[1] 赵丹莹[1] 李晔[1] 郭爱华[1] 温雅[1] LI Kun;ZHAO Danying;LI Ye;GUO Aihua;WEN Ya(Psychology Department of Disease Prevention and Control Center in Xicheng District,Beijing,100120,China)

机构地区：[1]北京市西城区疾病预防控制中心理化科,北京100120

出　　处：《职业与健康》2024年第6期761-766,共6页Occupation and Health

摘　　要：目的建立检测鸡肝、鸡胗中11种喹诺酮、4种四环素、氯霉素残留的高效、便捷的检测方法。方法鸡胗、鸡肝经提取、净化、固相萃取等步骤处理后,利用超高压液相色谱-质谱/质谱仪(ultra-high performance liquidchromatography-tandem mass spectrometer,UPLC-MS/MS)对兽药残留进行分离,定量测定。结果 16种兽药残留线性范围为1.0~40 ng/mL(氯霉素0.1~4.0 mg/mL),相关系数除诺氟沙星其他均>0.999 0,在不同浓度情况下测定平均回收率在61.6%~107.1%,诺氟沙星、环丙沙星、达氟沙星、四环素、强力霉素、土霉素、金霉素方法检出限为0.6μg/kg,定量限为1.8μg/kg;二氟沙星、培氟沙星、氧氟沙星、恩诺沙星、洛美沙星、沙拉沙星、恶喹酸、氟甲喹方法检出限为0.2μg/kg,定量限为0.6μg/kg;氯霉素方法检出限为0.02μg/kg,定量限为0.06μg/kg。结论用本方法对2022年采集的鸡胗、鸡肝样本进行检测,线性范围、检出限、精密度、准确度均达到检测要求。本方法提高了检测效率,适合市场上鸡肝、鸡胗的大量样品的兽药筛查检测,适合作为食品安全风险监测快速筛查的方法。Objective To establish efficient and convenient detection methods for detecting 11 kinds of quinolones,4 kinds of tetracycline and chloramphenicol residues in chicken liver and gizzard.Methods After processing chicken gizzards and liver through extraction,purification and solid phase extraction,UPLC-MS/MS was used to separate and quantitatively determine the residues of veterinary drugs.Results The linear range of residues of 16 veterinary drugs was 1.0-40 ng/mL(chloramphenicol 0.1-4.0 ng/mL),the correlation coefficient was greater than 0.9990 except norfloxacin,and the average recovery rate was 61.6%-107.1%determined at different concentrations,and the detection limit of norfloxacin,ciprofloxacin,dafloxacin,tetracycline,doxycycline,oxytetracycline,chlortetracycline,doxycycline,and chlortetracycline was 0.6μg/kg,and the limit of quantification was 1.8μg/kg.The detection limit of difloxacin,pefloxacin,ofloxacin,enrofloxacin,lomefloxacin,salafloxacin,oxaquinic acid,and flumequine was 0.2μg/kg,and the limit of quantification was 0.6μg/kg.The detection limit of chloramphenicol was 0.02μg/kg,and the limit of quantification was 0.06μg/kg.Conclusion Using this method to detect the chicken gizzards and liver samples collected in 2022,the liner range,detection limit,precision and accuracy all meet the detection requirements.This method improves the detection efficiency,is suitable for veterinary drug screening and detection of a large number of samples of chicken liver and gizzard on the market,and is suitable as a rapid screening method for food safety risk monitoring.

关 键 词：超高压液相色谱-质谱/质谱仪 固相萃取 喹诺酮 四环素 氯霉素 鸡胗 鸡肝 

分 类 号：O657.63[理学—分析化学] R155.5[理学—化学]