超高效液相色谱-串联质谱法测定禽肉中金刚烷胺、金刚乙胺和二甲金刚胺残留  

Determination of amantadine,rimantadine and dimethylamantadine residues in poultry by ultra-performance liquid chromatography-tandem mass spectrometry

作　　者：马健 陈艳宏 张明 赵媛坤 Ma Jian;Chen Yanhong;Zhang Ming;Zhao Yuankun(Gansu Longnan Center for Disease Control and Prevention,Longnan 746000,China;Gansu Chengxian Center for Disease Control and Prevention,Longnan 742500,China)

机构地区：[1]甘肃省陇南市疾病预防控制中心,陇南746000 [2]甘肃省陇南市成县疾病预防控制中心,陇南742500

出　　处：《卫生研究》2023年第2期286-291,共6页Journal of Hygiene Research

摘　　要：目的建立超高效液相色谱-串联质谱法测定禽肉基质中金刚烷胺、金刚乙胺和二甲金刚胺3种抗病毒类兽药残留的检测技术。方法禽肉样品采用酸化乙腈提取,盐析后取乙腈相,用十八烷基硅烷键合硅胶(C18)和N-丙基乙二胺(primary secondary amine,PSA)吸附剂分散固相萃取净化后,采用UPLC HSS T3色谱柱(100 mm×2.1 mm,1.7 mm)分离后于电喷雾正离子源和多反应监测扫描模式下进行测定,溶剂标准曲线结合稳定同位素内标法定量。结果3种目标化合物阴性样品加标水平在0.5、1.0和5.0μg/kg下,回收率为81.3%~99.7%,精密度为3.6%~11.1%(n=6)。3种目标化合物的检出限为0.06~0.20μg/kg,定量限为0.20~0.50μg/kg。对30件禽肉样品进行检测,均未检测到相关兽药残留。结论该方法操作简便、快速,灵敏度和准确度高,适用于禽肉中该类兽药残留的日常监测。OBJECTIVE To establish a method for determination of amantadine,rimantadine and dimethylamantadine residues in poultry matrix by ultra-performance liquid chromatography-tandem mass spectrometry.METHODS Poultry samples were extracted with acid acetonitrile,salting out,and then the organic phase was cleaned up by C18and PSA.A Waters ACQUITYTM UPLC HSS T3 column(100 mm×2.1 mm,1.7 mm)was used for liquid chromatography separation,ESI positive ion scan was used with multiple reaction monitoring(MRM)mode and quantified by matrix-matched external standard method.RESULTS At the spiked level of 0.5,1.0 and 5.0μg/kg,the recoveries of each compound were in the range of 81.3%-91.1%with the relative standard deviations of 6.5%-11.3%.The qualitative limits of detections were 0.06-0.2μg/kg and the quantitative limits were 0.2-0.5μg/kg for the 3 target compounds.The established method was applied to the detection of the 3 target compounds in 30 poultry samples,and none of the target compounds exceeded the residue limits.CONCLUSION The method is simple,rapid,high sensitivity and good stability,with a wide variety and a certain development.It can be used for the daily monitoring of the veterinary drug residues in poultry.

关 键 词：QUECHERS 金刚烷胺 金刚乙胺 二甲金刚胺 超高效液相色谱-串联三重四级杆质谱 禽肉 兽药残留 

分 类 号：R155.5[医药卫生—营养与食品卫生学]