摘要
目的验证实验室是否能够依据标准方法准确开展养殖水产品中氟喹诺酮类药物残留检测工作。方法本文按照《水产品中17种磺胺类及15种喹诺酮类药物残留量的测定液相色谱-串联质谱法》(农业部1077号公告—1—2008)和《实验室质量控制规范食品理化检测》(GB/T 27404—2008)中的方法要求,采用高效液相色谱串联质谱法(HPLC-MS/MS)对养殖水产品中5种氟喹诺酮类药物残留检测进行方法验证,验证参数包括线性范围、方法灵敏度、正确度、精密度。结果恩诺沙星、诺氟沙星、氧氟沙星、达氟沙星、沙拉沙星添加含量为0.5~100μg/kg时,相关系数均大于0.99具有良好的线性关系,回收率在93.0%~110%之间,相对标准偏差(RSD)均小于15%,方法灵敏度(最低检出含量为0.940μg/kg,定量限为2μg/kg)满足检测方法中检出限、定量限要求。结论表明该实验室现有检测条件符合标准方法的技术能力要求,能够正确运用标准方法开展养殖水产品中氟喹诺酮类药物的残留检测工作。
Objective To verify whether the laboratory can accurately detect fluoroquinolone residues in aquaculture products according to standard Methods.Methods In this article,according to the Methods of Determination of 17 Sulfonamides and 15 Quinolones Residues in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry(Ministry of Agriculture Announcement No.1077-1-2008)and Laboratory Quality Control Specifications for Food Physical and Chemical Testing(GB/T 27404-2008),the method validation of the determination of 5 fluoroquinolones residues in cultured aquatic products by Liquid Chromatography-Tandem Mass Spectrometry was carried out,including linearity range,method sensitivity,accuracy and precision.Results The results showed that the 5 target compounds had good linear relationships in the range of 0~100μg/kg,with correlation coefficients above 0.99.The method sensitivity(detection limit,quantification limit)met the method requirements,the average recovery rate was 93.0%~110%,and the relative standard deviation was≤15%,all of which met the method requirements.Conclusion It indicates that the laboratory can correctly apply this method for detection work under the existing detection conditions.
作者
郭兰
刘鑫
邬杰
吕婷
王建军
白志荣
GUO Lan;LIU Xin;WU Jie;LV Ting;WANG Jian-Jun;BAI Zhi-Rong(Baotou Agricultural and livestock Product Quality and Safety Center,Baotou 014000,China)
出处
《实验室检测》
2024年第2期102-108,共7页
Laboratory Testing
关键词
液相色谱-串联质谱法
养殖水产品
氟喹诺酮类药物
方法验证
liquid chromatography-tandem mass spectrometry
farmed aquatic products
fluoroquinolones
method validation
作者简介
通信作者:刘鑫,硕士,高级兽医师,主要从事农畜产品质量安全监管研究。E-mail:474647378@qq.com;郭兰,硕士,初级工程师,包头市农畜产品质量安全中心,主要从事农畜水产品中农兽药残留检测研究。Email:gl17886750621@163.com
