养殖水产品中氟喹诺酮类药物残留检测的方法验证
Method validation for the detection of fluoroquinolone residues in farmed aquatic products
郭兰 1刘鑫 1邬杰 1吕婷 1王建军 1白志荣1
作者信息
- 1. 包头市农畜产品质量安全中心,包头 014000
- 折叠
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 0.5～100 μg/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 0.940 μg/kg,定量限为 2 μg/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.
Abstract
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 0～100 μg/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.
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Key words
liquid chromatography-tandem mass spectrometry/farmed aquatic products/fluoroquinolones/method validation引用本文复制引用
出版年
2024
NETL
NSTL
万方数据