摘要
采用固相萃取(SPE)结合液相色谱-串联质谱(LC-MS/MS)技术,建立了不同水产品组织中四环素类药物残留的测定方法。样品通过含EDTA的弱酸性MCI缓冲盐提取,醋酸铅沉淀蛋白,并结合正己烷和固相萃取(SPE)同时净化技术,以液相色谱-串联质谱多反应监测(MRM)离子模式定性,工作曲线法定量分析。结果表明,被测组分在对应范围内线性关系良好;方法的检出限为1.00μg/kg,定量限为5.00μg/kg;以空白鳗、鲤、海参和河豚鱼作为基质进行回收率评价,四环素、土霉素、金霉素和强力霉素等4种四环素类药物在不同加标浓度时的回收率范围为70%~100%,相对标准偏差皆小于10%(n=6)。将所建立的方法应用于实际养殖鳗中四环素类药物残留的分析,结果表明,该方法灵敏度高、重现性好,适用于不同水产生物样品中四环素类药物残留的同时检测。
A method for determination of tetracycl ines （TCs） antibiotics in aquatic products tissue was developed bysolid -phase extraction （SPE） coupled with liquid chromatography tandem mass spectrometry （LC -MS/MS）. The target analytes were extracted from the aquatic products using the Mcllvaine buffer solution. The proteins in samples were precipitated by lead acetate. Then the samples were cleaned-up through n - hexane combined with Oasis HLB solid phase extraction. LC - MS/MS in multiple reaction monitoring （MRM） mode was performed for the simultaneous qualitative and matrix external standard quantitative analysis of 4 kinds of tetracyclines antibiotics in eel tissues. The results showed that the good linearity was obtained in the corresponding range of all target analytes, with detection lim- its of 1.00 μg/kg and quantity limits of 5.00μg/kg. The average recoveries for 4 kinds of tetracyclines antibiotics were between 70.0% - 100% at different spiking levels in blank eel, cyprinoid, sea cucumber and puffer fish ma trices. The relative standard deviations （RSD） were all less than 10% （n = 6）. The presented method has high sen- sitivity, good reproducibility and is suitable for detection of residual TCs antibiotics residues in the aquatic products.
出处
《中国渔业质量与标准》
2017年第3期44-51,共8页
Chinese Fishery Quality and Standards
基金
中国水产科学研究院黄海水产研究所基本科研业务费(No.20603022016007)
国家自然科学基金项目(No.21207162)
山东省农业重大应用技术创新项目(No.SF1405303301)
农业部行业标准(No.2015-403)
关键词
水产品
四环素类药物
固相萃取
液相色谱-串联质谱
aquatic products
tetracycl ines （TCs）
solid phase extraction （SPE）
liquid chromatography - tandemmass spectrometry （ LC - MS/MS）
