【作者】 余丽梅； 张聪； 宋超； 裘丽萍； 张石云； 陈家长；

【Author】 YULimei;ZHANGCong;SONGChao;QIULiping;ZHANGShiyun;CHENJianzhang;Wuxi Fishery College of Nanjing Agricultural University;Freshwater Fisheries Research Center of Chinese Academy of Fishery Science;

【机构】 南京农业大学无锡渔业学院； 中国水产科学研究院淡水渔业研究中心； 农业部水产品质量安全环境因子风险评估实验室(无锡)； 农业部长江下游渔业生态环境监测中心；

【摘要】 建立了分散固相萃取(d SPE)-超高液相色谱/质谱(UPLC/MS/MS)测定水产品中磺胺类抗生素残留量的方法。实验主要比较了三种样品净化方法:分散固相萃取(d SPE)法、旋转蒸发浓缩法、国家标准净化方法,处理的水产样品,稀释后经UPLC/MS/MS进行检测分析。结果表明,分散固相萃取(d SPE)对样品前处理在快速,精确,简易程度上均优于其他两种方法。经分散固相萃取(d SPE)法净化后的磺胺类药物在0.5μg/L-50μg/L浓度范围内线性关系良好,相关系数均大于0.9;仪器检出限为0.0007μg/L-0.002μg/L,方法的检出限为0.007μg/kg-0.02μg/kg,定量限为0.02μg/kg-0.08μg/kg。在水产品中的加标回收率为67.5%-147.1%,RSD为2%-24.5%。该方法实现了快速、简单、准确地测定水产品中磺胺类抗生素残留分析,为研究水产品中磺胺类抗生素残留快速准确检测的方法提供参考。更多还原

【Abstract】 A method based on dispersive solid-phase extraction(d SPE)-ultra perfomance liquid chromatography-tandem mass spectrometry(UPLC/MS/MS)has been developed for the determination residues of sulfonamide antibiotics in aquatic products.The methods of dispersive solid-phase extraction(d SPE),rotary evaporation concentration and the purification method of national standard were compared mainly in dealing with aquatic samples,which were detected by UPLC/MS/MS after dilution.The results showed that dispersive solid-phase extraction(d SPE) was superior to another two methods on celerity,accuracy and the level of briefness.The calibration curves for all sulfonamide antibiotics(concentration range 0.5μg/L-50μg/L) were linear with correlation coefficients more than 0.9.Detection limits of instrument of 12 sulfonamide antibiotics were 0.0007μg/L-0.002μg/L, while detection limits of the method were 0.007μg/kg-0.02μg/kg and their quantity limits were 0.02μg/kg-0.08μg/kg.The recoveries were in the range of67.5%-147.1%,which the relative standard deviation ranged from 2% to24.5%.更多还原