快速高效液相色谱-串联质谱法同时测定水产品中5类33种药物残留

建立了快速高效液相色谱-串联质谱法(RRLC-MS/MS)同时测定水产品中四环素类、喹诺酮类、磺胺类、磺胺增效剂和三苯甲烷类共5大类33种药物残留的方法。样品用Na2EDTA-Mcllvaine缓冲溶液及乙腈提取,正己烷脱脂后,用RRLC进行分离。在电喷雾正离子模式下,以动态多反应监测(Dynamic MRM)方式采集数据进行定性与定量分析。33种药物在相应的浓度范围内线性良好,相关系数均大于0.99;在3个不同浓度添加水平下,平均回收率为63.6%～115.2%;相对标准偏差(RSD)为4.6%～14.6%;检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.1～2.0μg/kg和0.5～5.0μg/kg。本方法简便快速、灵敏可靠,适用于水产品中药物多残留的同时快速定性与定量测定。

Simultaneous Determination of 33 Medicine Residues in Aquatic Products by Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry

A new approach for the simultaneous determination of five classes residues,tetracyclines,quinolones,sulfoamides,tripmethoprim and triphenylmethane,in aquatic products by rapid resolution liquid chromatography-tandem mass spectrometry(RRLC-MS/MS) was established.Analytes were extracted by Na2EDTA-Mcllvaine buffer and acetonitrile,then defatted using hexane.Electrospray ionization mass spectrometry was operated in the positive mode using dynamic multiple reaction monitoring(DMRM) for the qualitative and quantitative analysis of 33 analytes after the separation on RRLC.The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration range.The average recoveries of the 33 analytes ranged from 63.6% to 115.2%,and the relative standard deviation(RSD) in three different concentrations was 4.6%-14.6%.The limit of detection(LOD,S/N≥3) and quantification(LOQ,S/N≥10) were 0.1-2.0 μg/kg and 0.5-5.0 μg/kg,respectively.The method is simple,fast,sensitive and reliable,and is suitable for the determination of residues in aquatic products.