【摘要】 采用超高效液相色谱-电喷雾串联质谱仪(UPLC-ESI-MS/MS)同时测定水产品中的氯霉素、甲砜霉素和氟苯尼考3种氯霉素类药物残留量。该方法经乙酸乙酯提取样品,正己烷脱脂净化,超高效液相色谱C18柱分离,电喷雾负离子多反应模式(MRM)检测。氯霉素定量检出限为0.10μg/kg,线性范围为0.10～50.0μg/L,在阴性样品0.10～2.00μg/kg的氯霉素添加浓度下,平均回收率为84.7%～104.9%;甲砜霉素和氟苯尼考定量检出限均为0.50μg/kg,线性范围为0.50～50.0μg/L,在阴性样品0.50～10.0μg/kg的添加浓度下,甲砜霉素平均回收率为88.2%～104.1%,氟苯尼考平均回收率为91.9%～104.1%。且所有测定结果的批内相对标准偏差(RSD)均小于15%。结果表明该方法简便快捷,准确度和精密度高,适用于水产品中氯霉素类药物残留快速检测的要求。更多还原

【Abstract】 A method was developed for the simultaneous determination of chloramphenicol,thiamphenicol and florfenicol residues in aquatic products using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS).The homogenized samples were extracted with ethylacetate and the extracts were partitioned with n-hexane to remove lipids.Further chromatographic separation was carried out on UPLC C18 column.Multiple reaction monitoring(MRM) with electrespray ioniza tion in positive mode was used for detection.Quantitation limit was 0.10μg/kg for chloramphenicol,with goodlinearity ranged from 0.10-50.0μg/L.Average recoveries spiked in negative samples at the levels ofchloramphenicol from 0.10-2.00μg/kg were 84.7%-104.9%.Quantitation limit was 0.50μg/kg for thiamphenicoland florfenicol,and linearity rang was 0.50-50.0μg/L.Spiked at the levels from 0.50-10.0μg/kg,the averagerecoveries were 88.2%-104.1%for thiamphenicol and 91.9%-104.1%for florfenicol.The relative standarddeviations(RSD)for all intra-tests were less than 15%.With the advantages of simplicity,rapidity,highaccuracy and precision,this method could be suitable for the rapid detection of chloramphenicol drugs residuein aquatic products.更多还原