摘要
建立了水产品中左氧氟沙星残留的超高效液相色谱串联质谱检测法。采用乙腈对样品中的待测物进行提取,正已烷除脂,浓缩后用固相萃取小柱进行净化,吹氮浓缩后采用超高效液相色谱质谱联用-电喷雾正离子和MRM多反应监测模式进行定性定量分析。检测浓度线性范围为0～100μg/kg,线性相关系数为0.9922,检出限为4.5μg/kg。在鳗鱼、虾和罗非鱼三种不同样品基质中进行添加浓度为10,20,50μg/kg的验证试验,该药物的回收率在72.5%～83.5%内,相对标准偏差(n=6)在7.9～11.4%之间,并对其质谱裂解和基质效应进行了研究。本检测方法快速,高效,灵敏度高,符合检测要求。
An analytical method was developed with Ultra Performance Liquid Chromatography Tandem Mass Spectrometry to determine Levofloxacin residues in aquatic products.The compound was extracted with acetonitrile and cleaned with hexane,followed by cleanup with LC-SCX SPE column,and concentrated with N2.Then the reconstituted sample solution was qualitative and quantitative analysis by UPLC-MS/MS under electrospray positive ion mode and multi-reaction monitoring（MRM）.The coefficient correlation of this method was 0.9922 for spiked samples（range from 0 to 100μg/kg）,the limit of quantification were 4.5 μg/kg.The method was validated at 10,20,50μg/kg in eel,shrimp and tilapia fish,the mean recoveries were 72.5%-83.5%,the RSD were 7.9-11.4%,investigated the MS fragmentation mechanism of this compound.The method is effective,fast and high sensitivity,meet the request of detection.
出处
《福建分析测试》
CAS
2011年第5期15-19,共5页
Fujian Analysis & Testing
基金
福建出入境检验检疫局科技计划项目(FK2008-12)
