摘要
建立了以伊诺沙星为内标,环丙沙星、恩诺沙星、沙拉沙星、二氟沙星在鱼组织中的毛细管电泳多残留检测方法。研究了缓冲溶液的类型,pH值,有机试剂添加等电泳条件.得到最佳的缓冲溶液是含10ml/L乙腈的pH5.0的磷酸氢二钠-柠檬酸缓冲溶液。用C18固相萃取柱浓缩和净化处理,用二极管阵列检测器进行检测(275nm)。结果,四种药物在组织中的溶度25￣400μg/kg范围内R>0.999,线性关系良好。环丙沙星,恩诺沙星,沙拉沙星和二氟沙星回收率分别为75.2%,79.7%,80.1%,79.2%。恩诺沙星的检测限低于25μg/kg,其余的检测限均为25μg/kg,,方法的日内变异系数小于13.5%,日间变异系数小于12.3%。该方法简单快速,经济环保,适用于大量阳性样本的筛选。
A method for the determination of veterinary antimicrobial agent enrofloxacin, ciprofloxacin, sarafloxacin and difloxacin in fish muscle, using enoxacin as internal standard, has been developed. The influence of different separation conditions, such as the buffer, pH of the electrolyte and the organic added to the electrolyte was studied. The most suitable buffer is Na2HPO4-citrate at pH 5.0 containing 10%（v/v） acetonitrile. Clean-up and pre-concentration of the samples were effected by C18 solid-phase extraction and determination was carried out by capillary electrophoresis using a photodiode array detector （275nm）. The calibration graphs are linear for the four fluoroquinolones from 25 to 400 μg/kg. The method recoveries for enrofloxacin,ciprofloxacin,sarafloxacin and difloxacin are 75.2%,79.7%,80.1%,79.2%. The limit of detection for Enrofloxacin is lower than 25 μg/kg, and the other are 25μg/kg. The Rsds for intraday and interday are not more than 13.5% and 12.3%, respectively. It is a fast and simple method that allows the detection of positive muscle samples.
出处
《中国农学通报》
CSCD
2007年第2期93-97,共5页
Chinese Agricultural Science Bulletin
基金
国家自然科学基金重点项目"兽药及添加剂残留毒性
生态毒理学研究"部分内容(课题编号:30130140)
关键词
毛细管电泳
氟喹诺酮
残留
鱼组织
capillary electrophoresis
fluoroquinolone
residues
fish muscle
