A method was developed for the determination of Ciprofloxacin Hydrochloride and Enrofloxacin in Caviar by high performance liquid chromatography with fluorescence detection . The homogenized sample was extracted with methanol and acidified acetonitrile .The extract was concentrated by nitrogen ,and redissolved into 2 mL mobile phase and defatted with n-hexane .Ciprofloxacin Hydrochloride and Enrofloxacin were separated on Eclipse XDB-C18 Column with mobile phases containing acetonitrile and 0.02 mol · L -1 oxalic acid (14 ∶ 86 ) and finally determined by fluorescence Detector .The detection limit of Ciprofloxacin Hydrochloride and Enrofloxacin were 1μg · kg -1 and 0.5 μg · kg -1 , separately .In the range of 5 -120 μg · kg -1 , the mean recoveries were more than 80% . The intraday and interday precisions were less than 5% .It showed that this accurate and sensitive method could be applied for the conventional residue testing requirements .%建立了鱼籽酱中盐酸环丙沙星和恩诺沙星的高效液相色谱-荧光检测方法。样品经甲醇及酸化乙腈提取，提取液经氮吹浓缩，残渣用2 mL流动相溶解，正己烷脱脂净化，采用Eclipse XDB-C18色谱柱，以乙腈∶0.02 mol · L -1草酸（14∶86）为流动相，荧光检测器检测。盐酸环丙沙星和恩诺沙星的检出限分别为1、0.5μg · kg -1，在添加量5～120μg · kg -1范围内，平均回收率均大于80％，相对标准偏差均小于5％。说明该方法灵敏、准确，满足常规残留检测要求。
展开▼
