高效液相色谱法同时测定禽蛋中环丙沙星、达氟沙星和恩诺沙星的残留量
Simultaneous Determination of the Residues of Ciprofloxacin, Danofloxacin and Enrofloxacin in Eggs by HPLC
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摘要: 采用高效液相色谱法同时测定禽蛋中环丙沙星、达氟沙星和恩诺沙星的残留量。样品经酸化甲醇超声提取后,提取液经正己烷脱脂,上清液在Purospher STAR LP RP-18色谱柱上分离,以pH 2.4的0.05 mol·L-1磷酸溶液-乙腈为流动相进行洗脱,采用荧光检测器检测,激发波长为280 nm,发射波长为450 nm。环丙沙星、达氟沙星、恩诺沙星的线性范围分别为0.005~0.50,0.001~0.10,0.005~0.50 mg·L-1,检出限(3S/N)分别为0.8,0.1,0.6 μg·kg-1。加标回收率在91.5%~98.3%之间,测定值的相对标准偏差(n=6)在0.45%~1.3%之间。Abstract: HPLC was applied to the simultaneous determination of the residues of ciprofloxacin, danofloxacin and enrofloxacin in eggs. The sample was treated with acidic methanol for extraction by ultrasonic. The extract solution was degeased with acetonitrile. The supernatant was separated on a Purospher STAR LP RP-18 chromatographic column, with a mixture of acetonitrile and 0.05 mol·L-1 phosphoric acid solution (pH 2.4) for elution. Fluorescence detector was used with λex of 280 nm and λem of 450 nm. The linearity ranges of ciprofloxacin, danofloxacin and enrofloxacin were 0.005-0.50, 0.001-0.10, 0.005-0.50 mg·L-1, respectively, with detection limits of 0.8, 0.1, 0.6 μg· kg-1, respectively. Recovery rates obtained by standard addition method were in the range of 91.5%-98.3%, and RSDs (n=6) were in the range of 0.45%-1.3%.