高效液相色谱-荧光法测定水产品中氟苯尼考的残留量

HPLC Determination of Residual Amount of Florfenicol in Aquatic Products with Fluorimetric Detection

摘要: 提出了高效液相色谱-荧光法检测水产品中残留的氟苯尼考.以乙酸乙酯为提取溶液,C18固相萃取柱上净化.采用Agilent TC-C18反相色谱柱(250 mm×4.6 mm,5 μm)为固相柱,以pH 3.5乙酸盐缓冲溶液和乙腈以体积比55比45混合后作为流动相,在激发波长为225 nm,发射波长为280 nm的条件下进行荧光光度检测.结果表明:氟苯尼考质量浓度在0.1~5.0 mg·L-1范围内与峰面积呈线性关系,检出限(3S/N)为5.6 μg·kg-1.方法的回收率为88.6%~95.4%,相对标准偏差(n=6)为3.5%~8.3%.

Abstract: A method of HPLC determination of florfenicol in aquatic products with FPD was proposed.The sample was extracted with ethyl acetate and treated by SPE on C18 column.Reversed-phase chromatographic column of Agilent TC-C18 (250 mm×4.6 mm,5 μm) was used as the stationary phase,and a mixed solution of acetate buffer solution of pH 3.5 and acetonitrile mixed in the ratio of 55 to 45,was used as the mobile phase.Fluorimetric detection at the wavelengths of (λex) 225 nm and (λem) 280 nm was adopted.Linearity range of the method was found between 0.1-5.0 mg·L-1 of florfenicol,with detection limit (3S/N) of 5.6 μg·kg-1.Values of recovery and RSD (n=6) found were in the ranges of 88.6%-95.4% and 3.5%-8.3% respectively.