鱼肌肉中氟苯尼考和氟苯尼考胺残留的高效液相色谱检测

Simultaneous determination of residual florfenicol and florfenicol amine in fish muscle by high performance liquid chromatography

建立了同时检测鱼肌肉组织中氟苯尼考和氟苯尼考胺残留的高效液相色谱检测法。以水和丙酮为提取溶液，Oasis MCX固相萃取柱为净化柱，采用Inertsil ODS-3（5μm，250mm×4．6mmi．d．）反相色谱柱，以A液（0．02mol／L庚烷磺酸钠-0．025mol／L磷酸钠溶液，二者体积比68：32，pH3．85）与B液（含1mL／L三乙胺的甲醇溶液）为流动相，梯度洗脱，紫外检测器225nm处检测。结果显示，在10～1000μg／kg浓度范围内，线性关系良好；加标回收率为75．9％～82．8％，日内变异系数为2．1％～5．8％，日间变异系数为4．7％～7．7％；氟苯尼考胺和氟苯尼考的检测限分别为5μg／kg和10μg／kg，定量限分别为10μg／kg和20μg／kg。结果表明，所建立的检测方法具有灵敏、准确、简便、快速的特点，适于同时检测鱼肌肉中氟苯尼考和氟苯尼考胺的残留。

A HPLC method was developed for simultaneous determination of residues of florfenicol （FF） and florfenicol amine（FFa） in fish muscle. Extractions were acetone and water, clean-up column was Oasis MCX solid-phase extraction（SPE） cartridge, analysis column was reversed-phase column of Inertsil ODS-3（5 μm, 250 mm×4.6 mm i. d. ）, mobile phase were solution A （ 0. 02 mol/L heptanesulphonate- 0. 025 mol/L trisodium phosphate, pH3. 85 ） and solution B（methanol containing 1 mL/L triethylamine） with a ratio of 68 ： 32, elution was gradients and ultraviolet detection wavelength was 225 nm. In results, calibration curves were linear for two analytes at 10-1 000 μg/kg of fortified. Overall recoveries were between 75.9% and 82.8%, and variation coefficients for within a day and between days were in the range of 2.1%-5.8% and 4.7%-7.7%, respectively. The detection limits were 5 μg/kg and 10 μg/kg for FFa and FF,respectively. The limits of quantitation were 10 μg/kg and 20 μg/kg for FFa and FF, respectively. The results showed that this method is sensitive, accurate, convenient and quick, which can be used to detect simultaneously FF and FFa residues in fish muscle.