虾肌肉中氟苯尼考和氟苯尼考胺残留的高效液相色谱检测方法研究

Determination of Florfenicol and Florfenicol Amine Residues in Shrimp Muscle by High Performance Liquid Chromatography

建立了虾肌肉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固相萃取柱净化，采用Inertsil ODS-3（5μm，250mm×4．6mmi．d．）反相色谱柱，以比例为68：32的A液（0．02mol／L戊烷磺酸钠-0．025mol／L磷酸钠溶液，pH3．85）与B液（含0．1％三乙胺的甲醇溶液）为流动相，在225nm处检测。氟苯尼考和氟苯尼考胺在10～1000μg／kg浓度范围内，线性关系良好；添加浓度为50、100、200、500μg／kg时，回收率在75．8％～85．9％，日内变异系数在2．4％～4．5％，日间变异系数在4．0％～5．8％；方法的检测限为10μg／kg，定量限为30μg／kg。本方法灵敏、准确、简便、快速，适于虾肌肉中氟苯尼考和氟苯尼考胺残留的同时检测。

An HPLC method was developed for determining the residues of florfenicol （FF） and florfenicol amine （FFa） in shrimp muscle. The extractions were acetone and water, the clean -up column was Oasis MCX solid - phase extraction（SPE） cartridge, the analysis column was reversed- phase column of Inertsil ODS-3（5μm , 250 mm×4.6 mm i. d. ）, the mobile phase were solution A （ O. 02M pentanesulphonate - O. 025M trisodium phosphate, pH 3.85 ） and solution B （ methanol containing O. 1% triethylamine ） with a comparison of 68： 32, ultraviolet detection wavelength was 225 nm. Calibration curves were linear for two analytes at 10～1 000 μg/kg fortified. Overall recoveries were between 75.8% and 85.9%. Variation coefficients for with - day and between - day were in the range of 2.4%～4.5 % and 4.0% ～ 5.8 %. The limit of detection （LOD） was 10 μg/kg, the limit of quantitation （LOQ） was 30μg/kg. The results showed that the method was sensitive, accurate, convenient and quick, which can be used to detect simultaneously FF and FFa residues in shrimp muscle.