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

Detection of Florfenicol and Florfenicol amine Residues in Shrimp Muscle by High Performance Liquid Chromatography

关键词:  氟苯尼考  氟苯尼考胺  虾肌肉  高效液相色谱  残留

Key words:  florfenicol  florfenicol amine  shrimp muscle  high performance liquid chromatography  residue

摘要:

[摘 要] 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×4.6mm i.d.)反相色谱柱，以比例为68:32的A液（0.02 mol/L戊烷磺酸钠—0.025 mol/L磷酸钠溶液，pH 3.85）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10～1000 µg/kg浓度范围内，线性关系良好；添加浓度为50、100、200、500 μg/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10 μg/kg,定量限为30 μg/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。

Abstract:

Abstract: A 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 , 250mm×4.6mm i.d.), the mobile phase were solution A ( 0.02M pentanesulphonate-0.025M trisodium phosphate,PH 3.85 ) and solution B ( methanol containing 0.1% triethylamine ) with a comparison of 68:32, ultraviolet detection wavelength was 225nm. Calibration curves were linear for two analytes at 10~1000 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 30 µg/kg. The results show that the method is sensitive, accurate, convenient and quick, which can be used to detect simultaneously FF and FFa residues in shrimp muscle.