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×4.6mmi.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.
出处
《中国兽药杂志》
2008年第7期13-16,共4页
Chinese Journal of Veterinary Drug
关键词
氟苯尼考
氟苯尼考胺
虾肌肉
高效液相色谱
残留
florfenicol
florfenicol amine
shrimp muscle
high performance liquid chromatography
residue