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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
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郭霞，张素霞，沈建忠，李建成
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（中国农业大学 动物医学院，北京100094）
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摘要：
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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×4.6mm i.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%～828%，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。 |
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关键词：
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氟苯尼考；氟苯尼考胺；鱼肌肉；高效液相色谱；残留 |
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中图分类号：S 859.796文献标识码：
A 文章编号：1673-4696(2006)09-0743-05 |
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Simultaneous determination of residual florfenicol and florfenicol amine
in fish muscle by high performance liquid chromatography |
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GUO Xia，ZHANG Su-xia，SHEN Jian-zhong, LI Jian-cheng |
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(College of Veterinary Medicine, China Agricultural University，Beijing 100094，China) |
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Abstract: 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(5μm， 250mm×4.6mm i.d.), mobile phase were solution A ( 0.02mol/L heptanesulphonate-0.025mol/L trisodium phosphate,pH3.85 ) and solution B(methanol containing 1mL/L triethylamine) with a ratio of 68∶32, elution was gradients and ultraviolet detection wavelength was 225nm. In results, calibration curves were linear for two analytes at 10-1000μg/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 5μg/kg and 10μg/kg for FFa and FF，respectively. The limits of quantitation were 10μg/kg and 20μg/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. |
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Key words: florfenicol; florfenicol amine; fish muscle; HPLC; residues |
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