快速溶剂萃取-高效液相色谱法测定鸡肉中磺胺类药物残留  被引量:3

Determination of Residual Sulfonamides in Animal Originated Food by High Performance Liquid Chromatography with Accelerated Solvent Extraction

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作  者:于辉[1] 游辉 武彦文 汪雨 赵萍[1] 

机构地区:[1]北京吉天仪器有限公司,北京100015 [2]北京理化分析测试中心,北京100089

出  处:《现代科学仪器》2010年第6期93-96,共4页Modern Scientific Instruments

基  金:科技部专项支持项目;项目编号:2009IM033200

摘  要:目的利用快速溶剂萃取(ASE),反相高效液相色谱-紫外检测技术,建立了鸡肉中5种磺胺类药物残留的定量分析方法。方法选择乙腈作为萃取溶剂,优化了快速溶剂萃取法的条件,快速溶剂萃取仪在l0.0MPa、120℃条件下萃取10 min,萃取液经正己烷去脂净化,减压干燥后用流动相溶解定容。选择C18分析柱,体积比为25∶2∶73的乙腈-乙酸-水溶液作为流动相,在柱温为30℃,流动相流速为1.0 mL/min,进样量为10μL,于268nm波长处,用紫外检测器检测,外标法定量。结果当添加水平为500μg/kg时,鸡肉中5种磺胺类药物的加标回收率在86.0%~101.7%,加标回收率的相对标准偏差在3.1%~4.3%(n=5),检出限为3~9μg/kg。Objective A method is developed for determining residual five sulfonamides in chicken using accelerated solvent extraction and high performance liquid chromatography.Method Extraction was performed with acetonitrile at 10.0MPa and a temperature of 120°C for 10 min.Hexane was used for clean up.Evaporate to dryness on rapid concentrating apparatus.Dissolve the residue in 1mL mobile phase.For the HPLC determination,an C18 column was used with a mixture of acetonitrile-acetic acid-water(25:2:73,v/v) as the mobile phase.Column temperature was 30°C;Flow rate was 1.0 mL/min;Injection volume was 10 μL;Determination was by UV detection at 268nm.The external standard method was employed for qualitative and quantitative analysis.Results The recoveries of sulfonamides in chicken were 86.0%~101.7% when the spiked concentration was 500 μg/kg,the relative standard deviation lower than 4.3%(n=5),the detection limits were 3~9 μg/kg.

关 键 词:快速溶剂萃取 高效液相色谱 磺胺类药物 

分 类 号:S859.84[农业科学—临床兽医学]

 

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