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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
引用本文:于辉,游辉,武彦文,汪雨,赵萍.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[J].现代科学仪器,2010(6):93-96.
作者姓名:于辉  游辉  武彦文  汪雨  赵萍
作者单位: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
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。

关 键 词:快速溶剂萃取  高效液相色谱  磺胺类药物

Determination of Residual Sulfonamides in Animal Originated Food by High Performance Liquid Chromatography with Accelerated Solvent Extraction
Yu Hui,You Hui,Wu Yanwen,Wang yu,Zhao Ping.Determination of Residual Sulfonamides in Animal Originated Food by High Performance Liquid Chromatography with Accelerated Solvent Extraction[J].Modern Scientific Instruments,2010(6):93-96.
Authors:Yu Hui  You Hui  Wu Yanwen  Wang yu  Zhao Ping
Affiliation:1 Beijing Titan Instruments Co.,Ltd.,Beijing 100015;2Beijing Center for Physical & Chemical Analysis Beijing 100089)
Abstract: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.
Keywords:Accelerated solvent extraction  High performance liquid chromatography  Sulfonamides
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