快速溶剂萃取-高效液相色谱法同时测定牛肉中5种磺胺类药物残留  

Determination of Sulfonamide Residues in Beef by Accelerated Solvent Extraction Technique and High Performance Liquid Chromatography

作　　者：游辉[1] 于辉[2] 武彦文[1] 汪雨[1] 刘聪[1] 陈舜琮[1] 

机构地区：[1]北京市理化分析测试中心国产科学仪器应用示范中心,北京100089 [2]北京吉天仪器有限公司,北京100016

出　　处：《化学通报》2010年第9期854-857,共4页Chemistry

基　　金：科技部专项支持项目(2009IM033200)资助

摘　　要：建立了同时测定牛肉中5种磺胺药物残留量的快速溶剂萃取-高效液相色谱法。以乙腈为萃取剂在120℃、10MPa条件下用快速溶剂萃取仪提取样品中的目标物,提取液经冷冻除脂净化后,采用UltimateXB-C18色谱柱(4.6mm×250mm×5μm)分离,乙腈-3%乙酸溶液(体积比25:75)为流动相,流速1.0mL/min,柱温为30℃,在紫外检测波长268nm条件下进样10μL。该方法在0.01～0.10g/L范围内线性关系良好(r=0.999),最低检出限为0.011mg/kg,加标回收率在89.0%～107.8%范围内,相对标准偏差小于5.3%(n=5)。该方法快速、准确、简便,能够满足检测要求。A method for the determination of sulfonamide residues in beef was developed by high performance liquid chromatography（HPLC） coupled with accelerated solvent extraction（ASE）.The sulfonamide residues were extracted with acetonitrile at 120℃ and 10.0MPa.The extract was pretreated by a series of procedures such as freezing-lipid filtration.The determination was performed on a Ultimate XB-C18（4.6mm × 250mm × 5μm） column（30℃） using acetonitrile-3% acetic acid（25：75,V/V） as mobile phase at the flow rate of 1.0mL/min and the UV detection wavelength at 268nm.A good linearity was obtained within the range of 0.01 ～ 0.10g /L（r = 0.999）.The limit of detection for the method was 0.011mg /kg.The average recovery was ranged from 89.0% to 107.8% with relative standard deviations below 5.3%（n = 5）.This method is rapid,accurate,simple and able to meet the testing requirements.

关 键 词：磺胺 药物残留 快速溶剂萃取 高效液相色谱 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]