快速溶剂萃取-基质固相分散-高效液相色谱法测定牛肉中5种磺胺类药物残留  

Determination of Five Sulfonamide Residues in Beef by Accelerated Solvent Extraction-Matrix Solid-phase Dispersion Coupled with High Performance Liquid Chromatography

作　　者：游辉[1] 于辉[2] 武彦文[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：《分析测试学报》2010年第10期1087-1090,共4页Journal of Instrumental Analysis

基　　金：科技部创新方法工作专项资助项目(2008IM041400;2009IM033200)

摘　　要：建立了同时测定牛肉中5种磺胺类药物残留量的快速溶剂萃取-基质固相分散-高效液相色谱分析方法。通过优化样品处理条件,确定选取1.0g牛肉样品与3.0g弗罗里硅土混合,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磺胺。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。5种磺胺类药物在0.5～10.0mg/kg范围内线性关系良好(r≥0.9995),检出限为0.011～0.030mg/kg,加标回收率为89%～109%,相对标准偏差(n=5)为0.5%～4.3%。An analytical method was developed for the determination of 5 sulfonamide residues in beef by combination of matrix solid-phase dispersion（MSPD）,accelerated solvent extraction（ASE）and high performance liquid chromatography（HPLC）.The experimental conditions were optimized.Under the optimal conditions,1.0 g tissue sample was dispersed with 3.0 g Florisil.The sulfonamide residues were extracted with acetonitrile at 120 ℃ and 10 MPa.The determination of 5 sulfonamides was performed on an Ultimate XB-C18（4.6 mm×250 mm×5 μm）column（30 ℃）using acetonitrile-3% acetic acid（25∶75,by volume）as mobile phase at a flow rate of 1.0 mL/min.The UV detection wavelength was set at 268 nm.Good linearities for 5 sulfonamides were obtained within the range of 0.5-10.0 mg/kg with correlation coefficients not less than 0.999 5.The limits of detection were in the range of 0.011-0.030 mg/kg.The average recoveries ranged from 89% to 109% with relative standard deviations（n=5）of 0.5%-4.3%.

关 键 词：磺胺 基质固相分散 快速溶剂萃取 高效液相色谱 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]