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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 预览 被引量:13

Determination of Five Sulfonamide Residues in Beef by Accelerated Solvent Extraction-Matrix Solid-phase Dispersion Coupled with High Performance Liquid Chromatography
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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%.
作者 游辉 于辉 武彦文 陈舜琮 YOU Hui,YU Hui,WU Yan-wen,CHEN Shun-cong(1.Application & Demonstration Center for Homegrown Scientific Instruments,Beijing center for Physical & Chemical Analysis,Beijing 100089,China;2.Beijing Titan Instruments Co.,Ltd.,Beijing 100016,China)
出处 《分析测试学报》 CAS CSCD 北大核心 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)
关键词 磺胺 基质固相分散 快速溶剂萃取 高效液相色谱 sulfonamide matrix solid-phase dispersion(MSPD) accelerated solvent extraction(ASE) high performance liquid chromatography(HPLC)
作者简介 游辉(1981-),男,河南洛阳人,硕士,Tel:010—68466757,E-mail:yh2201@163.com
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