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

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.