色谱

色谱

• 研究简报 • 上一篇    下一篇

固相萃取-高效液相色谱法测定动物肉组织中磺胺类药物的残留

张艳1,吴银良2

  

  1. 1. College of Science, China Agricultural University, Beijing 100094, China; 2. Quality Control and Inspection Center for Domestic Animal Products of Ministry of Agriculture, Beijing 100026, China
  • 收稿日期:2004-10-26 修回日期:1900-01-01 出版日期:2005-11-30 发布日期:1987-12-25
  • 通讯作者: 张艳

Determination of Residual Sulfonamides in Meat by High Performance Liquid Chromatography with Solid-Phase Extraction

ZHANG Yan1, WU Yinliang2   

  1. 1. College of Science, China Agricultural University, Beijing 100094, China; 2. Quality Control and Inspection Center for Domestic Animal Products of Ministry of Agriculture, Beijing 100026, China
  • Received:2004-10-26 Revised:1900-01-01 Online:2005-11-30 Published:1987-12-25

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摘要：

建立了一种快速、灵敏、环保的固相萃取-反相高效液相色谱同时分析动物肉组织中5种磺胺类药物残留的方法。将样品加入到盛有无水硫酸钠的离心管中，再用乙酸乙酯提取；提取液经氨基固相萃取柱净化后，用1.5%（体积分数）乙酸乙醇溶液洗脱。洗脱液用高效液相色谱分离,二极管阵列检测器检测,外标法定量。5种磺胺类药物的线性关系良好,磺胺二甲基嘧啶(SM2)、磺胺间甲氧嘧啶(SMM)、磺胺甲唑(SMZ)的线性范围均为30～5000 μg/L,磺胺二甲氧嘧啶(SDM)、磺胺喹啉(SQ)的线性范围均为60～5000 μg/L。2种动物肉组织(鸡肉、猪肉)中5种磺胺类药物的加标回收率在73.2%至97.3%范围内，当添加水平为50 μg/kg时，加标回收率的相对标准偏差在2.5%至11.6%范围内；SM2，SMM和SMZ的检测限（S/N=3）和定量限（S/N=10）分别为3 μg/kg和10 μg/kg，SDM和SQ的检测限和定量限分别为7 μg/kg和25 μg/kg。

关键词: 残留, 动物肉组织 , 高效液相色谱, 固相萃取, 磺胺类药物

Abstract:

A method was developed for determining residual sulfonamides (SAs) such as sulfamethazine (SM2), sulfamonomethoxine (SMM), sulfamethiazole (SMZ), sulfadimethoxine (SDM) and sulfaquinoxaline (SQ) in pork and chicken using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with a photodiode array detector. The samples were extracted with ethyl acetate. An NH2 column was used for clean up. For the HPLC determination, an Intersil ODS-2 column was used with a mixture of methanol-acetonitrile-water-acetic acid (2∶2∶9∶0.2, v/v) as the mobile phase. The detection limits (S/N=3) were 3 μg/kg for SM2， SMM and SMZ, and 7 μg/kg for SDM and SQ. The quantitation limits (S/N=10) were 10 μg/kg for SM2, SMM and SMZ, and 25 μg/kg for SDM and SQ. The linear ranges were 30-5000 μg/L for SM2, SMM and SMZ, and 60-5000 μg/L for SDM and SQ. The recoveries were between 73.2% and 97.3% with the relative standard deviations between 2.5% and 11.6% originated from the spiked level of 50 μg/kg.

Key words: high performance liquid chromatography, meat , residues, sulfonamides, solid-phase extraction