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高效液相色谱与质谱联用检测猪肉中头孢类抗生素的残留

Determination of Cephalosporins Residues in Pork by High Performance Liquid Chromatography-Mass Spectrometry

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【作者】 范莹莹其鲁杨树民

【Author】 FanYingying~1 Qi Lu~2 Yang Shumin~3 (~1Citic GuoAn Meng GuLi Powder Source Technology Co.LTD,Beijing 102200,China;~2 PeKing University,Bejing 100871,China;~3Doping Control Center of China,Bejing 100029,China)

【机构】 中信国安盟固利电源技术有限公司北京大学国家体委兴奋剂检测中心 北京 102200北京 100871北京 100029

【摘要】 采用高效液相色谱与质谱联用法简单快速测定猪肉组织中8种头孢类抗生素的残留。样品添加8种头孢类抗生素(头孢羟氨苄、头孢氨苄、头孢克洛、头孢拉定、头孢噻肟、头孢唑啉、头孢孟多酯钠、头孢噻吩),采用0.5%的冰醋酸水溶液提取,匀浆离心分离后通过固相萃取柱净化,甲醇洗脱,用二极管阵列检测器及质谱检测器检测,信噪比较高,数据结果准确。采用XTerra MS-C18(2.1×150mm,5μm)色谱柱,以10mmoL/L甲酸铵和乙腈为流动相进行梯度洗脱。对于不同的药物,回收率范围为52%~98%(添加水平为0.1mg/kg,0.2mg/kg,0.5mg/kg),相对标准偏差在1.1%~10.55%以内,方法的最低检出限为0.2ppb~2.2ppb。大量的实验结果表明,该方法适合于猪肉中头孢类抗生素残留的测定。

【Abstract】 A simple and rapid method was developed for the determination of 8 Cephalosporins residues in pork by high performance liquid chromatography tandem mass spectrometry.The samples,with spiked 8 Cephalo- sporins( Cephadroxi、Cephalexin、Cephaclor、Cepharadine、Cephotaxime、Cephazolin、Cephamandole Sodium Salt、Cephalothin) were extracte 0.5% glacial acetic acid,followed by homogenizing and centrifuging precipitation, purified with solid-phase extraction column,eluted by methanol.The separation was performed on a XTerra MS -C18 (2.1×150mm,5μm)column using a mobile phase of 10mmol/L ammonium formate and acetonitrile and de- tected with diode-array detector,S/N is higher,data results is veracity.The limit of detection of the method is 0.2~2.2ppb for the various antibiotics and the recovery of the spike experiment is from 52% to 98% at three differ- ent spiked levels 0.1mg/kg,0.2mg/kg,0.5mg/kg,relative standard deviations are between 1.1%~10.55%.The results showed that the method is suitable for the determination of residues of Cephalosporins in pork.

【基金】 国家科技部“奥运科技(2008)行动计划”项目名称:“运动员食物安全保障系统研究”(编号:2002BA904B02)。
  • 【文献出处】 现代科学仪器 ,Modern Scientific Instruments , 编辑部邮箱 ,2007年06期
  • 【分类号】TS251.7
  • 【被引频次】16
  • 【下载频次】529
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