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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
【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.
【Key words】 high performance liquid chromatography-mass spectrometry (HPLC/MS); pork; Cephalosporins;
- 【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