节点文献
高效液相色谱-串联质谱法同时测定蜂蜜中甲硝唑、二甲硝咪唑和洛硝哒唑残留
Simultaneous Determination of Residues of Metronidazole,Dimetridazole and Ronidazole in Honey by High Performance Liquid Chromatography Tandem Mass Spectrometry
【摘要】 目的采用高效液相色谱-串联质谱(HPLC-MS/MS)技术,建立同时检测蜂蜜中甲硝唑(MNZ)、二甲硝咪唑(DMZ)和洛硝哒唑(RNZ)残留量的方法。方法样品加入水均质后,采用乙腈-氯仿-异丙醇(3∶57∶40,V/V/V)的混合液提取,亲水/亲油平衡(HLB)固相萃取柱净化,高效液相色谱-串联质谱-电喷雾正离子多反应监测方式(MRM)进行测定。结果3种药物在检测范围内线性良好,相关系数r均大于0.999。在0.2~100ng/g范围内,加样回收率在90.78%~101.61%之间,相对标准偏差均小于9.4%。结论此方法具有灵敏、准确、简便、快速等优点,适用于蜂蜜中硝基咪唑类药物残留的同时确证检测。
【Abstract】 Objective A high performance liquid chromatography tandem mass spectrometry (HPLC MS/MS) method was used to simultaneously detect the amount of metronidazole (MNZ),dimetridazole (DMZ) and ronidazole (RNZ) remained in honey. Methods After a preliminary homogenization in water,samples were extracted with a mixture of acetonitrile-chloroform-isopropanol (3∶57∶40,V/V/V) and purified by HLB SPE cartridge. Then,the samples were evaluated and determined by high performance liquid chromatography-electrospray (HPLC-ESI) (+)-tandem mass spectrometry (MS/MS) using the multiple reaction monitoring (MRM) mode. Results MNZ,DMZ and RNZ showed a good linear relationship and the related coefficient was all more than 0.999. The average recoveries of spiked samples were changed from 90.78% to 101.61% and the relative standard deviation (RSD) was lower than 9.4%. Conclusion The method was sensitive,accurate,convenient and fast,and could be used to simultaneously confirm multi-residue of nitromidazole in honey.
【Key words】 metronidazole; dimetridazole; ronidazole; honey; solid phase extraction; high performance liquid chromatography-tandem mass spectrometry;
- 【文献出处】 华中科技大学学报(医学版) ,Acta Medicinae Universitatis Scientiae et Technologiae Huazhong , 编辑部邮箱 ,2008年06期
- 【分类号】R155.5
- 【被引频次】14
- 【下载频次】273