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固相萃取高效液相色谱-质谱法测定动物组织中硝基呋喃代谢产物

Determination of Nitrofuran Metablolites in Animal Tissues by High Performance Liquid Chromatography-Mass Spectrometry and Study of Their Residual Discipline

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【作者】 林黎明林回春刘心同王曼霞张鸿伟王建华邱芳

【Author】 Lin Liming *, Lin Huichun, Liu Xintong, Wang Manxia, Zhang Hongwei, Wang Jianhua, Qiu Fang (Qingdao Exit-Entry Inspection and Quarantine Bureau,Qingdao 266002)

【机构】 青岛出入境检验检疫局青岛出入境检验检疫局 青岛200662青岛200662现在胶州市人民医院工作青岛200662

【摘要】 研究了对动物组织中4种硝基呋喃类代谢产物AOZ、AMOZ、SEM和AHD的自动固相萃取HPLCMS分析方法,分别以2氯苯甲醛和2硝基苯甲醛作为衍生化试剂,分别用AMOZd5、AOZd4作内标,用ENSPE柱进行提取,以乙腈0.1%甲酸为流动相,采用梯度洗脱,可在15min内将4种代谢产物完全分离并进行测定。回收率为85%~90%;检出限可达0.5μg/kg。采用两种衍生化方法可获得较多的定性确证信息。采用本方法研究了硝基呋喃在鸡饲养过程中的残留规律。

【Abstract】 A liquid chromatography-mass spectrometris method was developed for the simultameous determination of the metablolites of nitrofuran antibacterial drugs such as 3-amino-2-oxaolidone (AOZ), 5-mopholino-3-amino-2-oxazolidone (AMOZ)、semicabazide (SEM) and 1-aminohydantion (AHD) in animal tissues. Samples were derivatised using 2-chlorobenzaldehyde or 2-nitrobenzaldehyde,and using AMOZ-d5、AOZ-d4 as internal standards cleaned up with EN SPE columns and determined by high performance liquid chromatography-mass spectrometry. The analytes were separated and analysed by gradient elution of acetonitrle and 0.1% fomic acid in 15 minutes. The recoveries ranged from 85.0% to 90.0% and the detection limit was 0.5 μg/kg . More identified information is available by using two different derivative methods. Furthermore,the regulation of nitrofuran residues in chick feeding was studied.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2005年05期
  • 【分类号】TS251.7
  • 【被引频次】84
  • 【下载频次】648
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