陈笑艳, 钟大放, 姜浩, 顾景凯. 电喷雾离子阱质谱法直接测定几种药物的葡萄糖苷酸型代谢物J. 药学学报, 1998, 33(11): 849-854.
引用本文: 陈笑艳, 钟大放, 姜浩, 顾景凯. 电喷雾离子阱质谱法直接测定几种药物的葡萄糖苷酸型代谢物J. 药学学报, 1998, 33(11): 849-854.
Chen Xiaoyan, Zhong Dafang, Jiang Hao , Gu Jingkai, . CHARACTERIZATION OF SOME GLUCURONIDE CONJUGATES BY ELECTROSPRAY ION TRAP MASS SPECTROMETRYJ. Acta Pharmaceutica Sinica, 1998, 33(11): 849-854.
Citation: Chen Xiaoyan, Zhong Dafang, Jiang Hao , Gu Jingkai, . CHARACTERIZATION OF SOME GLUCURONIDE CONJUGATES BY ELECTROSPRAY ION TRAP MASS SPECTROMETRYJ. Acta Pharmaceutica Sinica, 1998, 33(11): 849-854.

电喷雾离子阱质谱法直接测定几种药物的葡萄糖苷酸型代谢物

CHARACTERIZATION OF SOME GLUCURONIDE CONJUGATES BY ELECTROSPRAY ION TRAP MASS SPECTROMETRY

  • 摘要: 为研究药物代谢产物的质谱规律,用电喷雾离子阱质谱法对溶液中乙氧苯柳胺、SFZ-47羧基衍生物、5-羟基普罗帕酮及普罗帕酮的β-D-葡萄糖苷酸型代谢物的结构进行了测定。结果表明,它们的(-)ESI-MS均生成M-H-准分子离子,(-)ESI-MS2和(-)ESI-MS3则分别生成m/z175和m/z113碎片离子。提示这些共同特征可用于LC/MS法直接分析药物的葡萄糖苷酸型代谢物。

     

    Abstract: To investigate the characteristics of mass spectra of some drug metabolites, solutions of glucuronide conjugates of N-(4-ethoxyphenyl)-2-hydroxyl-benzamide (etofesalamide), 4-(3H-1,2-dihydro-1-pyrrolizinone-2-methylamino)-benzoic acid, 5-hydroxypropafenone and propafenone were analyzed using electrospray ion trap mass spectrometry in a multi-stage full scan mode performed on a Finnigan LCQ instrument. Sample solutions were directly introduced into the ESI source at a flow rate of 15~30 μl·min-1 by a syringe pump. The mass spectrometer was operated in the negative ion mode. A full scan mass spectra of each analyte provided quasimolecular ion m/z M-1, and full scan MS2 and MS3 spectra gave characteristic fragment ions m/z 175 and m/z 113, respectively, which were derived from the glucuronate moiety of each analyte. The proposed interpretation of m/z 175 is the negative ion of glucuronic acid with a loss of 18 u (H2O), which produces m/z 113 after further losing 18 u (H2O) and 44 u (CO2). Fragmentation pathway has been established for each analyte. The results show that quasimolecular ion m/z M-1 and the characteristic fragment ions m/z 175 and m/z 113 in the multi-stage full scan mass analysis of each analyte can be predicted for future structure elucidation or quantitative determination of glucuronide conjugates by LC/MS.

     

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