RAPID AND EFFICIENT PURIFICATION OF CIMETROPIUM BROMIDE AND MIFENTIDINE DRUG METABOLITE MIXTURES DERIVED FROM MICROSOMAL INCUBATES FOR ANALYSIS BY MASS-SPECTROMETRY

被引:16
作者
KAJBAF, M [2 ]
JAHANSHAHI, M
PATTICHIS, K
GORROD, JW
NAYLOR, S
机构
[1] UNIV LONDON,KINGS COLL,CHELSEA DEPT PHARM,LONDON SW3 6LX,ENGLAND
[2] MRC,TOXICOL UNIT,CARSHALTON SM5 4EF,SURREY,ENGLAND
来源
JOURNAL OF CHROMATOGRAPHY-BIOMEDICAL APPLICATIONS | 1992年 / 575卷 / 01期
关键词
D O I
10.1016/0378-4347(92)80506-L
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A comparative study of the use of organic solvent extraction versus Sep-Pak C18 cartridges in the recovery and analysis of phase I (unconjugated) drug metabolites using mass spectrometry is presented. Standard mixtures of putative metabolites of the anticholinergic drug cimetropium bromide and the H-2-antagonist mifentidine were purified from inactivated liver microsomal preparations using both methods, and subsequently the recovery of each compound was quantitated. In general, the percentage recovery and degree of purification were greater when using Sep-Pak C18 cartridges compared with organic solvent extraction. Even more efficient recovery was achieved when zinc sulphate precipitation of proteins in the liver microsomal mixtures was carried out prior to analysis. Also, the HPLC-grade solvents used in this study contained a variety of ultraviolet-inactive, hydrophobic components. This leads to problems of suppression in fast atom bombardment mass spectrometric analysis. Using Sep-Pak C18 cartridges directly prior to analysis by fast atom bombardment with single or tandem mass spectrometry leads to far superior mass spectral results compared with organic solvent extraction.
引用
收藏
页码:75 / 85
页数:11
相关论文
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