Preparative isolation and structural elucidation of impurities in fluconazole by LC/MS/MS.

Abstract:

:Three impurities were detected in the LC/MS analysis of fluconazole bulk drug substance. Two of the impurities were unknowns having not been reported previously. Structural assignment of these impurities was carried out by LC/MS/MS using electrospray ionization source and an ion trap mass analyzer. Structural elucidation using nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy was facilitated by newly developed rapid preparative isolation method. These impurities were characterized as 1-(1-H-1,2,4-triazole-1-yl) propane-2,3-diol and Z-2-(2,4-difluorophenyl)-3-(1-H-1,2,4-triazole-1-yl)-2-propen-1-ol. Their formation and synthesis are discussed.

journal_name

J Pharm Biomed Anal

authors

Dongre VG,Karmuse PP,Ghugre PD,Salunke SM,Panda N,Kumar A

doi

10.1016/j.jpba.2006.04.012

subject

Has Abstract

pub_date

2006-09-26 00:00:00

pages

334-40

issue

3

eissn

0731-7085

issn

1873-264X

pii

S0731-7085(06)00320-7

journal_volume

42

pub_type

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