Separation, isolation, and characterization of isoform impurities of Gemcitabine formed during the Anomerization of protected α‐Gemcitabine to Gemcitabine

Hiriyanna, S. G. and Basavaiah, K. and Pati, Hari N. and Bijay, K. (2007) Separation, isolation, and characterization of isoform impurities of Gemcitabine formed during the Anomerization of protected α‐Gemcitabine to Gemcitabine. Journal of Liquid Chromatography & Related Technologies, 30 (20). pp. 3093-3105. ISSN 1520-572X

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Official URL: https://doi.org/10.1080/10826070701633780

Abstract

In the impurity profile of the gemcitabine active pharmaceutical ingredient, two process related impurities (0.12%) were detected other than the known α‐isomer of gemcitabine impurity in HPLC with respect to gemcitabine. The mass spectral data and UV spectrum of these two impurities were similar to that of gemcitabine. These impurities were referred as isoform impurity I and isoform impurity II. These isoform impurities were isolated from a crude sample of gemcitabine bulk drug using a reverse phase preparative high performance liquid chromatography (prep‐HPLC), and were characterized by LC‐MS, LC‐MS/MS, and FT‐NMR experimental techniques. Based on the results obtained from the different spectroscopic experiments, these isoform impurities were characterized as β‐anomer of 4‐amino‐1‐(3,3‐difluoro‐4,5‐dihydroxy tetrahydro‐2H‐pyran‐2‐yl)pyrimidin‐2(1H)‐one (isoform impurity I) and α‐anomer of 4‐amino‐1‐(3,3‐difluoro‐4,5‐dihydroxy tetrahydro‐2H‐pyran‐2‐yl)pyrimidin‐2(1H)‐one (isoform impurity II), respectively. Formation, separation, isolation, and characterization of these isoform impurities were discussed in detail.

Item Type: Article
Subjects: C Chemical Science > Chemistry
Divisions: Department of > Chemistry
Depositing User: C Swapna Library Assistant
Date Deposited: 23 Sep 2019 10:24
Last Modified: 23 Sep 2019 10:24
URI: http://eprints.uni-mysore.ac.in/id/eprint/8390

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