Authors:
S. G. Hiriyanna Department of Chemistry, University of Mysore, Manasagangothri, Mysore, 570006, Karnataka, India

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K. Basavaiah Department of Chemistry, University of Mysore, Manasagangothri, Mysore, 570006, Karnataka, India

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Summary

Five new peaks of potential impurities, ranging from 0.05 to 0.12% on an area-percent basis, have been observed in reversed-phase high-performance liquid chromatography of capecitabine drug substance. On the basis of comparison of relative retention times and mass values two of the impurities were identified as intermediates in the process used for synthesis of capecitabine and were characterized as (2-(4-amino-5-fluoro-2-oxopyrimidin-1(2H)-yl)-5-methyltetrahydrofuran-3,4-diyl diacetate and 2-(5-fluoro-2-oxo-4-(pentyloxycarbonylamino)pyrimidin-1(2H)-yl)-5-methyl tetrahydrofuran-3,4-diyl diacetate. The area percentages of two of the other peaks increased substantially when the drug was treated with acid and base. The three compounds other than the two intermediates were isolated by preparative HPLC with gradient elution and were characterized by use of spectroscopic techniques, viz. MS-MS, FTIR, and NMR (1H, 13C and DEPT). On the basis of the spectral data, the structures 5′-deoxy-5-fluorocytidine, 5′-deoxy-5-fluorouridine, and 2-(4-(bis(pentyloxycarbonyl)amino)-5-fluoro-2-oxopyrimidin-(2H)-yl)-5-methyltetrahydrofuran-3,4-diyl diacetate were proposed for the three impurities.

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Senior editors

Editor(s)-in-Chief: Kowalska, Teresa (1946-2023)

Editor(s)-in-Chief: Sajewicz, Mieczyslaw, University of Silesia, Katowice, Poland

Editors(s)

  • Danica Agbaba, University of Belgrade, Belgrade, Serbia
  • Łukasz Komsta, Medical University of Lublin, Lublin, Poland
  • Ivana Stanimirova-Daszykowska, University of Silesia, Katowice, Poland
  • Monika Waksmundzka-Hajnos, Medical University of Lublin, Lublin, Poland

Editorial Board

  • Ravi Bhushan, The Indian Institute of Technology, Roorkee, India
  • Jacek Bojarski, Jagiellonian University, Kraków, Poland
  • Bezhan Chankvetadze, State University of Tbilisi, Tbilisi, Georgia
  • Michał Daszykowski, University of Silesia, Katowice, Poland
  • Tadeusz H. Dzido, Medical University of Lublin, Lublin, Poland
  • Attila Felinger, University of Pécs, Pécs, Hungary
  • Kazimierz Glowniak, Medical University of Lublin, Lublin, Poland
  • Bronisław Glód, Siedlce University of Natural Sciences and Humanities, Siedlce, Poland
  • Anna Gumieniczek, Medical University of Lublin, Lublin, Poland
  • Urszula Hubicka, Jagiellonian University, Kraków, Poland
  • Krzysztof Kaczmarski, Rzeszow University of Technology, Rzeszów, Poland
  • Huba Kalász, Semmelweis University, Budapest, Hungary
  • Katarina Karljiković Rajić, University of Belgrade, Belgrade, Serbia
  • Imre Klebovich, Semmelweis University, Budapest, Hungary
  • Angelika Koch, Private Pharmacy, Hamburg, Germany
  • Piotr Kus, Univerity of Silesia, Katowice, Poland
  • Debby Mangelings, Free University of Brussels, Brussels, Belgium
  • Emil Mincsovics, Corvinus University of Budapest, Budapest, Hungary
  • Ágnes M. Móricz, Centre for Agricultural Research, Budapest, Hungary
  • Gertrud Morlock, Giessen University, Giessen, Germany
  • Anna Petruczynik, Medical University of Lublin, Lublin, Poland
  • Robert Skibiński, Medical University of Lublin, Lublin, Poland
  • Bernd Spangenberg, Offenburg University of Applied Sciences, Germany
  • Tomasz Tuzimski, Medical University of Lublin, Lublin, Poland
  • Yvan Vander Heyden, Free University of Brussels, Brussels, Belgium
  • Adam Voelkel, Poznań University of Technology, Poznań, Poland
  • Brata Walczak, University of Silesia, Katowice, Poland
  • Wiesław Wasiak, Adam Mickiewicz University, Poznań, Poland
  • Igor G. Zenkevich, St. Petersburg State University, St. Petersburg, Russian Federation

 

KOWALSKA, TERESA (1946-2023)
E-mail: kowalska@us.edu.pl

SAJEWICZ, MIECZYSLAW
E-mail:msajewic@us.edu.pl

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2023  
Web of Science  
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Rank by Impact Factor Q3 (Chemistry, Analytical)
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Acta Chromatographica
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Acta Chromatographica
Language English
Size A4
Year of
Foundation
1988
Volumes
per Year
1
Issues
per Year
4
Founder Institute of Chemistry, University of Silesia
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PL-40-007 Katowice, Poland, Bankowa 12
Publisher Akadémiai Kiadó
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Chief Executive Officer, Akadémiai Kiadó
ISSN 2083-5736 (Online)

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