Identification of related substances in capecitabine by LC-MS
Author(s): ZHANG Ge, LIU Chao-yi, CHEN Lei-lin, HANG Tai-jun, SONG Min, Department of Pharmaceutical Analysis, China Pharmaceutical University
Pages: 1902-1910
Year: 2015 Issue: 16
Journal: Chinese Journal of New Drugs
Keyword: capecitabine; related substances; HPLC; LC-TOF/MS; LC-MS /MS;
Abstract: Objective: To develop an LC-MS method for identification of the related substances in capecitabine. Methods: HPLC separation was carried out on a Sepax BR-C18column( 250 mm × 4. 6 mm,5 μm) with linear gradient elution by a mobile phase consisting of methyl alcohol,acetonitrile and 0. 1% acetic acid aqueous solution. All the related substances were characterized by hyphenated chromatographic techniques with accurate mass determination of the ion formula by ESI-TOF / MS,product MS spectra by triple quadrapole mass spectrometer,reference substances comparison and spectroscopic elucidation. Results: Capecitabine and its related substances were completely separated under the established HPLC conditions. Twelve related substances were detected and identified to be two starting materials,three synthetic by-products and seven degradation products. Conclusion: The established method is useful for the identification of related substances in capecitabine. The results obtained are valuable for its manufacturing process control and quality assurance.
Pages: 1902-1910
Year: 2015 Issue: 16
Journal: Chinese Journal of New Drugs
Keyword: capecitabine; related substances; HPLC; LC-TOF/MS; LC-MS /MS;
Abstract: Objective: To develop an LC-MS method for identification of the related substances in capecitabine. Methods: HPLC separation was carried out on a Sepax BR-C18column( 250 mm × 4. 6 mm,5 μm) with linear gradient elution by a mobile phase consisting of methyl alcohol,acetonitrile and 0. 1% acetic acid aqueous solution. All the related substances were characterized by hyphenated chromatographic techniques with accurate mass determination of the ion formula by ESI-TOF / MS,product MS spectra by triple quadrapole mass spectrometer,reference substances comparison and spectroscopic elucidation. Results: Capecitabine and its related substances were completely separated under the established HPLC conditions. Twelve related substances were detected and identified to be two starting materials,three synthetic by-products and seven degradation products. Conclusion: The established method is useful for the identification of related substances in capecitabine. The results obtained are valuable for its manufacturing process control and quality assurance.
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