Isolation and identification of unknown impurities of alogliptin benzoate

ZHANG Yilun; ZHAO Xinyi; DONG Shubo; DONG Chao; SHEN Wenbin; DONG Haijuan

doi:10.11665/j.issn.1000-5048.20200415

Journal of China Pharmaceutical University > 2020 > 51(4): 488-493. > DOI: 10.11665/j.issn.1000-5048.20200415

ZHANG Yilun, ZHAO Xinyi, DONG Shubo, DONG Chao, SHEN Wenbin, DONG Haijuan. Isolation and identification of unknown impurities of alogliptin benzoate[J]. Journal of China Pharmaceutical University, 2020, 51(4): 488-493. DOI: 10.11665/j.issn.1000-5048.20200415

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Isolation and identification of unknown impurities of alogliptin benzoate

1.
Institute of Pharmaceutical Sciences, China Pharmaceutical University, Nanjing 210009
2.
Jiangsu Deyuan Pharmaceutical Co.,Ltd., Lianyungang 222000, China

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Received Date: June 04, 2020

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By silica gel column chromatography, solvent extraction and preparative high performance liquid chromatography (HPLC), four new related substance were isolated and purified from the mass production and preparation process of alogliptin benzoate. Then it was analyzed and confirmed by various spectrum identification methods such as nuclear magnetic resonance (NMR) spectroscopy, high-resolution mass spectrometry (HR-MS) and Fourier-transform infrared spectroscopy (FTIR) according to its physical and chemical properties. The chemical structures of the four related substances produced in each step of the synthesis process of alogliptin benzoate were determined, and they were named as impurities L, M, T, and V. These four related substances were new impurities which were found for the first time. The isolation and identification of these impurities are of great importance to the quality control of alogliptin benzoate, and the optimization of manufacturing process.
- alogliptin benzoate,
- type 2 diabetes,
- DPP-IV inhibitor,
- related substance,
- isolation and identification

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Isolation and identification of unknown impurities of alogliptin benzoate

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