Identification, characterization and HPLC quantification of process-related impurities in Trelagliptin succinate bulk drug: Six identified as new compounds
| Autor: | Liang Zou, Lei Liu, Wenkai Hui, Pingkai Ouyang, Qiaogen Zou, Hui Zhang, Lili Sun |
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| Rok vydání: | 2016 |
| Předmět: |
Magnetic Resonance Spectroscopy
Spectrophotometry Infrared Potassium Clinical Biochemistry Pharmaceutical Science chemistry.chemical_element Tandem mass spectrometry Sensitivity and Specificity 01 natural sciences Analytical Chemistry chemistry.chemical_compound Drug Stability Tandem Mass Spectrometry Impurity Liquid chromatography–mass spectrometry Drug Discovery Uracil Acetonitrile Triethylamine Chromatography High Pressure Liquid Spectroscopy Chromatography 010405 organic chemistry Chemistry 010401 analytical chemistry Nuclear magnetic resonance spectroscopy Phosphate 0104 chemical sciences Drug Contamination |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 128:18-27 |
| ISSN: | 0731-7085 |
| Popis: | A sensitive, selective and stability indicating reversed-phase LC method was developed for the determination of process related impurities of Trelagliptin succinate in bulk drug. Six impurities were identified by LC-MS. Further, their structures were characterized and confirmed utilizing LC-MS/MS, IR and NMR spectral data. The most probable mechanisms for the formation of these impurities were also discussed. To the best of our knowledge, six structures among these impurities are new compounds and have not been reported previously. The superior separation was achieved on an InertSustain C18 (250mm×4.6mm, 5μm) column in a gradient mixture of acetonitrile and 20mmol potassium dihydrogen phosphate with 0.25% triethylamine (pH adjusted to 3.5 with phosphate acid). The method was validated as per regulatory guidelines to demonstrate system suitability, specificity, sensitivity, linearity, robustness, and stability. |
| Databáze: | OpenAIRE |
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