Determination of Degradation Products of Doxercalciferol by Solid-Phase Extraction and Reversed-Phase HPLC

• Published in: Journal of chromatographic science Vol. 52; no. 6; pp. 520 - 525
• Main Authors: Simonzadeh, Ninus, Ronsen, Bruce, Upadhyaya, Subhash, Wilkinson, Erik, Kanesvaran, Kiran, Patel, Vijay, Bendale, Pravin
• Format: Journal Article
• Language: English
• Published: United States Oxford University Press 01.07.2014
• Subjects: Chromatography; Chromatography, High Pressure Liquid - methods; Chromatography, Reverse-Phase - methods; Degradation; Ergocalciferols - analysis; Ergocalciferols - chemistry; Extraction; Formulations; Impurities; Ingredients; Reproducibility of Results; Solid Phase Extraction - methods; Vitamins
• ISSN: 0021-9665; 1945-239X
• DOI: 10.1093/chromsci/bmt073

In the current study, injectable formulations containing Doxercalciferol as the active pharmaceutical ingredient are analyzed by using gradient-elution high-performance liquid chromatography with ultraviolet detection. Various related impurities and degradants are quantified by using solid-phase extraction (SPE) for enhanced sensitivity. The assay of possible related impurities and Doxercalciferol analogues present at trace quantities is performed by using Trans-1-α-hydroxy vitamin D2 (Doxercalciferol related degradation product/Impurity B) as standard and 1-β-hydroxy vitamin D2 (Doxercalciferol related degradation product/Impurity C) as internal standards for the SPE study. The current method is shown to be stability-indicating and free from interferences from any of the formulation excipients and potential degradation products and impurities. The validated method is shown to be reproducible, accurate, sensitive and selective.