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Development of Stability Indicating HPLC–UV Method for Determination of Daclatasvir and Characterization of Forced Degradation Products

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Abstract

A simple and sensitive stability indicating high performance liquid chromatography method was developed for quantification of Daclatasvir hydrochloride in bulk and tablet dosage forms. The analysis was performed on water symmetry analytical column (150 mm × 3.9 mm, 5 µm), packing octyl silica (Si-[CH2]7-CH3) C8. Mobile phase containing potassium phosphate buffer (pH 2.0) and acetonitrile (38: 62) v/v was used at flow rate 0.7 mL min−1 for isocratic elution. Detection was performed on 304 nm using UV detector. The method was validated appropriately according to the requirements of United State Pharmacopeia and International Conference on Harmonization guideline Q2 (R1). Recovery, precision, linearity and specificity of the method were assured. The correlation coefficient for linearity ranged from 2 to 24 µg mL−1 was (r > 0.9999). The limits of detection and quantification of Daclatasvir were 0.08 and 0.28 µg mL−1, respectively. Stability studies of Daclatasvir were performed under various stressed conditions, i.e., hydrolytic (acidic, basic and neutral), oxidation, photolytic and thermal conditions, according to International Conference on Harmonization Q1A (R2) and QIB Guidelines. The degradation products were resolved using proposed method and further characterized by MS, NMR and IR spectroscopic analyses. The proposed method was successfully applied to assay determination of bulk drugs and tablet dosage forms.

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Acknowledgments

The authors are thankful to Genome Pharmaceuticals for providing generic products, reference standards and for their support in this work.

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  1. Institute of Chemical Sciences, University of Peshawar, Peshawar, Khyber Pakhtunkhwa, 25120, Pakistan

    Bakht Zaman & Waseem Hassan

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  1. Bakht Zaman
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  2. Waseem Hassan
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Correspondence to Waseem Hassan.

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Zaman, B., Hassan, W. Development of Stability Indicating HPLC–UV Method for Determination of Daclatasvir and Characterization of Forced Degradation Products. Chromatographia 81, 785–797 (2018). https://doi.org/10.1007/s10337-018-3503-7

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  • DOI: https://doi.org/10.1007/s10337-018-3503-7

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