Separation and simultaneous estimation of enantiomers and Diastereomers of muscarinic receptor antagonist Solifenacin using stability‐indicating Normal‐phase HPLC technique with chiral stationary phase amylose tris‐(3,5‐dimethylphenylcarbamate)
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Published:2023-11-23
Issue:2
Volume:36
Page:
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ISSN:0899-0042
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Container-title:Chirality
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language:en
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Short-container-title:Chirality
Author:
Vadagam Niroja1ORCID,
Haridasyam Sharath Babu1ORCID,
Venkatanarayana Muvvala1ORCID,
Lakka Narasimha S.2ORCID,
Chinnakadoori Sanjeeva R.3ORCID
Affiliation:
1. Department of Chemistry GITAM School of Science (Deemed to be University) Hyderabad Telangana India
2. Research & Development and Quality Operations InvaHealth Inc. Cranbury New Jersey USA
3. Analytical Research and Development Amneal Pharmaceuticals. Piscataway New Jersey USA
Abstract
AbstractThe R,S‐enantiomer impurity and diastereomer impurities (S,S‐isomer and R,R‐isomer) of the solifenacin (S,R‐enantiomer) were effectively separated and quantified simultaneously utilizing normal‐phase high‐performance liquid chromatography with a chiral stationary phase consisting of amylose tris (3,5‐dimethylphenylcarbamate) coated on silica‐gel (Chiralpak, AD‐H). The enantiomeric and stereo‐selective separation was achieved within a run time of 35 minutes using a mobile phase of ‘n‐hexane, ethanol, and diethylamine’ in an isocratic elution mode with a detection wavelength of 220 nm. The validation attributes assessed were accuracy (which showed excellent recoveries between 97.5% and 100.4%) and linearity (which was proven in the range of 0.081–1.275 μg.mL−1, with a linear regression of 0.999). The stress testing experiments proved that the developed methodology by the HPLC technique has stability‐indicating characteristics, as all closely eluting peak pairs were separated well with a resolution of 2.3 and without any interference. The proposed methodology was highly efficient in separating and simultaneously determining the chiral impurities (enantiomers and diastereomers) of the solifenacin in the release and stability sample analyses of drug substances and tablets in pharmaceutical formulations.
Subject
Organic Chemistry,Spectroscopy,Drug Discovery,Pharmacology,Catalysis,Analytical Chemistry
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