title: Development and validation of a new stability indicating reversed phase liquid chromatographic method for the determination of prednisolone acetate and impurities in an ophthalmic suspension.
abstract: A new stability indicating reversed phase high performance liquid chromatography (RP-HPLC) method was developed and validated under current International Conference of Harmonisation (ICH) guidance for the determination of prednisolone acetate (PAC) and impurities in an ophthalmic suspension. The developed method is presented as an alternative to a modified version of the current RP-HPLC method described in the USP monograph for the assay of PAC in an ophthalmic suspension. Along with the assay of PAC, the new method is also capable of identifying and quantifying eight selected PAC impurities and degradation products in an ophthalmic suspension. Using an Agilent Poroshell 120 EC-C18 100 mm × 4.6mm (dp: 2.7 μm) column set to 60°C with step gradient elution generated using mobile phase A: acetonitrile/water (10:90) (v/v) and mobile phase B: acetonitrile delivered at 1.2 mL min(-1), all peaks of interest are eluted in 33 min with resolution of 1.5 between the critical pairs. The developed method was validated for PAC and impurities to ICH recommendations for accuracy, linearity, precision (repeatability), limit of detection, limit of quantitation, robustness and specificity.
authors.affiliation: Allergan Pharmaceuticals, Westport, Mayo, Ireland; Irish Separation Science Cluster (ISSC), National Centre for Sensor Research, Dublin City University, Glasnevin, Dublin 9, Ireland. Electronic address: marley_adrian@allergan.com.
authors.forename: Adrian
authors.initials: A
authors.lastname: Marley
authors.affiliation: Irish Separation Science Cluster (ISSC), National Centre for Sensor Research, Dublin City University, Glasnevin, Dublin 9, Ireland.
authors.forename: Apryll M
authors.initials: AM
authors.lastname: Stalcup
authors.affiliation: Pharmaceutical and Molecular Biotechnology Research Centre (PMBRC), Department of Chemical and Life Sciences, Waterford Institute of Technology, Waterford, Ireland. Electronic address: dconnolly@wit.ie.
authors.forename: Damian
authors.initials: D
authors.lastname: Connolly
mesh_terms: D056148:Chromatography, Reverse-Phase / Q000379:methods*; D004340:Drug Contamination; D004355:Drug Stability; D011239:Prednisolone / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D013535:Suspensions
chemical_list: D013535:Suspensions; C009935:prednisolone acetate; D011239:Prednisolone
keywords: Core–shell particles; Impurity analysis; Ophthalmic suspension; Prednisolone acetate; Reversed-phase high performance liquid chromatography