title: Development and validation of a stability-indicating reversed-phase high performance liquid chromatography method for assay of betamethylepoxide and estimation of its related compounds.
abstract: Betamethylepoxide (16beta-methyl-Delta(1,4)-pregnadiene-9beta-11beta-oxide-17alpha,21-diol-3,20-dione) is a key intermediate for the synthesis of various active pharmaceutical ingredients (APIs) of steroid compounds. A stability-indicating reversed-phase HPLC method for assay of betamethylepoxide and estimation of its related compounds has been developed and validated. This method can accurately quantitate betamethylepoxide in the presence of numerous structurally related compounds (including the alpha-epimer, known as alphamethylepoxide). This method can also adequately separate most of the impurities from each other and estimate their quantities in betamethylepoxide samples. The stability-indicating capability of this method has been demonstrated by adequate separation of the degradation products from betamethylepoxide in stress degraded and aged stability samples. The HPLC column used in the method was a 5 cm YMC Hydrosphere C(18) column (4.6 mm I.D.) and the mobile phase consisted of (A) water and (B) acetonitrile:methanol (8:25, v/v).
authors.affiliation: Global Quality Services-Analytical Sciences, Schering-Plough Corporation, Union, NJ 07083, USA. kangping.xiao@spcorp.com
authors.forename: Kang Ping
authors.initials: KP
authors.lastname: Xiao
authors.forename: Dwight
authors.initials: D
authors.lastname: Chien
authors.forename: Robert
authors.initials: R
authors.lastname: Markovich
authors.forename: Abu M
authors.initials: AM
authors.lastname: Rustum
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004852:Epoxy Compounds / Q000032:analysis*; D011083:Polycyclic Compounds / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D004852:Epoxy Compounds; D011083:Polycyclic Compounds; C524007:betamethylepoxide