title: [Analysis of steroids. Part 40. Isolation and identification of unusual impurities in ethynodiol diacetate].
abstract: In the course of the estimation of the impurity profile of ethynodiol diacetate, in addition to common impurities such as norethisterone acetate, ethynodiol-3-acetate and alpha-ethynodiol diacetate, two unknown impurities were detected by analytical reversed phase HPLC (C-18 silica and 80% aq. methanol as the eluent) and isolated by normal phase preparative HPLC (silica and 98:2 mixture of hexane and 2-propanol as the eluent). The 1H- and 13C-NMR spectra of the isolated impurities revealed that their structures could be characterized as the E and Z isomers of an analogue of EDDA containing "trimerised acetyl" group at the 17-hydroxy group (structures 4 and 4a). These structures were in good agreement with the extended UV spectra of the impurities and the mass spectra with the m/z 438 peak which can be derived from 4 and 4a by the loss of ketene.
authors.affiliation: Richter Gedeon Vegyészeti Gyár Rt., Budapest.
authors.forename: S
authors.initials: S
authors.lastname: Görög
authors.forename: Z
authors.initials: Z
authors.lastname: Halmos
authors.forename: B
authors.initials: B
authors.lastname: Herényi
authors.forename: A
authors.initials: A
authors.lastname: Georgakis
authors.forename: G
authors.initials: G
authors.lastname: Balogh
authors.forename: E
authors.initials: E
authors.lastname: Csizér
authors.forename: Z
authors.initials: Z
authors.lastname: Tuba
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004340:Drug Contamination; D005040:Ethynodiol Diacetate / Q000302:isolation & purification*
chemical_list: D005040:Ethynodiol Diacetate
vernacular_title: Adatok a szteránvázas vegyületek analitikájához 40. Etinodiol-diacetát szokatlan szennyezéseinek izolálása és szerkezetük felderítése.