[Analysis of steroids. Part 40. Isolation and identification of unusual impurities in ethynodiol diacetate].
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.
Görög
S
S
Richter Gedeon Vegyészeti Gyár Rt., Budapest.
Halmos
Z
Z
Herényi
B
B
Georgakis
A
A
Balogh
G
G
Csizér
E
E
Tuba
Z
Z
D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004340:Drug Contamination; D005040:Ethynodiol Diacetate / Q000302:isolation & purification*
D005040:Ethynodiol Diacetate
Adatok a szteránvázas vegyületek analitikájához 40. Etinodiol-diacetát szokatlan szennyezéseinek izolálása és szerkezetük felderítése.