Estimation of impurity profiles of drugs and related materials -: Part XXI.: HPLC/UV/MS study of the impurity profile of ethynodiol diacetate

被引：15

作者：

Babják, M ^{[1
]}

Balogh, G ^{[1
]}

Gazdag, M ^{[1
]}

Görög, S ^{[1
]}

机构：

[1] Gedeon Richter Chem Works Ltd, Chem Works, H-1475 Budapest, Hungary

来源：

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2002年 / 29卷 / 06期

关键词：

ethynodiol diacetate; impurity profiling; HPLC/MS; diode-array UV spectra; NMR spectroscopy;

D O I：

10.1016/S0731-7085(02)00165-6

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

The impurity profile of ethynodiol diacetate was investigated using the HPLC/UV/MS method. Using the slightly modified HPLC method of USP 24 two impurities, earlier isolated by preparative HPLC and investigated by NMR spectroscopy were separated and characterised. The mass spectra amended by the diode-array UV spectra supported the earlier found structures (E and Z isomers of 17alpha-ethinyl-estr-4-ene-3beta,17-diol-3-acetate-17-(3'-acetoxy-2'-butenoate). Another, hitherto not described impurity, 17alpha-ethinyl-estr-4-ene-3beta,17-diol-3-acetate-17-(3-oxo-butanoate) has also been separated and characterised by means of its mass spectrum, NMR and UV spectra. (C) 2002 Published by Elsevier Science B.V.

引用

页码：1153 / 1157

页数：5

共 13 条

[1] ANALYSIS OF STEROIDS .30. SIMULTANEOUS DETERMINATION OF ALPHA-ETHYNODIOL AND BETA-ETHYNODIOL DIACETATE BY HIGH-PRESSURE LIQUID-CHROMATOGRAPHY [J].

GOROG, S ;

HERENYI, B .

JOURNAL OF CHROMATOGRAPHY, 1978, 152 (01) :240-242

[2] Estimation of impurity profiles of drugs and related materials Part 19:: Theme with variations.: Identification of impurities in 3-oxosteroids [J].

Görög, S ;

Babják, M ;

Balogh, G ;

Brlik, J ;

Dravecz, F ;

Gazdag, M ;

Horváth, P ;

Laukó, A ;

Varga, K .

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 1998, 18 (4-5) :511-525

[3] ANALYSIS OF STEROIDS .43. ESTIMATION OF IMPURITY PROFILES OF DRUGS AND RELATED MATERIALS .8. COMBINED APPLICATION OF HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY AND NMR-SPECTROSCOPY IN THE IMPURITY PROFILING OF DRUGS [J].

GOROG, S ;

BALOGH, G ;

GAZDAG, M .

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 1991, 9 (10-12) :829-833

[4] Estimation of impurity profiles of drugs and related materials .14. The role of HPLC/diode-array UV spectroscopy in the identification of minor components (impurities, degradation products, metabolites) in various matrices [J].

Gorog, S ;

Bihari, M ;

Csizer, E ;

Dravetz, F ;

Gazdag, M ;

Herenyi, B .

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 1995, 14 (1-2) :85-92

[5]

Gorog S, 2000, Acta Pharm Hung, V70, P131

[6]

GOROG S, ROLE DIODE ARRAY UV, P252

[7]

GOROG S, 1991, ADV STEROID ANAL 90, P323

[8]

GOROG S, 1994, ULTRAVIOLET VISIBLE, P55

[9]

GOROG S, 2000, IDENTIFICATION DETER, P267

[10]

NIESSEN WMA, 2001, LIQUID CHROMATOGRAPH, P405

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