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Titolo:
Simultaneous determination of a novel thrombin inhibitor and its two metabolites in human plasma by liquid chromatography/tandem mass spectrometry
Autore:
Riffel, KA; Song, HC; Gu, XM; Yan, K; Lo, MW;
Indirizzi:
Merck Res Labs, Dept Drug Metab, W Point, PA 19486 USA Merck Res Labs W Point PA USA 19486 ept Drug Metab, W Point, PA 19486 USA
Titolo Testata:
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
fascicolo: 2-3, volume: 23, anno: 2000,
pagine: 607 - 616
SICI:
0731-7085(20000815)23:2-3<607:SDOANT>2.0.ZU;2-O
Fonte:
ISI
Lingua:
ENG
Soggetto:
IDENTIFICATION;
Keywords:
thrombin inhibitor; LC/MS/MS; liquid-liquid extraction;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Life Sciences
Citazioni:
10
Recensione:
Indirizzi per estratti:
Indirizzo: Riffel, KA Merck Res Labs, Dept Drug Metab, W Point, PA 19486 USA Merck Res Labs W Point PA USA 19486 tab, W Point, PA 19486 USA
Citazione:
K.A. Riffel et al., "Simultaneous determination of a novel thrombin inhibitor and its two metabolites in human plasma by liquid chromatography/tandem mass spectrometry", J PHARM B, 23(2-3), 2000, pp. 607-616

Abstract

I, 3-(2-phenethylamino)-6-methyl-1-(2-amino-6-methyl-5-methylene-carboxamidomethylpyridinyl)-pyrazinone dihydrochloride monohydrate, is a potent, orally active thrombin inhibitor. The compound also has two metabolites which have been shown to have thrombin inhibitory activity: benzylic alcohol M3 metabolite (II) and hydroxymethylpyrazinone M7 metabolite (III). A liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the simultaneous determination of I and its two metabolites in human plasma has successfully been developed. The method consists of treating 0.5 mi plasma with 2 N NaOH and extracting I, II, III and internal standard (IV) with ethyl acetate:methyl-t-butyl ether (1:3,v/v). The analytes were then back-extracted into2% formic acid. The analytes were chromatographed by high performance liquid chromatography (HPLC) and detected by MS/MS. Positive ionization was used on a heated nebulizer probe monitoring precursor-->product ion combinations in multiple reaction monitoring mode. The linear range is 0.5-1000 nM for I and III and 0.75-1000 nM for II. Recoveries were 88, 74, 78 and 102.1% for I, II and III and the internal standard, respectively in human plasma. Intraday variation using this method was less than or equal to 7.9%; for I,less than or equal to 9.0% for II and less than or equal to 9.5% for III across the standard curve range, This method exhibits good linearity and reproducibility for the three analytes. (C) 2000 Elsevier Science B.V. All rights reserved.

ASDD Area Sistemi Dipartimentali e Documentali, Università di Bologna, Catalogo delle riviste ed altri periodici
Documento generato il 08/08/20 alle ore 18:03:31