High-performance liquid chromatography-ionspray mass spectrometry for the specific determination of digoxin and some related cardiac glycosides in human plasma.
Details
Serval ID
serval:BIB_C900A770E0E8
Type
Article: article from journal or magazin.
Collection
Publications
Institution
Title
High-performance liquid chromatography-ionspray mass spectrometry for the specific determination of digoxin and some related cardiac glycosides in human plasma.
Journal
Journal of Chromatography. B, Biomedical Sciences and Applications
ISSN
1387-2273[print], 1387-2273[linking]
Publication state
Published
Issued date
1997
Volume
692
Number
1
Pages
101-109
Language
english
Abstract
An original method based upon high-performance liquid chromatography coupled to ionspray mass spectrometry (HPLC-ISP-MS) has been developed for the identification and quantification in plasma of several cardiac glycosides, namely digoxin, digitoxin, lanatoside C and acetyldigitoxin. After single-step liquid-liquid extraction by chloroform-2-propanol (95:5, v/v) at pH 9.5 using oleandrin as an internal standard, solutes are separated on a 4 microm NovaPak C18 (Waters) column (150x2.0 mm, I.D.), using a gradient of acetonitrile-2 mM NH4COOH, pH 3 buffer (flow-rate 200 microl/min, post-column split 1:3). Detection is done by a Perkin-Elmer Sciex API-100 mass analyzer equipped with an ISP interface. In most instances the major ion observed is not [M+H]+ as expected, but [M+NH4]+. The mean retention times (min) are: lanatoside C, 5.74; digoxin, 6.00; digitoxin, 8.08, oleandrin, 8.30, acetyldigitoxin, 8.66 and 9.01 (isomers alpha and beta, respectively). The lower limits of detection in single ion monitoring mode range from 0.15 ng/ml (alpha- and beta-acetyldigitoxin) to 0.60 ng/ml (lanatoside C), making the method less sensitive than radioimmunoassay, whereas it is much more specific.
Keywords
Acetyldigitoxins/blood, Cardiac Glycosides/blood, Cardiotonic Agents/blood, Chromatography, High Pressure Liquid, Digitoxin/blood, Digoxin/blood, Gas Chromatography-Mass Spectrometry, Humans, Lanatosides/blood, Ouabain/blood, Sensitivity and Specificity
Pubmed
Create date
19/10/2010 17:13
Last modification date
20/08/2019 16:44