Research article summary (published 30 Aug 2009):

Determination of digoxin and digitoxin in whole blood.

Full Abstract

A liquid chromatography-tandem mass spectrometry (LC-MS-MS) method has been developed and validated for the determination of digoxin and digitoxin in whole blood samples in autopsy cases. Samples were prepared by liquid-liquid extraction (LLE) with ethyl acetate/heptane/dichloromethane (3:1:1). LC separation was achieved using an Atlantis dC(18)-column (2.1 x 50 mm, 3 microm). The time between injections was 11 min. Mass detection was performed by positive ion mode electrospray LC-MS-MS on the ammonium adducts with two transitions for each analyte and one for the internal standard (digoxin-d(3)). Within-day precision was between 8.3 and 10.8%, between-day precision was between 8.7 and 14.2% and accuracy (bias) was between -17.3 and 11.5%. LOQ was 0.1 nmol/L (0.08 ng/mL), with an accuracy and precision of 19% and -17% (digoxin) and 18% and 3% (digitoxin). Matrix effects ranged from 104 to 117%. Good qualitative correlation with previous findings was achieved for 38 autopsy cases. The median (range, number of cases) B-digitoxin and B-digoxin found with the LC-MS-MS method in this very limited material were 9.3 (3.4-23.8, n = 24) and 5.6 (3.4-26.5, n = 4) nmol/L, respectively.

Author information

Author/s: Oiestad, Elisabeth Leere (EL); Johansen, Unni (U); Stokke Opdal, Mimi (M); Bergan, Stein (S); Christophersen, Asbjørg Solberg (AS);

Affiliation: Norwegian Institute of Public Health, Division of Forensic Toxicology and Drug Abuse, P.O. Box 4404 Nydalen, NO-0403 Oslo, Norway. elisabeth.oiestad(-atsign-)fhi.no

Journal and publication information

Publication Type: Journal Article

Journal: Journal of analytical toxicology (J Anal Toxicol), published in United States. (Language: eng)

Reference: 2009-Sep; vol 33 (issue 7) : pp 372-8

Dates: Created 2009/10/02; Completed 2009/10/27;

PMID: 19796507, status: MEDLINE (last retrieval date: 10/27/2009, IMS Date: )

Sourced from the National Library of Medicine. Abstract text and other information may be subject to copyright.

External Links for this article
(including full text providers, if available):

Click Electronic Full-text Provider Links to see options for finding the electronic full text links to this article. Note there may be a subscription or fee required for access to the full text. See our FAQ for information on finding FREE full text articles.

This article may also be located in paper journal collections available in many libraries. Use the Journal and Publication Information above to find the full article.

MeSH headings (categories)

This article was linked to the MESH Headings shown below.

Autopsy Calibration Cardiotonic Agents - blood Chromatography, High Pressure Liquid Digitoxin - blood Digoxin - blood Humans

Immunoassay Indicators and Reagents Mass Spectrometry Quality Control Reference Standards Reproducibility of Results Solutions

Associated Chemicals: Cardiotonic Agents (0) ; Indicators and Reagents (0) ; Solutions (0) ; Digoxin (20830-75-5) ; Digitoxin (71-63-6)

Related articles

These are the highest related articles currently in the database:

• Determination of the cardiac glycosides digoxin and digitoxin by liquid chromatography combined with isotope-dilution mass spectrometry (LC-IDMS)--a candidate reference measurement procedure. 30 Dec 2002
• LC-MS assay for quantitative determination of cardio glycoside in human blood samples. 12 Jun 2007
• High-performance liquid chromatography-ionspray mass spectrometry for the specific determination of digoxin and some related cardiac glycosides in human plasma. 23 Apr 1997
• Measuring the unbound concentration fails to resolve analytic interferences in digoxin immunoassays. 30 Jul 2008
• Unexpected suppression of total digoxin concentrations by cross-reactants in the microparticle enzyme immunoassay: elimination of interference by monitoring free digoxin concentration. 29 Jun 1998
• Elimination of cardiac glycosides through hemofiltration. 30 Dec 1976
• An improved method for measuring plasma and tissue concentrations of digitalis glycosides. 30 May 1966
• Digitalis and vasoactive drugs. 30 Aug 1981
• [Is it necessary to determine digitalis preparation levels?] 30 Jan 1979
• Application of canine plasma kinetics of digoxin and digitoxin to therapeutic digitalization in the dog. 30 Jul 1973

See 100+ related articles.

Related Article Map

Legend: - FREE Full text Article. - Abstract only. - Title only. More help.

See a large map of 100+ related articles.