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Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry

A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (2.1 × 100; 1.8 μm), at 35°C. The mobile phase...

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Detalles Bibliográficos
Autores principales: Melo, Paula, Machado, Rita, Teixeira, Helena M.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Hindawi Publishing Corporation 2012
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3132508/
https://www.ncbi.nlm.nih.gov/pubmed/21776271
http://dx.doi.org/10.1155/2012/975824
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author Melo, Paula
Machado, Rita
Teixeira, Helena M.
author_facet Melo, Paula
Machado, Rita
Teixeira, Helena M.
author_sort Melo, Paula
collection PubMed
description A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (2.1 × 100; 1.8 μm), at 35°C. The mobile phase consisted of acetonitrile (70%) and ammonium formate 5 mM (30%). Total run time was 1.5 min operating at isocratic mode with a flow rate of 0.3 mL/min. Mass spectrometry detection was performed by positive mode electrospray, on the ammonium adducts with two transitions for each analyte and one for the IS (d(3)-digoxin). The method proved to be specific and linear over the range (0.3–10) ng/mL. This technique also showed high sensitivity with a 0.09 ng/mL LOD and a 0.28 ng/mL LOQ, for both substances. Percentage recovery ranged from 83 to 100% for digoxin and from 62 to 94% for metildigoxin. The intra- and interday precision CV were ≤10%.
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spelling pubmed-31325082011-07-20 Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry Melo, Paula Machado, Rita Teixeira, Helena M. Int J Anal Chem Research Article A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (2.1 × 100; 1.8 μm), at 35°C. The mobile phase consisted of acetonitrile (70%) and ammonium formate 5 mM (30%). Total run time was 1.5 min operating at isocratic mode with a flow rate of 0.3 mL/min. Mass spectrometry detection was performed by positive mode electrospray, on the ammonium adducts with two transitions for each analyte and one for the IS (d(3)-digoxin). The method proved to be specific and linear over the range (0.3–10) ng/mL. This technique also showed high sensitivity with a 0.09 ng/mL LOD and a 0.28 ng/mL LOQ, for both substances. Percentage recovery ranged from 83 to 100% for digoxin and from 62 to 94% for metildigoxin. The intra- and interday precision CV were ≤10%. Hindawi Publishing Corporation 2012 2011-06-22 /pmc/articles/PMC3132508/ /pubmed/21776271 http://dx.doi.org/10.1155/2012/975824 Text en Copyright © 2012 Paula Melo et al. https://creativecommons.org/licenses/by/3.0/ This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
spellingShingle Research Article
Melo, Paula
Machado, Rita
Teixeira, Helena M.
Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
title Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
title_full Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
title_fullStr Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
title_full_unstemmed Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
title_short Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
title_sort analysis of digoxin and metildigoxin in whole blood using solid-phase extraction and liquid chromatography tandem mass spectrometry
topic Research Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3132508/
https://www.ncbi.nlm.nih.gov/pubmed/21776271
http://dx.doi.org/10.1155/2012/975824
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