Determination of clavulanic acid in calf plasma by liquid chromatography tandem mass spectrometry

A method for the quantification of clavulanic acid in calf plasma using high‐performance liquid chromatography combined with electrospray ionization (ESI) mass spectrometry, operating in the negative ionization mode (LC‐MS/MS), is presented. Sample preparation includes a simple and fast deproteiniza...

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Bibliographic Details
Published in:Journal of mass spectrometry. Vol. 41; no. 11; pp. 1414 - 1420
Main Authors: Reyns, Tim, De Baere, Siegrid, Croubels, Siska, De Backer, Patrick
Format: Journal Article
Language:English
Published: Chichester, UK John Wiley & Sons, Ltd 01.11.2006
Wiley
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ISSN:1076-5174, 1096-9888
Online Access:Get full text
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Summary:A method for the quantification of clavulanic acid in calf plasma using high‐performance liquid chromatography combined with electrospray ionization (ESI) mass spectrometry, operating in the negative ionization mode (LC‐MS/MS), is presented. Sample preparation includes a simple and fast deproteinization with acetonitrile and a back‐extraction of the acetonitrile with dichloromethane. Chromatography is performed on a reversed‐phase PLRP‐S polymeric column using 0.05% formic acid in water and acetonitrile. The limit of quantification is 25 ng/ml, which is lower than other published methods using ultraviolet (UV), fluorimetric or mass spectrometric detection. The limit of detection is calculated to be 3.5 ng/ml. The stability of clavulanic acid was demonstrated according to The Guidelines of Bioanalytical Method Validation of The Food and Drug Administration (FDA): freeze and thaw stability, short‐term stability, long‐term stability, stock solution stability and postpreparative stability. The method is used in a pharmacokinetic and bioequivalence study of amoxycillin/clavulanic acid formulations in calves. Copyright © 2006 John Wiley & Sons, Ltd.
Bibliography:ark:/67375/WNG-2WNXMRFX-2
ArticleID:JMS1106
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ISSN:1076-5174
1096-9888
DOI:10.1002/jms.1106