Development and validation of a sensitive solid phase extraction/hydrophilic interaction liquid chromatography/mass spectrometry method for the accurate determination of glucosamine in dog plasma.
[en] A sensitive and accurate LC/MS method was developed for the monitoring of glucosamine (GLcN) dog plasmatic concentration. In this scope, relatively low plasmatic concentrations of GLcN were expected, ranging from 50 to 1000ng/mL. Liquid chromatography coupled to simple quadrupole mass spectrometry detection (LC/MS) was selected bringing the selectivity and the sensitivity needed for this application. Additionally, a solid phase extraction (SPE) step was performed to reduce matrix and ion suppression effects. Due to the ionisable character of the compound of interest, a mixed-mode strong cation exchange (Plexa PCX) disposable extraction cartridge (DEC) was selected. The separation was carried out on a Zorbax SB-CN column (5mum, 4.6mm i.d.x250mm), considering hydrophilic interaction liquid chromatography (HILIC). Indeed, the mobile phase was made of methanol and 5mM ammonium hydrogen carbonate buffer at pH 7.5 (95/5, v/v). The detection was led at m/z ratios of 180.0 and 417.0, for GLcN and IS, respectively. Reliability of the results was demonstrated through the validation of the method using an approach based on the accuracy profile allowing managing the risk associated to the use of these methods in routine analysis: it is thus guaranteed that each future result will fall in the +/-30% acceptance limits with a probability of at least 90%. Successful application of the method to a preliminary pharmacokinetic study illustrated the usefulness of the method for pre-clinical studies.
Research center :
CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Hubert, Cédric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Houari, Sabah ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Lecomte, Frédéric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Houbart, Virginie ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
De Bleye, Charlotte ; Université de Liège - ULiège > 2e an. master sc. pharm., fin. approf.
Fillet, Marianne ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Piel, Géraldine ; Université de Liège - ULiège > Département de pharmacie > Pharmacie galénique
Rozet, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Language :
English
Title :
Development and validation of a sensitive solid phase extraction/hydrophilic interaction liquid chromatography/mass spectrometry method for the accurate determination of glucosamine in dog plasma.
Publication date :
2010
Journal title :
Journal of Chromatography. A
ISSN :
0021-9673
eISSN :
1873-3778
Publisher :
Elsevier Science, Amsterdam, Netherlands
Volume :
1217
Pages :
3275-3281
Peer reviewed :
Peer Reviewed verified by ORBi
Name of the research project :
Development and validation of a sensitive solid phase extraction/hydrophilic interaction liquid chromatography/mass spectrometry method for the accurate determination of glucosamine in dog plasma
Funders :
F.R.S.-FNRS - Fonds de la Recherche Scientifique [BE]
Commentary :
Copyright (c) 2010 Elsevier B.V. All rights reserved.
Zhang L., Huang T., Fang X., Li X., Wang Q., Zhang Z., Sha X. J. Chromatogr. B 2006, 842:8.
Zhang X., Amelung W. Soil Biol. Biochem. 1996, 28:1201.
Yu Y., Cai L., Zuo M., Duan G. Ann. Chim. 2005, 95:709.
Huang T.M., Cai L., Yang B., Man-Xiang Z., Yun-Fei S., Geng-Li D. Biomed. Chromatogr. 2006, 20:251.
Roda A., Sabatini L., Barbieri A., Guardigli M., Locatelli M., Violante F.S., Rovati L.C., Persiani S. J. Chromatogr. B 2006, 844:119.
Zhong S., Zhong D., Chen X. J. Chromatogr. B 2007, 854:291.
Nováková L., Vlčková H. Anal. Chim. Acta 2009, 10.1016/j.aca.2009.10.004.
Buck K., Voehringer P., Ferger B. J. Neurosci. Methods 2009, 182:78.
Lu S., Tran B.N., Nelsen J.L., Aldus K.M. J. Chromatogr. B 2009, 877:2499.
Blanchard J. J. Chromatogr. B 1981, 226:455.
Polson C., Sarkar P., Incledon B., Raguvaran V., Grant R. J. Chromatogr. B 2003, 785:263.
Marchi I., Rudaz S., Veuthey J.-L. J. Pharm. Biomed. Anal. 2009, 49:459.
Bonfiglio R., King R.C., Olah T.V., Merkle K. Rapid Commun. Mass Spectrom. 1999, 13:1175.
Annesley T.M. Clin. Chem. 2003, 49:1041.
Skelley A.M., Mathies R.A. J. Chromatogr. A 2006, 1132:304.
Hubert Ph., Nguyen-Huu J.-J., Boulanger B., Chapuzet E., Chiap P., Cohen N., Compagnon P.-A., Dewe W., Feinberg M., Lallier M., Laurentie M., Mercier N., Muzard G., Nivet C., Valat L. J. Pharm. Biomed. Anal. 2004, 36:579.
Hubert Ph., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Chiap P., Cohen N., Compagnon P.A., Dewé W., Feinberg M., Lallier M., Laurentie M., Mercier N., Muzard G., Nivet C., Valat L., Rozet E. J. Pharm. Biomed. Anal. 2007, 45:70.
Hubert Ph., Nguyen-Huu J.J., Boulanger B., Chapuzet E., Cohen N., Compagnon P.-A., Dewé W., Feinberg M., Laurentie M., Mercier N., Muzard G., Valat L., Rozet E. J. Pharm. Biomed. Anal. 2007, 45:82.
Mee R. Technometrics 1984, 26:251.
Guidance for Industry: Bioanalytical Method Validation May 2001, US Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), Center for Biologics Evaluation and Research (CBER).
Viswanathan C.T., Bansal S., Booth B., DeStefano A.J., Rose M.J., Sailstad J., Shah V.P., Skelly J.P., Swann P.G., Weiner R. AAPS J. 2007, 9:E30.
Rozet E., Wascotte V., Lecouturier N., Preat V., Dewe W., Boulanger B., Hubert P. Anal. Chim. Acta 2007, 591:239.
ISO 5725-1, Application of the statistics-accuracy (trueness and precision) of the results and methods of measurement-Part 1: general principles and definitions, International Organization for Standardization (ISO), Geneva, Switzerland (1994).
Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., Boulanger B., Hubert Ph. J. Chromatogr. A 2007, 1158:111.