Integrated on-line sample clean-up using cation exchange restricted access sorbent for the LC determination of atropine in human plasma coupled to UV detection
[en] A new, simple and fully automated liquid chromatographic (LC) method with UV detection has been developed for the direct determination of atropine in plasma. Sample clean-up was based on the use of cation exchange restricted access material (RAM) in a pre-column, coupled to LC by means of a column switching system. After direct injection of a 200 microl-volume of plasma sample, the biological matrix was washed out for 10 min using a washing liquid composed of 2 mM lithium perchlorate adjusted to pH 3.0 and methanol (97:3; v/v). By rotation of the switching valve, atropine was then eluted in the back-flush mode for 2 min and transferred to the analytical column packed with octadecyl silica by the LC mobile phase constituted of a mixture of acetonitrile and potassium phosphate buffer (pH 3.0; 50 mM) containing 2 mM sodium heptanesulfonate (16:84; v/v). The UV detection was performed at 220 nm. The method was validated according to a new approach based on accuracy profile over a concentration range from 25 ng/ml, corresponding to the limit of quantitation, to 1000 ng/ml. The method was then applied for the determination of atropine in plasma after intravenous administration to hospitalised patients.
Crommen, Jacques ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Chiap, Patrice ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Language :
English
Title :
Integrated on-line sample clean-up using cation exchange restricted access sorbent for the LC determination of atropine in human plasma coupled to UV detection
Publication date :
04 January 2005
Journal title :
Journal of Pharmaceutical and Biomedical Analysis
ISSN :
0731-7085
eISSN :
1873-264X
Publisher :
Pergamon-Elsevier Science Ltd, Oxford, United Kingdom
A. El Mahjoub, and C. Staub J. Chromatogr. B 742 2000 381 390
C. Schäfer, and D. Lubda J. Chromatogr. A 909 2001 73 78
G. Lambrecht, T. Kraushofer, K. Stoschitzky, and W. Lindner J. Chromatogr. B 740 2000 219 226
P. Chiap, O. Rbeida, B. Christiaens, Ph. Hubert, D. Lubda, K.-S. Boos, and J. Crommen J. Chromatogr. A 975 2002 145 155
O. Rbeida, B. Christiaens, P. Chiap, Ph. Hubert, D. Lubda, K.-S. Boos, and J. Crommen J. Pharm. Biomed. Anal. 32 2003 829 838
Z. Yu, and D. Westerlund J. Chromatogr. A 725 1996 137 147
Ph. Hubert, J.J. Nguyen-Huu, B. Boulanger, E. Chapuzet, P. Chiap, N. Cohen, P.A. Compagnon, W. Dewé, M. Feinberg, M. Lallier, M. Laurentie, N. Mercier, J.C. Nivet, G. Muzard, and L. Valat STP Pharm. Pract. 13 2003 101 138
U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), Guidance for Industry, Bioanalytical Method Validation, 2001.
Ph. Hubert, P. Chiap, J. Crommen, B. Boulanger, E. Chapuzet, N. Mercier, S. Bervoas-Martin, P. Chevalier, D. Grandjean, P. Lagorce, M. Lallier, M.C. Laparra, M. Laurentie, and J.C. Nivet Anal. Chim. Acta 391 1999 135 148
I. Onnen, G. Barrier, S. Sureau, and G. Olive Eur. J. Clin. Pharmacol. 15 1979 443 451
P. Clair, K. Wiberg, I. Granelli, I.C. Bratt, and G. Blanchet Eur. J. Pharm. Sci. 9 2000 259 263
E.A. Michaelson, S.M. Schneider, and T.G. Martin Vet. Hum. Toxicol. 33 1991 360 369