Reference : Application of a new optimization strategy for the separation of tertiary alkaloids e...
Scientific journals : Article
Physical, chemical, mathematical & earth Sciences : Chemistry
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/89785
Application of a new optimization strategy for the separation of tertiary alkaloids extracted from Strychnos usambarensis leaves
English
Nistor, Iolanda mailto [Université de Liège - ULg > > > Form. doc. sc. bioméd. & pharma.]
Cao, Martine [Université de Liège - ULg > Département de pharmacie > Pharmacognosie >]
Debrus, Benjamin [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Lebrun, Pierre [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Lecomte, Frédéric [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Rozet, Eric [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Angenot, Luc [Université de Liège - ULg > Département de pharmacie > Département de pharmacie >]
Frederich, Michel [Université de Liège - ULg > Département de pharmacie > Pharmacognosie >]
Oprean, Radu [Université de Médicine et Pharmacie "Iuliu Hatieganu" Cluj-Napoca > Pharmacie > Chimie Analytique > >]
Hubert, Philippe [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
2011
Journal of Pharmaceutical & Biomedical Analysis
Elsevier Science
56
30-37
Yes (verified by ORBi)
International
0731-7085
1873-264X
Oxford
United Kingdom
[en] HPLC-UV ; independent component analysis ; design space ; design of experiment ; Strychnos usambarensis
[en] The HPLC separation of six alkaloids extracted from Strychnos usambarensis leaves has been
developed and optimized by means of a powerful methodology for modelling chromatographic
responses, based on three steps, i.e. design of experiments (DoE), independent component analysis (ICA) and design space (DS). This study was the first application of a new optimization strategy to a complex natural matrix. The compounds separated are the isomers isostrychnopentamine and strychnopentamine, 10-hydroxyusambarine and 11-hydroxyusambarine, also strychnophylline and strychnofoline. Three LC parameters have been optimized using a multifactorial design comprising 29 experiments that includes 2 center point replicates. The parameters were the percentage of organic modifiers used at the beginning of a gradient profile which consisted in different proportions of methanol (MeOH) and acetonitrile (MeCN), the gradient time to reach 70% of organic modifiers starting from the initial percentage and the percentage of MeCN found in the mobile phase. Subsequent to the experimental design application, predictive multilinear models were developed and used in order to provide optimal analytical conditions. The optimum assay conditions were: methanol/acetonitrile-sodium pentane
sulfonate (pH 2.2; 7.5 mM) (33.4:66.6, v/v) at a mobile phase flow rate of 1mL/min during a 40.6
minutes gradient time. The initial organic phase contained 3.7% MeCN and 96.3% MeOH. The method showed good agreement between the experimental data and predictive value throughout the studied parameters space. Improvement of the analysis time and optimized separation for the compounds of interest was possible due to the original and powerful tools applied. Finally, this study permitted the acquisition of isomers profiles allowing the identification of the optimal collecting period of Strychnos usambarensis.
Wallonie Bruxelles International
Researchers ; Professionals ; Students ; Others
http://hdl.handle.net/2268/89785
10.1016/j.jpba.2011.04.027
http://www.sciencedirect.com/science/article/pii/S073170851100238X

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