Reference : APPLICATION OF DESIGN OF EXPERIMENTS AND DESIGN SPACE METHODOLOGY FOR THE HPLC-UV SEPARA...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/109321
APPLICATION OF DESIGN OF EXPERIMENTS AND DESIGN SPACE METHODOLOGY FOR THE HPLC-UV SEPARATION OPTIMIZATION OF APORPHINE ALKALOIDS FROM LEAVES OF Spirospermum penduliflorum THOUARS
English
Rafamantanana, Mamy [ > > ]
Debrus, Benjamin mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Raoelison, Guy [ > > ]
Rozet, Eric mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Lebrun, Pierre mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Uverg-Ratsimamanga, S. [ > > ]
Hubert, Philippe mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Quetin-Leclercq, J. [ > > ]
2012
Journal of Pharmaceutical & Biomedical Analysis
Elsevier Science
62
23-32
Yes (verified by ORBi)
International
0731-7085
1873-264X
Oxford
United Kingdom
[en] Design of experiments ; Spirospermum penduliflorum ; quantitative determination ; validation ; dicentrine ; design-space
[en] Spirospermum penduliflorum Thouars (Menispermaceae) is an endemic species of Madagascar traditionally used as vasorelaxant. Recently, two aporphine alkaloids known to possess antihypertensive activity (dicentrine and neolitsine) were isolated and identified from the leaves of this plant. In the present study, a HPLC-UV method allowing the separation of all alkaloids and the quantification of dicentrine in the alkaloidic extract of leaves was developed using design of experiments and design space methodology. Three common chromatographic parameters (i.e. the mobile phase pH, the initial proportion of methanol and the gradient slope) were selected to construct a full factorial design of 36 experimental conditions. The times at the beginning, the apex (i.e. the retention time) and the end of each peak were recorded and modelled by multiple linear equations. The corresponding residuals were normally distributed which confirmed that the models can be used for the prediction of the retention times and to optimize the separation. The optimal separation was predicted at pH 3, with a gradient starting at 32% of methanol and a gradient slope of 0.42%/min. Good agreement was obtained between predicted and experimental chromatograms. The method was also validated using total error concept. Using the accuracy profile approach, validation results gave a LOD and LOQ for dicentrine of 3 µg/ml and 10 µg/ml, respectively. A relative standard deviation for intermediate precision lower than 10% was obtained. This method was found to provide accurate results in the concentration range of 10 µg/ml to 75 µg/ml of dicentrine and is suitable for routine analysis.
Researchers ; Professionals ; Students
http://hdl.handle.net/2268/109321

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