We developed a cryo-HPLC/UV method for the simultaneous determination of artemisinin (1), alpha-dihydroartemisinin (2 alpha), beta-dihydroartemisinin (2 beta). and a ubiquitous thermal decomposition product of 2 (designated as diketoaldehyde, 3), starting from the International Pharmacopoeia monograph on dihydroartemisinin. The method takes for the first time the on-column epimerization process of 2 into consideration. Chromatographic separation was obtained under reversed-phase conditions on a Symmetry C18 column (3.5 mu m particle size) with a mobile phase consisting of acetonitrile-water 60:40 (v/v), delivered at 0.60-1.00 ml/min flow-rates, with ultraviolet detection at low wavelength (lambda = 210 nm). Low temperatures (T=0-10 degrees C) were selected on the grounds of a diastereoselective dynamic HPLC (DHPLC) study performed at different temperatures, aimed at identifying the best experimental conditions capable of minimizing the on-column interconversion process. (c) 2008 Elsevier B.V. All rights reserved.
On-column epimerization of dihydroartemisinin: An effective analytical approach to overcome the shortcomings of the International Pharmacopoeia monograph / Cabri W; Ciogli A; D'Acquarica I; Di Mattia M; Galletti B; Gasparrini F; Giorgi F; Lalli S; Pierini M; Simone P. - In: JOURNAL OF CHROMATOGRAPHY. B. - ISSN 1570-0232. - ELETTRONICO. - 875:1(2008), pp. 180-191. [10.1016/j.jchromb.2008.06.037]
On-column epimerization of dihydroartemisinin: An effective analytical approach to overcome the shortcomings of the International Pharmacopoeia monograph
Cabri W;
2008
Abstract
We developed a cryo-HPLC/UV method for the simultaneous determination of artemisinin (1), alpha-dihydroartemisinin (2 alpha), beta-dihydroartemisinin (2 beta). and a ubiquitous thermal decomposition product of 2 (designated as diketoaldehyde, 3), starting from the International Pharmacopoeia monograph on dihydroartemisinin. The method takes for the first time the on-column epimerization process of 2 into consideration. Chromatographic separation was obtained under reversed-phase conditions on a Symmetry C18 column (3.5 mu m particle size) with a mobile phase consisting of acetonitrile-water 60:40 (v/v), delivered at 0.60-1.00 ml/min flow-rates, with ultraviolet detection at low wavelength (lambda = 210 nm). Low temperatures (T=0-10 degrees C) were selected on the grounds of a diastereoselective dynamic HPLC (DHPLC) study performed at different temperatures, aimed at identifying the best experimental conditions capable of minimizing the on-column interconversion process. (c) 2008 Elsevier B.V. All rights reserved.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
