双氢青蒿素的柱上差向异构化：一种克服《国际药典》专论缺点的有效分析方法。
On-column epimerization of dihydroartemisinin: an effective analytical approach to overcome the shortcomings of the International Pharmacopoeia monograph.
作者信息
Cabri Walter, Ciogli Alessia, D'Acquarica Ilaria, Di Mattia Michela, Galletti Bruno, Gasparrini Francesco, Giorgi Fabrizio, Lalli Silvana, Pierini Marco, Simone Patrizia
机构信息
Analytical Development, R&D Department, sigma-tau S.p.A., Via Pontina km 30,400, 00040 Pomezia, Italy.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Nov 1;875(1):180-91. doi: 10.1016/j.jchromb.2008.06.037.
We developed a cryo-HPLC/UV method for the simultaneous determination of artemisinin (1), alpha-dihydroartemisinin (2alpha), beta-dihydroartemisinin (2beta), 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 microm 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.
我们从国际药典中有关双氢青蒿素的专论出发，开发了一种低温高效液相色谱/紫外检测法，用于同时测定青蒿素（1）、α-双氢青蒿素（2α）、β-双氢青蒿素（2β）以及双氢青蒿素的一种常见热分解产物（命名为二酮醛，3）。该方法首次考虑了2的柱上差向异构化过程。在反相条件下，于Symmetry C18柱（粒径3.5微米）上进行色谱分离，流动相为乙腈-水（60:40，v/v），流速为0.60 - 1.00毫升/分钟，在低波长（λ = 210纳米）处进行紫外检测。基于在不同温度下进行的非对映选择性动态高效液相色谱（DHPLC）研究，选择了低温（T = 0 - 10℃），旨在确定能够使柱上互变过程最小化的最佳实验条件。
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