Department of Natural Medicinal Chemistry, China Pharmaceutical University, Nanjing, PR China.
J Sep Sci. 2011 Apr;34(7):806-11. doi: 10.1002/jssc.201000779. Epub 2011 Mar 8.
To isolate atropine and scopolamine from Daturae metelis Flos, three different elution modes have been applied in pH-zone-refining counter-current chromatography. These separations were performed with a two-phase solvent system composed of ethyl acetate/n-butanol/water (4:1:5 v/v) with 0.50% triethylamine in the organic phase and 0.15% hydrochloric acid in the aqueous phase. As a result, the best separation was obtained by counter-rotation and dual-mode elution procedure. In this new separation mode, the mobile phase and stationary phase were exchanged when the rotation direction was reversed. The two purified alkaloids (purity over 98% as determined by HPLC) were identified by ESI-MS, (1)H-NMR and (13)C-NMR.
为了从曼陀罗花中分离阿托品和东莨菪碱，在 pH 区带精制逆流色谱中应用了三种不同的洗脱模式。这些分离是用乙酸乙酯/正丁醇/水（4:1:5 v/v）组成的两相溶剂系统在有机相中含有 0.50%三乙胺和在水相中含有 0.15%盐酸进行的。结果，通过反旋转和双模式洗脱程序得到了最佳的分离。在这种新的分离模式中，当旋转方向反转时，流动相和固定相被交换。通过 ESI-MS、（1）H-NMR 和（13）C-NMR 鉴定了两种纯化的生物碱（HPLC 测定纯度超过 98%）。
