Wang Xiao, Geng Yanling, Wang Daijie, Shi Xingang, Liu Jianhua
Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
J Sep Sci. 2008 Oct;31(20):3543-7. doi: 10.1002/jssc.200800322.
pH-zone-refining counter-current chromatography was successfully applied to the separation of alkaloids from a crude extract of Peganum harmala L. using a multilayer coil planet centrifuge. The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether/THF/water (2:2:3 by volume) where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 1.2 g of the crude extract, 554 mg harmine and 325 mg harmaline were obtained each with a purity of over 96% as determined by HPLC. The structures of the isolated compounds were identified by electron ionization MS (EI-MS), (1)H NMR, and (13)C NMR.
采用多层线圈行星离心机，成功地将pH区带精制逆流色谱法应用于从骆驼蓬粗提物中分离生物碱。实验采用由甲基叔丁基醚/四氢呋喃/水（体积比2:2:3）组成的两相溶剂体系，其中向上层有机固定相中加入三乙胺（10 mM）作为保留剂，向水相流动相中加入盐酸（5 mM）作为洗脱剂。从1.2 g粗提物中获得了554 mg的骆驼蓬碱和325 mg的去氢骆驼蓬碱，通过高效液相色谱法测定，其纯度均超过96%。通过电子电离质谱（EI-MS）、氢核磁共振（1H NMR）和碳核磁共振（13C NMR）对分离得到的化合物结构进行了鉴定。
