Wang Xiao, Geng Yanling, Li Fuwei, Shi Xingang, Liu Jianhua
Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan, Shandong 250014, China.
J Chromatogr A. 2006 May 19;1115(1-2):267-70. doi: 10.1016/j.chroma.2006.03.103. Epub 2006 Apr 18.
pH-zone-refining counter-current chromatography was successfully applied to the separation of alkaloids from a crude extract of Corydalis decumbens (Thunb.) Pers. using a multilayer coil planet centrifuge (CPC). The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether (MtBE)-acetonitrile-water (2:2:3, v/v) where triethylamine (5-10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5-10 mM) to the aqueous mobile phase as an eluter. From 3.1 g of the crude extract, 495 mg protopine, 626 mg tetrahydropalmatine and 423 mg bicuculline were obtained each with a purity of over 93% as determined by high performance liquid chromatography. The structures of the isolated compounds were identified by electron ionization mass spectrometry (EI-MS), high-performance liquid chromatography (HPLC)-electrospray ionisation-mass spectrometry (ESI-MS) and 1H NMR.
采用多层螺旋行星式离心机（CPC），成功地运用pH区带精制逆流色谱法从夏天无（Corydalis decumbens (Thunb.) Pers.）粗提取物中分离生物碱。实验采用由甲基叔丁基醚（MtBE）-乙腈-水（2:2:3，v/v）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（5 - 10 mM）作为保留剂，向水相流动相中加入盐酸（5 - 10 mM）作为洗脱剂。从3.1 g粗提取物中，获得了495 mg原阿片碱、626 mg延胡索乙素和423 mg荷包牡丹碱，通过高效液相色谱法测定，其纯度均超过93%。通过电子电离质谱（EI-MS）、高效液相色谱（HPLC）-电喷雾电离质谱（ESI-MS）和1H NMR对分离得到的化合物结构进行了鉴定。
