Abstract
Two high-speed countercurrent chromatography (HSCCC) modes were compared by separation of major alkaloids from crude extract of Picrasma quassioides. The conventional HSCCC separation was performed with a two-phase solvent system composed of petroleum ether–ethyl acetate–methanol–water (5:5:4.5:5.5, v/v/v/v) with 200 mg loading. pH-Zone-refining CCC was performed with two-phase solvent system composed of petroleum ether–ethyl acetate–n-butanol–water (3:2:7:9, v/v/v/v) where triethylamine (10 mM) was added to the upper organic stationary phase and hydrochloric acid (5 mM) was added to the lower aqueous phase with 2 g loading. From 2 g of crude extract, 87 mg of 5-methoxycanthin-6-one (a), 38 mg of 1-methoxy-β-carboline (b), 134 mg of 1-ethyl-4,8-dimethoxy-β-carboline (c), 74 mg of 1-ethoxycarbonyl-β-carboline (d), 56 mg of 1-vinyl-4,8-dimethoxy-β-carboline (e) and 26 mg of 1-vinyl-4-dimethoxy-β-carboline (f) were obtained with purities of over 97.0%. The results indicated that pH-zone-refining CCC is an excellent separations tool at the multigram level.
Highlights
IntroductionThe major active compounds in Picrasma quassioides are β-carbolines and canthin-6-one alkaloids which were reported to inhibit cAMP phosphodiesterase [3], and have anti-inflammatory, antihypertension and antiviral activities [2,4]
No report has been found on the use of pH-zone-refining CCC for the isolation and purification of alkaloids from Picrasma quassioides
1-methoxy-β-carboline (b), 76 mg of 1-ethyl-4,8-dimethoxy-β-carboline (c), 74 mg of 1-ethoxycarbonyl-β-carboline (d), 56 mg of 1-vinyl-4,8-dimethoxy-β-carboline (e) and 26 mg of 1-vinyl-4dimethoxy-β-carboline (f) were obtained in one step separation with purities of 98.1%, 98.2%, 98.4%, 98.7%, 99.1%, and 98.1%, respectively, as determined by HPLC (Figure 4). Both the conventional and pH-zone-refining modes of CCC successfully performed the preparative separation of alkaloids from crude extract of Picrasma quassioides
Summary
The major active compounds in Picrasma quassioides are β-carbolines and canthin-6-one alkaloids which were reported to inhibit cAMP phosphodiesterase [3], and have anti-inflammatory, antihypertension and antiviral activities [2,4] Because of these important activities and wide usage, large quantities of pure compounds are needed for further modern pharmacological and metabolic studies, as well as in the quality control of this traditional Chinese medicine and its products. No report has been found on the use of pH-zone-refining CCC for the isolation and purification of alkaloids from Picrasma quassioides. HSCCC in its two forms, conventional and pH-zone-refining CCC, was successfully applied to the separation of alkaloids from crude extract of Picrasma quassioides
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