Separation (statistics)

Phase (matter)

High-performance liquid chromatography

Statistics

Chromatography

Solvent

Thermodynamics

Physics

Organic chemistry

Mathematics

Analytical Chemistry (journal)

Countercurrent chromatography

Chemistry

Volumetric flow rate

Separation and Purification Technology

A preparative high-speed counter-current chromatography (HSCCC) was used to isolate and separate curculigoside and curculigoside B from the famous traditional Chinese medicinal herb Curculigo orchioides. Some parameters including two-phase solvent system, separation temperature, flow rate of the mobile phase and revolution speed of the apparatus were all investigated, and a successfully isolation and purification was achieved at the following conditions: the two-phase solvent system composed of ethyl acetate–ethanol–water at a volume ratio of 5:1:5 (v/v/v) was selected and the lower phase of the system was used as the mobile phase at the flow rate of 2.0 ml/min, and the isolation temperature and revolution speed were set at 30 °C and 800 rpm. The isolation produced a total of 14.5 mg curculigoside B and 72.8 mg curculigoside with purities of 96.5% and 99.4% determined by high performance liquid chromatography (HPLC) from 300 mg crude extract after cleaning-up by D101 macroporous resin, which was necessary for the excellent purification. The recoveries of the two compounds were 91.6% and 92.5%, respectively, and the chemical structure identification was carried out by UV, MS and NMR. This separation method was more effective than some conventional techniques.

Optimization suitable conditions for preparative isolation and separation of curculigoside and curculigoside B from Curculigo orchioides by high-speed counter-current chromatography