Separation preparation technique of high-purity saccular pterocarpin

A preparation process and technology for pterosin, applied in the direction of organic chemistry and the like, can solve the problems such as the industrial separation and preparation method of pterostilbene that has not yet been seen, and achieve the effects of high efficiency, low energy consumption, and improved adsorption rate.

Inactive Publication Date: 2012-12-19
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, there is no relevant report on the industrial separation and preparation method of cystic pterostilbene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take the sac-shaped red sandalwood heartwood, crush it, add 6L of 75% ethanol to ultrasonically extract 3 times, each time for 15min, and the ultrasonic frequency is 50KHz, filter to obtain the extract, add 0.3% diatomaceous earth to the extract, keep it at 55°C for 30min, and decolorize the decolorization solution Concentrate until there is no alcohol smell, pass through the H-50 macroporous resin column, first elute the impurities with water, and then elute with 3BV80% ethanol solution, collect the eluate rich in cystic pterostilbene, concentrate and dry, and use Separation by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-acetonitrile-water (4:4:3:4) as a two-phase solvent system, the upper phase is the stationary phase, and the lower phase is the mobile phase, pumped into the stationary phase and For the mobile phase, set the flow rate of the mobile phase to 3ml / min, start the main engine at the same time, adjust the speed to 850rpm, wait for ...

Embodiment 2

[0017] Take the sac-shaped red sandalwood heartwood, crush it, add 8L of 90% ethanol to ultrasonically extract twice, each time for 30min, and the ultrasonic frequency is 60KHz, filter to obtain the extract, add 0.3% diatomaceous earth to the extract, keep it at 50°C for 60min, and decolorize the decolorization solution Concentrate until there is no alcohol smell, enrich through HPD-700 macroporous resin column, first elute the impurities with water, then elute with 4BV75% ethanol solution, collect the eluate rich in cystic pterostilbene, concentrate and dry, dry The compound was separated by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-acetonitrile-water (3:4:2:3) as a two-phase solvent system, the upper phase was the stationary phase, and the lower phase was the mobile phase, which were pumped into the stationary phase successively. Phase and mobile phase, set the flow rate of the mobile phase to 3.5ml / min, start the main engine at the same time, adj...

Embodiment 3

[0019] Take the sac-shaped red sandalwood heartwood, crush it, add 18L of 70% ethanol to ultrasonically extract twice, each time for 18min, and the ultrasonic frequency is 75KHz, filter to obtain the extract, add 0.2% diatomaceous earth to the extract, keep it at 60°C for 50min, and decolorize the solution Concentrate until there is no alcohol smell, enrich through HPD-700 macroporous resin column, first elute the impurities with water, and then elute with 3BV80% ethanol solution, collect the eluate rich in cystic pterostilbene, concentrate and dry, and dry The compound was separated by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-acetonitrile-water (7:5:3:5) as a two-phase solvent system, the upper phase was the stationary phase, and the lower phase was the mobile phase, which were pumped into the stationary phase successively. Phase and mobile phase, set the mobile phase flow rate to 3ml / min, start the main engine at the same time, adjust the speed t...

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Abstract

The invention relates to a separation preparation technique of high-purity saccular pterocarpin, which comprises the following steps: taking saccular rosewood core, pulverizing, adding ethanol to carry out ultrasonic extraction, adding a right amount of kieselguhr into the extracting solution, keeping the temperature for decolorization, concentrating the decolorized solution, passing through a macroporous resin column for enrichment, eluting with a 75-85% ethanol solution, concentrating the eluate, drying, and separating the dried substance by high-speed counter-current chromatography to obtain the saccular pterocarpin. The method is simple to operate, has the advantages of high separation efficiency and high product purity, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of separation of natural products, and relates to a separation and preparation process of high-purity cystic pterostilbene, in particular to a method for preparing cystic pterostilbene by applying diatomite decolorization, macroporous resin enrichment and high-speed countercurrent chromatography. Background technique [0002] Cystic pterostilbene (Marsupsin), the molecular formula is C 16 h 14 o 6 , molecular weight 302.28, mp193~195℃, is from the leguminosae plant cystic red sandalwood Pterocarpus marsupium An active ingredient of aurones extracted from the heartwood of Roxb. Pharmacological studies have shown that pterostilbene vesicularis has hypoglycemic activity, and can significantly reduce the blood sugar level of experimental diabetic rats, and the effect can be compared with that of dimethyl biguanide. [0003] At present, there is no relevant report on the industrial separation and preparation method of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/83
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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