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Separating preparation process of high-purity broussin

A preparation process and high-purity technology, applied in the direction of organic chemistry, can solve the problems of low dendrimin content, low adsorption rate of macroporous resin, and difficulty in obtaining active ingredients, so as to achieve good product quality, high efficiency, and improved adsorption rate Effect

Inactive Publication Date: 2012-12-26
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic research on dendrimers is still in its infancy. Chinese patent 201010554172.5 uses dendrimers as raw materials to extract and separate dendrimers by means of microwave extraction, macroporous resin adsorption, and n-hexane crystallization. The content of dendrimers in dendrimers is The content is low, the adsorption rate of macroporous resin is low, and it is difficult to obtain high content of active ingredients in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 1 kg of Dracaena glabra resin, crush it, add 4L of 75% ethanol to ultrasonically extract twice, each time for 1.5h, the ultrasonic frequency is 40KHz, filter to obtain the extract, add 0.3% diatomaceous earth to the extract, and decolorize at 55°C for 30min , the decolorization solution is concentrated until it has no alcohol smell, passes through a polyamide resin column, first elutes impurities with water, and then elutes with 3BV80% ethanol solution, collects the eluate rich in dendrimin, concentrates and dries, and the dried product adopts high-speed countercurrent Chromatographic separation, using n-hexane-ethyl acetate-acetonitrile-water (4:4:3:4) as a two-phase solvent system, the upper phase is the stationary phase, the lower phase is the mobile phase, and the stationary phase and the mobile phase are pumped in sequence , set the flow rate of the mobile phase to 3ml / min, start the main engine at the same time, adjust the rotation speed to 850rpm, wait for th...

Embodiment 2

[0015] Take 1 kg of Dracaena glabra resin, crush it, add 8L of 90% ethanol for ultrasonic extraction once, each time for 2 hours, the ultrasonic frequency is 40KHz, filter to obtain the extract, add 0.3% diatomaceous earth to the extract, and decolorize it at 50°C for 60 minutes. The decolorization solution is concentrated until it has no alcohol smell, enriched by a polyamide resin column, the impurities are first eluted with water, and then eluted with 4BV75% ethanol solution, and the eluate rich in dendrimin is collected, concentrated and dried, and the dried product is dried by high-speed Separation by countercurrent chromatography, using n-hexane-ethyl acetate-acetonitrile-water (2:2:2:3) as a two-phase solvent system, the upper phase is the stationary phase, the lower phase is the mobile phase, pumped into the stationary phase and mobile phase successively Phase, set the flow rate of the mobile phase to 2.5ml / min, start the main engine at the same time, adjust the rotatio...

Embodiment 3

[0017] Take 2kg of Dracaena glabra resin, crush it, add 10L of 70% ethanol to ultrasonically extract twice, each time for 1.0h, the ultrasonic frequency is 25KHz, filter to obtain the extract, add 0.2% diatomaceous earth to the extract, and decolorize at 70°C for 50min , the decolorization solution is concentrated until it has no alcohol smell, enriched by a polyamide resin column, the impurities are first eluted with water, and then eluted with 3BV80% ethanol solution, the eluate rich in dendrimin is collected, concentrated and dried, and the dried product is used Separation by high-speed countercurrent chromatography, using n-hexane-ethyl acetate-acetonitrile-water (3:5:3:5) 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 rotation speed to 800rpm, wait fo...

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Abstract

The invention relates to a separating preparation process of high-purity broussin; and the method comprises the specific steps of: using dracaena cochinchinensis resin as raw materials; crushing the raw materials; adding 4-10 times of ethanol of 65-90% to the raw materials for ultrasonically extracting the raw materials; adding a proper amount of diatomite to an extracting liquor so as to preserve the heat of the extracting liquor and decolorize the extracting liquor; concentrating a decolorized solution; enriching the decolorized solution by using a polyamide resin column; eluting the decolorized solution by using 75-85% of ethanol solution; concentrating an eluting solution; drying the eluting solution; and separating a dry product by using a high speed counter-current chromatography so as to obtain the broussin. The separating preparation process of the high-purity broussin, provided by the invention, has the advantages of simplicity and convenience in operation, high separating efficiency and good 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 high-purity dendrimer separation and preparation process, in particular to a method for preparing dendrimer by diatomite decolorization, polyamide resin enrichment and high-speed countercurrent chromatography. Background technique [0002] Sword Leaf Dracaena ( Dracaena cochinchinensis (Lour.) S.C.chen) is the source plant of "Dragon's Blood", which is mainly produced in Guangxi, Yunnan and other provinces. It mainly contains flavonoids, saponins, stilbenes, phenols, organic acids, esters and volatile oils. It has anti-inflammatory, anti-bacterial, fungal, analgesic, blood-activating, hemostatic, and pharmacological effects such as changing blood rheology. It is clinically used to treat various indications of shell, gynecology, internal medicine, ENT, and dermatology. [0003] Structulin is one of the active components in the resin of Dracaena phoenix leaf, and it...

Claims

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Application Information

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IPC IPC(8): C07D311/60
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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