Technology for separating and preparing high-purity ailanthone

A preparation process, the technology of Ailanthus ketone, applied in the field of separation of natural products, can solve the problems of low Ailanthus ailanthus content, low adsorption rate of macroporous resin, and difficulty in obtaining high-content active ingredients, so as to achieve improved adsorption rate, good product quality, and high efficiency. high effect

Inactive Publication Date: 2013-08-28
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Domestic research on Ailanthonone is still in its infancy. The Chinese patent "A Preparation Method for Ailanthione" (application number: 201010170495.4) uses fresh bark or root bark as raw material, and adopts lye extraction, macroporous resin adsorption, Ailanthus ketone is extracted and separated by acetone recrystallization and other means. The content of Ailanthus ailanthus in Ailanthus bark is low, and the adsorption rate of macroporous resin is low. It is difficult to obtain high-content active ingredients in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 1kg Ailanthus bark, 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, keep it at 55°C for 40min, and decolorize the solution Concentrate until there is no alcohol smell, pass through a polyamide resin column, first elute impurities with water, and then elute with 4BV80% ethanol solution, collect the eluate rich in Ailanthonone, concentrate and dry, and the dried product is separated 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. The phase flow rate is 3ml / min, start the main engine at the same time, adjust the rotation speed to 850rpm, wait for the solvent system in the column to reach a dynamic equilibrium, inject a sample, collect a high-concentration Ailan...

Embodiment 2

[0018] Take 1kg Ailanthus bark, 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, keep it at 50°C for 60 minutes, and concentrate the decolorization solution Until there is no alcohol smell, it is enriched by a polyamide resin column, and the impurities are first eluted with water, and then eluted with 3BV80% ethanol solution, and the eluate rich in Ailanthonone is collected, concentrated and dried, and the dried product is separated by high-speed countercurrent chromatography , using n-hexane-ethyl acetate-acetonitrile-water (6:2:3:3) as a two-phase solvent system, the upper phase is the stationary phase, and the lower phase is the mobile phase, the stationary phase and the mobile phase are pumped in sequence, set The flow rate of the mobile phase is 2.5ml / min, start the main engine at the same time, adjust the rotating speed to 880r...

Embodiment 3

[0020] Take 2kg Ailanthus bark, crush it, add 10L of 80% ethanol to ultrasonically extract twice, each time for 1.0h, the ultrasonic frequency is 25KHz, filter to obtain the extract, add 0.4% diatomaceous earth to the extract, keep it at 70°C for 50min, and decolorize the solution Concentrate until there is no alcohol smell, enrich through polyamide resin column, first elute impurities with water, then elute with 5BV80% ethanol solution, collect the eluate rich in Ailanthonone, concentrate and dry, and the dried product adopts high-speed countercurrent chromatography For separation, use n-hexane-ethyl acetate-acetonitrile-water (5:5:5:2) as a two-phase solvent system, the upper phase is the stationary phase, and the lower phase is the mobile phase. 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 rotating speed to 800rpm, and wait for the solvent system in the c...

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Abstract

The invention relates to a technology for separating and preparing high-purity ailanthone. The technology comprises the following detailed steps of: grinding ailanthus tree bark taken as raw material; adding 75-90% ethanol to implement ultrasonic extraction, wherein the amount of the ethyl alcohol is 6-12 times that of the ground bark; adding an appropriate amount of kieselguhr into an extracted solution, preserving heat and destaining; concentrating a destained solution, enriching the destained solution by a polyamide resin column; eluting the destained solution by an 80% ethanol solution; and concentrating an eluent, implementing drying, and separating dried products in a high-speed counter-current chromatography way, thus obtaining the ailanthone. The method is simple and convenient to operate, high in separation efficiency, good in product purity, and 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 ailanthonone separation and preparation process, in particular to a method for preparing ailanthone by using diatomite decolorization, polyamide resin enrichment and high-speed countercurrent chromatography. Background technique [0002] Ailanthone (Ailanthone), needle crystal, molecular formula C 20 h 24 o 7 , with a molecular weight of 376.40, mainly derived from the bark of Ailanthus altissima (Mill.) Swingle. [0003] . [0004] Ailanthus ketone is one of the active ingredients in Ailanthus bark. Pharmacological studies have shown that Ailanthus ketone is a plant extract, a substance extracted from Ailanthus bark, which has antibacterial, antiprotozoal and antitumor effects, 100% The decoction has inhibitory effect on Shigella flexneri, Shigella sonnei and Escherichia coli in vitro. It has a strong inhibitory effect on amoeba and trichomonas va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/10
Inventor 苏刘花万冬梅
Owner NANJING ZELANG AGRI DEV
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