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Process for preparing oridonin

A technology of Rubescensin A and Rubescensin A, which is applied in the field of preparation of Rubescensin A, can solve the problem of not being the best process for large-scale industrial production, unclarified coarse crystals of Rubescensin A, low extraction yield, etc. Problems, to shorten the production cycle, reduce the space and area occupied by the workshop, and achieve good results

Inactive Publication Date: 2004-03-17
中国科学院武汉植物研究所
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AI Technical Summary

Problems solved by technology

[0006] This method uses industrial alcohol instead of ether and methanol, which is more suitable for industrial production, but the disadvantage is that the extraction yield is low
[0007] Although the above-mentioned two methods both consider the extraction of Rubescens A by column chromatography, they have a common defect: how to further refine the obtained coarse crystals of Rubescensin A into high-purity Rubescens A prime crystal
Although this method is simpler than the solvent system used in the previous method, the extract is still concentrated and then dissolved in 95% ethanol before it can be mixed with column chromatography silica gel. The selected chromatography column diameter-height ratio is 1: 18.75. The required equipment is huge, and the eluent flow rate is 1 / 150 / minute to 1 / 220 / minute (eluent volume / adsorbent volume / minute), which is too slow and obviously not the best process for large-scale industrial production

Method used

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Examples

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Embodiment 1

[0014] Embodiment 1. Get 30 kilograms of Radix Grasses, pulverize to 40~80 orders, add 220 kilograms, 160 kilograms, 130 kilograms of chloroform successively: ethanol (9: 1) solution refluxes three times, each 3.5 hours, extracting solution passes through Concentrate under reduced pressure to obtain 1 kg of Rubescensin A content of 11.3% oridonin extract, which is evenly treated with ethanol, mixed with 1.5 kg of 200-300 mesh silica gel, spread dry, take 8 kg of fresh silica gel for packing, and mix the Mixed silica gel is added on it. First wash the column with 50 liters of dichloromethane to remove impurities, and then use a mixed solvent of dichloromethane and acetone (4:1) for desorption. After washing the column with 65 liters of mixed solvent, begin to collect oridonin fractions To 15 liters, concentrated to 1.5 liters at a temperature of 50°C and a vacuum of 0.6Mpa. The concentrated solution was placed in an enamel plate for 10 hours to crystallize, and then vacuum filt...

Embodiment 2

[0015] Embodiment 2. With 500 kilograms of commercially available medicinal materials, Rubescens japonicus, pulverize to 40~80 orders, successively use 3000 kilograms, 2000 kilograms, 1000 kilograms of dichloromethane: acetone (4: 1) solution reflux three times, each 3 hours, The combined extracts were concentrated under reduced pressure to obtain about 10 kg of extract with a content of 12.8% oridonin, treated with acetone evenly, mixed into 18 kg of 200-300 mesh column chromatography silica gel, and spread to dry the solvent , first prepack 8 kg of fresh silica gel in each of the 15 chromatographic columns, then mix the samples with silica gel and evenly install them on the upper part of the 15 chromatographic columns, each chromatographic column is first eluted with 60 liters of dichloromethane , then use dichloromethane and acetone (4: 1) mixed solvent desorption, when the mixed solvent washes out about 70 liters, start to collect the desorption solution containing oridonin...

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PUM

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Abstract

The oridonin preparing process includes crushing rabdosia, reflux extracting with the mixed solvent of dichloromethane, acetone or chloroform and ethanol, decompression concentrating extractive liquid to obtain thick paste, defatting with petroleum ether, filtering and evaporating to obtain extract, acetone or ethanol treatment, mixing with column chromatographic silica gel, eluting with dichloromethane, desorbing with mixed solvent of dichloromethane and acetone, collecting the component of oridonin, decompression concentrating, letting the concentrate in crystallizer for crystallization to separate oridonin and mother liquid, and re-crystallizing in methanol solution for refining. The present invention has short chromatographic course, fast separation speed, high separation effect, high product purity over 90 % and low production cost.

Description

technical field [0001] The invention relates to a method for extracting and purifying plant medicines, and more specifically relates to a method for preparing oridonin. technical background [0002] The traditional extraction methods of Rubescensin A mainly include ether extraction and ethanol extraction. [0003] The steps of the ether extraction method are as follows: add 3 to 5 times the amount of ether to the raw material of Oryx japonicus and extract it for 2 to 3 hours, recover the ether, dissolve the green-brown viscous substance in methanol, add activated carbon for decolorization, and reduce the obtained light yellow and clear methanol liquid. Concentrate under pressure, leave the concentrated solution overnight, filter, and concentrate the filtrate to get a thick paste, add Al 2 o 3 The column was first eluted with benzene, and then eluted with ether, and the ether eluate recovered the solvent to obtain crude crystals, which were treated...

Claims

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Application Information

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IPC IPC(8): C07C45/81C07C49/517
Inventor 王有为卢大炎王跃进龚复俊斯缨王暐叶晚成丁时东
Owner 中国科学院武汉植物研究所
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