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Method for extracting total alkali, reserpine and rutin from devilpepper

A technology of Rauvolfia and reserpine, which is applied in the field of medicine, can solve the problems of difficult control of production elution conditions, unfavorable production, no effective utilization, etc., and achieves advantages of comprehensive utilization and development, improvement of utilization efficiency, and simplified production. The effect of craftsmanship

Inactive Publication Date: 2010-01-13
KUNMING INST OF BOTANY - CHINESE ACAD OF SCI +1
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Problems solved by technology

Although this process is simple and does not require high equipment, the amount of benzene is large and the toxicity is relatively high; at the same time, it requires the use of toxic thiocyanate, which will easily lead to changes in the structure of rauwolfia and is not conducive to the utilization of other alkaloids ; In the production, only the root is used as raw material for production, and the leaves are not effectively utilized, which is not conducive to the improvement of raw material utilization
The traditional method of producing Rauwolfia total alkaloids is to use Rauwolfia root powder to extract with acidic ethanol, neutralize, recycle the solvent, acidify and remove impurities, and then obtain alkalinized precipitation; The solubility of the aqueous solution is very poor, and it can settle out with the colloid during the acidification process, resulting in a large loss of non-polar active alkaloids of reserpine, which is not conducive to production
CN101016297A patent describes a method for extracting Rauwolfia root powder by ethanol, using adsorption resin to carry out adsorption separation, and chloroform-petroleum ether joint degumming to produce reserpine. Although the method has been improved on the original basis, the adsorption resin decomposes On the one hand, the adsorption process is likely to cause pollution of polymer materials such as resins. On the other hand, the production and elution conditions are not easy to control, and must be collected and tested in sections at any time. The third aspect is that resin regeneration is also very troublesome, which is not conducive to production. The fourth aspect No and not suitable for production with leaves as raw materials

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  • Method for extracting total alkali, reserpine and rutin from devilpepper

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 2000g of Rauwolfia root dry powder, add 20000mL of 70% ethanol solution containing 0.3% hydrochloric acid, heat to 65°C, heat-preserve and reflux for extraction for 4hrs, and filter; the residue is heated to 65°C with 10000mL of 70% ethanol solution for heat-preservation, extraction for 2hrs, and filter; Then heat 10,000mL of 70% ethanol to 65°C for extraction for 2 hours, and filter. Combine the ethanol extracts extracted and filtered three times, depressurize to a vacuum of 0.07MPa, heat to 60°C, recover the solvent until there is no ethanol, and obtain an acidic extraction aqueous solution 400mL, stirred and added 800mL of deionized water, cooled, adjusted to pH 9.5 with ammonia water, cooled for 6hr, filtered, the filter residue was washed with 500ml of cold water until neutral, dried at 60°C until anhydrous, and 106g of crude alkali extract was obtained. Heat and stir the crude alkali with 2000mL acetone to dissolve for 2 hours, cool and filter, heat and dissol...

Embodiment 2

[0029]Take 5000g of Rauvolwolfia leaf dry powder, add 40000mL of 60% ethanol solution containing 0.1% hydrochloric acid, heat to 70°C, heat-preserve and reflux for extraction for 4hrs, and filter; then heat the residue with 30000mL of 60% ethanol solution to 70°C for heat-preservation, extract for 2hrs, and filter; The residue was then heated to 65°C with 30,000mL of 60% ethanol and extracted for 2 hours, filtered. The ethanol extracts from the three extractions were combined, decompressed to a vacuum of 0.07MPa, heated to 60°C to recover the solvent until there was no ethanol, and acidic extraction was obtained. 900 mL of aqueous solution was stirred and added with 2000 mL of deionized water, cooled, adjusted to pHH9.5 with ammonia water, cooled for 5 hours, filtered, and the filter residue was washed with 1000 mL of cold water until neutral, dried at 60°C until anhydrous, and 157 g of crude alkali extract was obtained. Heat and stir the crude alkali with 3000mL of acetone for...

Embodiment 3

[0031] Put 200Kg of Rauwolfia root dry powder into a multi-functional extraction tank, add 1400L of 70% ethanol solution containing 0.3% hydrochloric acid and soak for 12 hours (overnight), heat to 70°C with steam, keep warm and reflux for extraction for 4hrs, and filter; the residue is re-used with 1000L of 70% ethanol The solution was heated to 70°C for 2 hours, then filtered; the residue was then heated to 70°C with 1000L of 70% ethanol for 2 hours, then filtered. The ethanol extracts from the three extractions were combined and added to the concentrated recovery kettle, and the pressure was reduced to a vacuum of 0.07 MPa, heat to 60°C to recover the solvent until there is no ethanol, and obtain about 80L of acidic extraction aqueous solution, stir and add 150L of deionized water, cool, adjust the pH to 9.5 with ammonia water, let it cool for 6hr, centrifugal filter, and wash the filter residue with 100L of cold water to Neutral, dried to anhydrous at 60°C to obtain 12Kg of...

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Abstract

The invention relates to a method for extracting reserpine, total alkali (verticilum) and rutin from devilpepper, which uses complete stools, roots and leaves of the devilpepper as raw materials for production, thereby improving the utilization efficiency of resources. The extracting method does not adopt salt formation separation of toxic thiocyanate, thereby reducing the pollution caused by production; the chromatographic separation method is not adopted for separation, and inorganic salt reagents are not added, thus the characteristics of the raw materials are not changed; only by using the solubility difference of the reserpine and the rutin in a solvent, the solvent is directly used for separation, thereby simplifying the production process; and moreover, the used equipment is simple, the cost of the method is lower, the operation is convenient, and the solvent can be recycled repeatedly. In addition, the associated production and utilization of the total alkali, the reserpine and the rutin are achieved, thereby facilitating comprehensive utilization and development of devilpepper resources.

Description

Technical field: [0001] The invention belongs to the technical field of medicine separation technology, and in particular relates to a method for simultaneously producing and extracting total alkaloids, reserpine and rutin from roots and leaves of Rauwolfia. Background technique: [0002] Rauwolfia contains a large amount of indole alkaloids, such as reserpine, amarin, amarixin, yohimbine and other active alkaloids. More than 200 biological species have been isolated and identified from Rauwolfia plants Alkalis, of which total alkaloids and reserpine have been widely used in clinical medicine, such as Jiangyaling Tablets, Reserpine Tablets, Beijing Jiangyaling No. It is an important raw material for industrial production of antihypertensive drugs, and has been included in the Chinese Pharmacopoeia. Rauwolfia not only contains a large amount of alkaloids in the root, but also contains a large amount of alkaloids in the branches, and also contains a large amount of other biol...

Claims

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Application Information

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IPC IPC(8): A61K36/24A61P9/12C07D459/00C07H17/07A61K125/00A61K127/00A61K135/00
Inventor 刘锡葵肖建青张方进
Owner KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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