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Preparation method of alkaloid in stephania tetrandra

A technology based on biological and alkaloids, which is applied in the field of extraction and separation of active ingredients in plants, can solve the problems of unmentioned refining methods, etc., and achieve the effects of short preparation cycle, high strength, and simple operation of process steps

Inactive Publication Date: 2012-08-29
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Existing methods for simultaneously extracting the water-soluble phenolic alkaloids and the fat-soluble non-phenolic alkaloids of Fanggui are few, and the patent "Preparation Technology of Fanggui Alkaloids" (publication number: CN101288695A), the method disclosed in this patent is dilute acid permeation Drain, the percolation liquid is absorbed by macroporous ion resin, eluted with ammonia / amine alcohol solution, the eluate is placed and crystallized to obtain the total alkaloids of Fangji, and finally the pure Fangji alkaloids are obtained by various refining methods
However, the patent does not mention specific refining methods for other alkaloids except tetrandrine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 1kg of Fangji dry powder, soak it with 500ml of ammonia water for 1h, dry it at 50°C, add 4 times of 75% methanol to reflux and extract twice, each time for 0.5h, combine the extracts, concentrate until there is no alcohol smell, add 1% hydrochloric acid to dilute and dissolve Adjust the acid to pH 4, filter out the precipitate, add potassium hydroxide solution to the acid solution to adjust to pH 9, filter out the precipitate and wash with water, collect the alkaline water part, the water washing part and the precipitated part respectively.

[0024] The alkaline water part and the washing liquid part were combined, concentrated through a nanofiltration membrane (alumina inorganic ceramic membrane) with a molecular weight cut-off of 100, and the concentrated solution was freeze-dried to obtain 3.4 g of Hanhexine extract with a Hanhexine content of 56.4%.

[0025] Heat the precipitated part with an appropriate amount of acetone to dissolve, filter out the insoluble m...

Embodiment 2

[0027] Take 1 kg of Fangji dry powder, soak it with 1000ml of ammonia water for 3 hours, dry it at 70°C, add 10 times of 90% ethanol to reflux extraction 4 times, each time for 3 hours, combine the extracts, concentrate until there is no alcohol smell, add 3% hydrochloric acid to dilute and adjust Acid to pH 1, filter out the precipitate, add sodium hydroxide solution to the acid solution to adjust to pH 11, filter out the precipitate and wash with water, collect the alkaline water part, the water washing part and the precipitated part respectively.

[0028] The alkaline water part and the washing liquid part were combined, concentrated through a nanofiltration membrane (zirconia inorganic ceramic membrane) with a molecular weight cut-off of 200, and the concentrated solution was vacuum-dried to obtain 3.8 g of Hanhexin extract with a Hanhexine content of 53.7%.

[0029] Heat the precipitated part with an appropriate amount of acetone to dissolve, filter out the insoluble matte...

Embodiment 3

[0031] Take 5 kg of Fangji dry powder, soak in 3L of ammonia water for 1.5h, dry at 55°C, add 5 times of 80% propanol to reflux and extract 3 times, each time for 1h, combine the extracts, concentrate until there is no alcohol smell, add 1.5% hydrochloric acid to dilute And adjust the acid to pH 3.5, filter out the precipitate, add sodium carbonate solution to the acid solution to adjust the pH to 10, filter out the precipitate and wash with water, collect the alkaline water part, the washing liquid part and the precipitate part respectively.

[0032] The alkaline water part and the washing liquid part were combined, concentrated through a nanofiltration membrane (an antimony oxide inorganic ceramic membrane) with a molecular weight cut-off of 100, and the concentrated solution was freeze-dried to obtain 15.7 g of Hanhexine extract with a Hanhexine content of 61.2%.

[0033] Heat the precipitated part with an appropriate amount of acetone to dissolve, filter out the insoluble m...

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Abstract

The invention provides a preparation method of alkaloid in stephania tetrandra. The alkaloid contains cissamine extract and mixed extract of tetrandrine and hanfangichin. The preparation method comprises the following steps of: soaking stephania tetrandra dry powder with ammonia water; drying and then adding 75-90 percent low-carbon alcohol to reflux and extract; concentrating extract until no alcohol smell exists; adjusting the extract to be acidic with diluted hydrochloric acid; filtering off precipitate; adding alkali into the acid solution to precipitate; washing precipitate; (1) combining the washed solution and alkali liquor part, concentrating through a nanofiltration membrane and drying concentrated solution to obtain cissamine extract; and (2) adding acetone into the precipitate to dissolve, filtering off insoluble, adding water into acetone solution to settle out, filtering the precipitate and drying to obtain the mixed extract of tetrandrine and hanfangichin. Two alkaloid extracts are simultaneously prepared by using the preparation method; and the preparation method has the advantages of high raw material utilization rate, safe preparation process, low cost, short period and contribution to industrial large-scale production.

Description

Technical field: [0001] The invention belongs to the field of extraction and separation of effective plant components, and in particular relates to a preparation method of alkaloids in Fangchi. Background technique: [0002] Fangji is the root tuber of Stephania tetrandra S.Moorc, a plant belonging to the genus Fangji. It is a rheumatism-dispelling, antipyretic and analgesic drug, and it is mainly used for edema, dysuria, rheumatic joint pain, and hypertension. Its active ingredients are alkaloids. Tetrandine has the effects of analgesia, anti-inflammation, lowering blood pressure, antibacterial, anti-tumor, and relaxation of striated muscles. Recent studies have found that tetrandrine has anti-arrhythmic effects. The total alkaloid content in Tetrandrine can reach 2.3%, mainly fat-soluble non-phenolic alkaloids: tetrandrine A and tetrandrine B, the contents are about 1% and 0.5% respectively; water-soluble phenolic alkaloids: tetrandrine Cyclophylline, the content is about...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/147C07D455/03
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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