Method for extracting ajmaline from devilpepper waste liquor

A technology of Rauvolfia and waste liquid, which is applied in the field of separation and purification of natural medicines, can solve the problems of wasting reserpine, affecting the yield of separation and purification, and difficult to purify, and achieves the advantages of increasing product types, simple extraction methods, and simple purification methods. Effect

Inactive Publication Date: 2012-12-19
海南制药厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main disadvantages of these separation and purification methods are: (1) the total extract of Rauwolfia is transferred to the aqueous solution after acidic extraction and then transferred to the alkaline extraction to obtain more impurities in the extract, which is difficult to follow-up purification and difficult to achieve qualified purity. (2) When using acid-dissolved partial extraction, the salt concentration of the extract is too large, which has a greater impact on the yield of separation and purification, which is not conducive to production scale-up; (3) Preparation of liquid phase The method can be used for research but cannot be used for scale-up production; (4) directly extracting Ayimalin from Rauwolfia will waste reserpine and cannot effectively utilize Rauwolfia resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Extraction and concentration: get 100 liters of the remaining aqueous solution after extracting reserpine, adjust the pH value of the remaining aqueous solution to 6.5 with ammonia water (concentration is 25-28% by mass), then extract with 90 liters of toluene (30 liters / time, 3 times), then adjust the pH value of the remaining aqueous solution to 9.5 with ammonia water, extract with toluene until there is no alkaloid reaction (determined qualitatively by color development of alkaloid characteristic chromogenic agent-bismuth potassium iodide solution), and combine Concentrate the toluene phase until a layer of solid matter precipitates out in the bottle, stop at room temperature to allow the solid matter to precipitate completely, filter out the solid matter, and dry at 60-65°C for 3 hours to obtain 291 grams of crude product, and the filtrate is recycled.

[0026] (2) Purification: use 1550 milliliters of dilute hydrochloric acid with a concentration of 5% by mass...

Embodiment 2

[0028] (1) Extraction and concentration: get 200 liters of the remaining aqueous solution after extracting reserpine, adjust the pH value of the remaining aqueous solution to 7 with ammonia (concentration is 25-28% by mass), then extract with 160 liters of chloroform (40 liters / time, 4 times), and then use ammonia water to adjust the pH value of the remaining aqueous solution to 10, then extract with chloroform until there is no alkaloid reaction (determined qualitatively with alkaloid characteristic chromogenic agent-bismuth potassium iodide solution for color development), and combine Chloroform phase, concentrated until a layer of solid matter precipitated in the bottle, stopped, placed at room temperature to completely precipitate the solid matter, filtered out the solid matter, and dried at 65-70°C for 3 hours to obtain 623 grams of crude product, and the filtrate was recycled. .

[0029] (2) Purification: use 2700 milliliters of dilute hydrochloric acid with a concentr...

Embodiment 3

[0031] (1) Extraction and concentration: get 300 liters of the remaining aqueous solution after extracting reserpine, adjust the pH value of the remaining aqueous solution to 6.0 with ammoniacal liquor (concentration is 25% to 28% by mass), then extract with 240 liters of ethyl acetate ( 60 liters / time, 4 times), after adjusting the pH value of the remaining aqueous solution to 9.5 with ammoniacal liquor, extract with ethyl acetate until there is no alkaloid reaction (with the characteristic chromogenic agent of alkaloid-bismuth potassium iodide solution for color development and qualitative determined), combined the ethyl acetate phases, concentrated until a layer of solid matter was precipitated in the bottle, stopped, placed at room temperature to completely precipitate the solid matter, filtered out the solid matter, and dried at 60°C for 3 hours to obtain 815 grams of crude product, filtered out Liquid recycling.

[0032](2) Purification: 3260 milliliters of dilute hydroc...

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Abstract

The invention discloses a method for extracting ajmaline from devilpepper waste liquor. The ajmaline is obtained by extracting a raffinate of devilpepper with extracted reserpine and adopting methods, i.e. stepped extraction, decoloration sedimentation, washing crystallization, and the like, i.e. the ajmaline is separated when the reserpine is produced by using devilpepper medicinal materials, thereby realizing the effective utilization of plant resources, solving the problem that the reserpine and the ajmaline are produced at the same time by using the devilpepper, enhancing the utility ratio of resources, increasing the types of products and generating new profit growth points. The invention adopts simple and easy extracting method and refining method, can conveniently and fast obtain the ajmaline according with the specifications of a pharmacopeia and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of separation and purification of natural medicines, in particular to a method for extracting ayimalin from waste liquid of Rauvolwolfia. Background technique [0002] Rauwolfia contains a variety of alkaloids with pharmacological activity, and more than 100 kinds have been isolated. The alkaloids with high content are reserpine, ayimarin, serpentine and yohimbine, among which the main clinical effect of reserpine is to lower blood pressure, and the content of reserpine in Rauvolwolfia is generally 1.2 %, accounting for about 30% of the total alkaloids of Rauwolfia, therefore, people usually extract reserpine from Rauwolfia. [0003] The main clinical effect of Ayimalin is anti-arrhythmia, and its content generally accounts for about 15% of the total alkaloids of Rauwolfia. Because there are alkaloids in Rauwolfia similar in structure to Ayimalin, they are isolated from Rauwolfia Ayi Malin is more difficult. The ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D459/00
Inventor 李秀峰蒲含林冯锦东赖潜
Owner 海南制药厂有限公司
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