Rhynchophylline preparation process

A preparation process, the technology of rhynchophylline, which is applied in the field of medicine, can solve the problems of difficult conversion of rhynchophylline, lower yield, isorhynchophylline, etc., and achieve the effects of increasing water solubility, reducing harm, and ensuring stability

Inactive Publication Date: 2017-12-29
上海源叶生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiencies in the prior art, the present invention provides a preparation process of rhynchophylline. This process optimization avoids the use of a large amount of organic solvents during extraction, ensures that rhynchophylline is not easy to transform and reduces its yield during the preparation process, and can be obtained more Rhynchophylline with higher purity solves the problems of easy conversion into isorhynchophylline, low purity, and easy decomposition at high temperature in the preparation process of existing processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation process of rhynchophylline, comprising the following steps:

[0024] (1) Extraction of medicinal materials: pulverize the medicinal materials of Uncaria, the ethanol concentration is 80%, the volume of HCL is 0.1% of the ethanol solution, the solid-liquid ratio of the medicinal materials of Uncaria and the mixed solution of ethanol and hydrochloric acid is 1:8, soak for 1- 3 days;

[0025] (2) Concentrated extraction of the extract: extract the solution soaked in step (1) to obtain the extract, concentrate the extract at 50°C to no alcohol, add sodium hydroxide solution after cooling to adjust the pH to 8, add 0.8 times Volume of chloroform is extracted, and after extraction, the concentrated chloroform layer obtains the crude product of rhynchophylline with low content;

[0026] (3) Preliminary separation by normal-phase silica gel chromatography: the obtained total rhynchophylline is preliminarily separated with silica gel, and the mixed solution of pet...

Embodiment 2

[0030] A preparation process of rhynchophylline, comprising the following steps:

[0031] (1) Extraction of medicinal material: Pulverize the medicinal material of Uncaria, the ethanol concentration is 80%, the volume of HCL is 0.1% of the ethanol solution, the solid-liquid ratio of the medicinal material of Uncaria and the mixed solution of ethanol and hydrochloric acid is 1:9, soak for 1- 3 days;

[0032] (2) Concentrated extraction of the extract: extract the solution soaked in step (1) to obtain the extract, concentrate the extract at 60°C until alcohol-free, add sodium carbonate solution after cooling to adjust the pH to 10, and add 1.2 times the volume The chloroform is extracted, and the chloroform layer is concentrated after extraction to obtain the crude product of rhynchophylline with low content;

[0033] (3) Preliminary separation by normal-phase silica gel chromatography: the obtained total rhynchophylline is preliminarily separated with silica gel, and the mixed...

Embodiment 3

[0037] A preparation process of rhynchophylline, comprising the following steps:

[0038] (1) Extraction of medicinal material: Pulverize the medicinal material of Uncaria, the ethanol concentration is 80%, the volume of HCL is 0.1% of the ethanol solution, the solid-liquid ratio of the medicinal material of Uncaria and the mixed solution of ethanol and hydrochloric acid is 1:10, soak for 1- 3 days;

[0039] (2) Concentrated extraction of the extract: extract the solution soaked in step (1) to obtain the extract, concentrate the extract at 70°C until alcohol-free, add sodium bicarbonate solution after cooling to adjust the pH to 9, and add 1.1 times Volume of chloroform is extracted, and after extraction, the concentrated chloroform layer obtains the crude product of rhynchophylline with low content;

[0040] (3) Preliminary separation by normal-phase silica gel chromatography: the obtained total rhynchophylline is preliminarily separated by silica gel, and the mixed solution...

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Abstract

A rhynchophylline preparation process includes: (1) soaking ground Ramulus Uncariae cum Uncis in ethyl alcohol and hydrochloric acid mixed solution; (2) heating and concentrating extract liquid to a non-alcohol state, cooling, adjusting PH to 8-10, adding chloroform, and extracting to obtain a low-content rhynchophylline crude product; (3) preliminarily separating through normal-phase silica gel chromatography to obtain a high-content rhynchophylline crude product; (4) dissolving the rhynchophylline crude product in hydrochloric acid solution, and adopting a reverse-phase C18 medium-pressure column for purification to obtain high-purity rhynchophylline hydrochloride; (5) reducing the rhynchophylline hydrochloride into rhynchophylline, filtering after separating out, washing off excessive ammonium hydroxide and salt with pure water, and directly performing freeze drying to obtain a high-purity rhynchophylline product. The rhynchophylline preparation process has advantages that (1) organic reagent extraction is mostly avoided, cost is reduced, and harms of organic reagents are reduced; (2) stability of rhynchophylline in a preparation process is guaranteed, and the target yield is increased; (3) the high-purity product is obtained.

Description

technical field [0001] The invention relates to a preparation process of rhynchophylline, which belongs to the technical field of medicine. Background technique [0002] Uncaria is an evergreen vine of the Rubiaceae Uncaria genus, which is a commonly used traditional Chinese medicine. Since ancient times, it has been used as a medicine for clearing heat, calming the liver, calming wind and relieving convulsions, and treating dizziness, convulsions, convulsions, general numbness and other cardiovascular and nervous system diseases. It has become a commonly used drug in the treatment of hypertension. [0003] Modern pharmacological studies have shown that the main active ingredients of Uncaria are Uncaria alkaloids, of which Rhynchophylline and Isorhynchophylline are the main active ingredients. Rhynchophylline accounts for a relatively high proportion of total alkaloids, and has a good curative effect. Studies have shown that rhynchophylline is unstable in polar solvents an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/20
CPCC07D471/20
Inventor 朱云飞
Owner 上海源叶生物科技有限公司
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