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Method for preparing tetrandrine from stephania tetrandra total alkali

A technology for tetrandrine and fangji, which is applied in the field of preparing tetrandrine, can solve problems such as being unsuitable for large-scale production and preparation, and achieve the effects of simple operation and high purity

Pending Publication Date: 2020-03-06
广西大海阳光药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Titled "Separation of Tetrandrine A and B from Tetrandrine by TLC", the authors are Xu Yingshu and Jiang Bo's published literature also reported a preparative thin-layer chromatography using silica gel, using cyclohexane-acetone (0.5:1) It is the method for developing agent to separate Tetrandrine and B, but this method is also only suitable for the preparation of a small amount of samples, and is not suitable for large-scale production preparation; this document once used cyclohexane-ethyl acetate (6: 2) It is a developing agent, but in the end, the developing agent could not be used in the actual separation and purification

Method used

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  • Method for preparing tetrandrine from stephania tetrandra total alkali
  • Method for preparing tetrandrine from stephania tetrandra total alkali
  • Method for preparing tetrandrine from stephania tetrandra total alkali

Examples

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Effect test

Embodiment 1

[0031] A method for preparing tetrandrine from tetrandrine total alkaloids, comprising the steps of:

[0032] (1) Take Fangji, pulverize it, add water and extract it twice, the amount of water added each time is equivalent to 10 times and 8 times the weight of Fangji, and the extraction time is 3 hours and 1 hour respectively, the combined extracts are filtered, and the filtrate is concentrated to The clear ointment with a relative density of 1.10 at 65°C was used to obtain the total alkaloid extract of Tetradendronata;

[0033] (2) Get 5g of the total alkaloids of tetrandrine extract, add 2 times of the weight of the total alkaloids of the tetrandrine extract to dissolve in methanol, add 4 times of the amount of neutral alumina (80 mesh) to the solution and stir evenly, evaporate to dryness, pulverize, pass 40 mesh sieve, spare;

[0034] (3) Take 100 times the amount of neutral alumina (80 mesh) of the total alkaloid extract of tetrandrine, use cyclohexane-ethyl acetate (vol...

Embodiment 2

[0041] A method for preparing tetrandrine from tetrandrine total alkaloids, comprising the steps of:

[0042] (1) Take Fangji, pulverize and extract 3 times with 65% ethanol under reflux, the amount of ethanol each time is 8 times, 7 times, 6 times of the total amount of medicinal materials, the extraction time is 3 hours, 2 hours, 2 hours, combined extraction liquid, filtered, and the filtrate was concentrated to a clear paste with a relative density of 1.20 at 75°C to obtain the total alkaloid extract of Tetradendronata;

[0043] (2) Get 30g of the total alkaloids of tetrandrine extract, add 3.5 times of the weight of the total alkaloids of the tetrandrine extract to dissolve in ethanol, add 2 times of the amount of neutral aluminum oxide (90 mesh) to the solution and stir evenly, evaporate to dryness, pulverize, pass 50 mesh sieve, spare;

[0044] (3) Get 30 times the amount of neutral alumina (90 mesh) of the tetrandrine total alkaloid extract, use cyclohexane-ethyl aceta...

Embodiment 3

[0051] A method for preparing tetrandrine from tetrandrine total alkaloids, comprising the steps of:

[0052] (1) Take Fangji, grind it and add water to extract 3 times, the amount of water added each time is equivalent to 10 times, 9 times, 8 times of the total weight of the medicinal material, each extraction time is 3 hours, 2 hours, 1 hour, and the combined extracts , filtered, and when the filtrate was concentrated to 70 DEG C, the relative density was a clear paste of 1.15, ethanol was added to make the alcohol content 60%, and it was left to stand for 20 hours, filtered, and when the filtrate was concentrated to 68 DEG C, the relative density was an extract of 1.15, to obtain Tetrandrine total alkaloid extract;

[0053] (2) Get 50g of the total alkaloids of tetrandrine extract, add 5 times of the weight of the total alkaloids of tetrandrine extract to dissolve in ethanol, add 5 times of the amount of neutral aluminum oxide (100 mesh) to the solution and stir evenly, eva...

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Abstract

The invention discloses a method for preparing tetrandrine from a stephania tetrandra total alkali extract. The method comprises the steps of sample mixing, column packing, sample loading, separation,purification and the like. According to the method, neutral alumina column chromatography is used, cyclohexane-ethyl acetate is used as an eluent for elution, and tetrandrine in the stephania tetrandra total alkali extract is rapidly obtained; a column chromatography filler used in the method can be repeatedly used, and the used eluent can be recycled, so that the method has the advantages of environmental protection, simple operation, high purity of the obtained tetrandrine, and suitableness for industrial production. The purity of the tetrandrine prepared by the method for preparing the tetrandrine from the stephania tetrandra total alkali extract is more than or equal to 99%.

Description

technical field [0001] The invention relates to the field of extraction of effective plant components, in particular to a method for preparing tetrandrine from total alkaloids of tetrandrine. Background technique [0002] Fangji powder, a traditional Chinese medicine, has been used in China for thousands of years. Fenfangji (also known as Fangji) is the dried root slice of Stephania tetrandra S. Moore in the family Fangjiaceae. Alkaline (tetrandrine), tetrandrine base (tetrandrine, fangehinoline), tetrandrine, in addition to flavonoid glycosides, phenols, organic acids, volatile oils, etc. Studies have shown that tetrandrine and tetrandrine have analgesic, anti-inflammatory, blood pressure-lowering, anti-tumor, and striated muscle relaxation effects. In recent years, studies have found that tetrandrine also has anti-arrhythmic effects. [0003] The active ingredients of Tetrandrine are alkaloids, mainly Tetrandrine and Tetrandrin. Currently, the pharmacological effects of T...

Claims

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Application Information

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IPC IPC(8): C07D491/18
CPCC07D491/18
Inventor 黄大权唐新邓春霞
Owner 广西大海阳光药业有限公司
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