A kind of preparation method of sodium aescinate

A technology of sodium aescinate and aescin, which is applied in the field of preparation of sodium aescinate, can solve the problems of long time consumption, restriction of production efficiency of sodium aescinate, low total yield, etc., and achieve the effect of improving production efficiency

Active Publication Date: 2021-01-15
GANSU CHANGEE BIO PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Judging from the above two existing schemes for preparing sodium aescinate, the total yields of both are not high, and the most direct problem is that the entire purification cycle (i.e. the entire purification process time after extracting the sage) is time-consuming Longer, these two points seriously restricted the production efficiency of sodium aescinate

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  • A kind of preparation method of sodium aescinate

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Embodiment 1

[0037] Embodiment 1: preparation method of the present invention

[0038] Preliminary purification: Weigh 1.0kg of sala seeds, add 4.0L of 50% by volume methanol solution, stir at room temperature for 12 hours, filter, add the filter residue to 2.0L of 50% by volume methanol solution, stir at room temperature for 6 hours, and filter Repeat the above operation once, combine the filtrate, concentrate under reduced pressure until the solution produces foam, adjust the pH to about 3 with a saturated oxalic acid solution, add 300ml of chloroform dropwise, a large amount of solid is produced, and centrifugally filter to obtain the crude aescin solid, to which 100ml of water is added , adjust the pH to about 6 with 1% sodium hydroxide, then add 60 g of needles to decolorize with activated carbon for 2 hours, filter, and concentrate the filtrate to about 100 ml under reduced pressure, drop the solution into 1 L of acetone, centrifugally filter, and vacuum dry to obtain aescin Sodium C...

Embodiment 2

[0042] Embodiment 2: preparation method of the present invention

[0043] Preliminary purification: Weigh 1.0kg of sala seeds, add 4.0L of 80% by volume methanol solution, stir at room temperature for 12 hours, filter, add the filter residue to 2.0L of 80% by volume methanol solution, stir at room temperature for 6 hours, and filter Repeat the above operation once, combine the filtrates, concentrate under reduced pressure until the solution produces foam, adjust the pH to about 4 with saturated citric acid solution, add 300 ml of dichloromethane dropwise, a large amount of solids are produced, and centrifugally filter to obtain aescin. Add 100ml of water to it, adjust the pH to about 5 with 1% sodium hydroxide, then add 80g of needles to decolorize with activated carbon for 6 hours, filter, and concentrate the filtrate to about 100ml under reduced pressure, drop the solution into 1L of acetone, centrifugal filter, vacuum Dry to obtain the crude product of sodium aescinate. Am...

Embodiment 3

[0047] Embodiment 3: preparation method of the present invention

[0048] Preliminary purification: Weigh 1.0kg of sala seeds, add 4.0L of 30% by volume methanol solution, stir at room temperature for 12 hours, filter, add the filter residue to 2.0L of 30% by volume methanol solution, stir at room temperature for 6 hours, and filter Repeat the above operation once, combine the filtrates, concentrate under reduced pressure until the solution produces foam, adjust the pH to about 2 with dilute hydrochloric acid, add 300 ml of ethyl acetate dropwise, a large amount of solids are produced, and centrifugally filter to obtain aescin. Add 100ml of water to it, adjust the pH to about 7 with 1% sodium hydroxide, then add 100g of needles and decolorize them with activated carbon for 4 hours, filter, concentrate the filtrate under reduced pressure to about 100ml, drop the solution into acetone, filter, and dry in vacuo to obtain Crude Sodium Aescinate. Among them, the content of sodium ...

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Abstract

Disclosed is a method for preparing sodium aescinate, relating to the technical field of plant extraction. The method comprises: semen aesculi is taken and subjected to alcohol extraction, the resulting extracting solution is subjected to extraction with chloroform, dichloromethane or ethyl acetate under acidic conditions, and the resulting aescine crude product is successively subjected to salifying, decoloring and acetone precipitation to obtain a sodium aescinate crude product: the sodium aescinate crude product is purified by high-performance liquid chromatography, aescine A, B, C and D are collected and combined to obtain an aescine mixture, wherein same is then further desalinized by high-performance liquid chromatography, and the aescine pure product is collected and salified to obtain the sodium aescinate pure product. The semen aesculi is subjected to extraction and primary purification by an organic solvent, the use of the existing long-lasting processes, such as using macroporous adsorption resins, is avoided, and HPLC deep purification and desalinization steps are carried out on this basis, thereby generally achieving the purpose of significantly shortening the purification cycle and improving the total yield of sodium aescinate, and thus improving the production efficiency of sodium aescinate.

Description

technical field [0001] The invention relates to the technical field of plant extraction, in particular to a preparation method of sodium aescinate. Background technique [0002] Sodium aescinate is a saponin sodium salt extracted from the dried mature seeds of Aesculus aesculus. Modern pharmacological studies have shown that it has good pharmacological activity: it has strong anti-inflammatory and anti-exudation effects; And eliminate the formation of edema or hematoma; antioxidant free radicals and neuroprotective effect. Clinically, it is mainly used to treat swelling caused by trauma or surgery, cerebral edema, and venous reflux disorders. At the same time, it has been found to be effective in many diseases such as pulmonary heart disease, Hunt's syndrome, tumors, anal canal edema, facial neuritis, and type I nephrotic syndrome. Also has very good curative effect. [0003] Sodium aescinate mainly has 4 components, which are named sodium aescinin A, sodium aescinin B, so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008C07H15/256C07J63/00
Inventor 汪伟
Owner GANSU CHANGEE BIO PHARMA
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