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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, low total yield, and restrictions on the production efficiency of sodium aescinate, and achieve the effect of improving production efficiency

Active Publication Date: 2018-06-29
GANSU CHANGEE BIO PHARMA
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  • Summary
  • 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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  • Preparation method of sodium aescinate
  • Preparation method of sodium aescinate
  • Preparation method of sodium aescinate

Examples

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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 to decolorize 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 aescin...

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Abstract

The invention relates to the technical field of plant extraction and discloses a preparation method of sodium aescinate. The preparation method comprises the following steps: taking semen aesculin foralcohol extraction; extracting an obtained extract with chloroform, dichloromethane or ethyl acetate under acidic conditions; sequentially performing salification, decolorization and acetone precipitation on an obtained coarse product of aescine to obtain a coarse product of sodium aescinate; purifying the coarse product of sodium aescinate by a high performance liquid chromatography (HPLC); collecting aescines A, B, C and D; combining to obtain a mixture of the aescines; then, continuing to desalt by the HPLC; collecting a purified product of aescine; and salifying to obtain a purified product of sodium aescinate. The preparation method provided by the invention extracts and preliminarily purifies the semen aesculin by an organic solvent, avoids adopting macroporous adsorption resin andother existing time-consuming processes, and performs HPLC deep purification and desalination processes on this basis, so as to integrally achieve the purposes of significantly shortening a purification cycle and increasing a total yield of sodium aescinate and to improve 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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IPC IPC(8): C07J63/00
CPCC07J63/008C07H15/256C07J63/00
Inventor 汪伟
Owner GANSU CHANGEE BIO PHARMA
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