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Preparation method for betulinic acid standard substance

A technology of betulinic acid and standard products, applied in the direction of steroids, organic chemistry, etc., can solve the problems of unstable product purity and unreachable purity, and achieve the effect of stable purity and simple operation

Inactive Publication Date: 2014-03-12
CHIFCON DRUG DISCOVERY SUZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, as disclosed in Chinese patent 200710025418.8, a method for preparing high-purity betulinic acid can obtain betulinic acid with a purity of more than 95%, but the purity of the product is unstable and still cannot reach the purity of a standard product

Method used

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Examples

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Effect test

Embodiment

[0017] A kind of betulinic acid standard substance preparation method of the present embodiment comprises the steps:

[0018] Step 1, crushing the collected sycamore bark into particles with a particle diameter of 3 to 5 mm;

[0019] Step 2, soak and wash with clean water 2 to 3 times, soak for 2 hours each time, to remove sediment and water-soluble sugar impurities;

[0020] Step 3, drain the particles washed in Step 2, soak and extract 3 times with 80% to 95% ethanol which is 5 times the weight of the bark, and combine the extracts for 24 hours each time;

[0021] Step 4, concentrating the extract obtained in Step 3 in a water bath at 60 degrees Celsius under reduced pressure to a saturated solution, cooling and crystallizing, filtering and drying to obtain a powdery solid;

[0022] Step 5, using petroleum ether to wash the powdery solid obtained in step 4 to remove some fat-soluble impurities;

[0023] Step 6, heat and dissolve the powdery solid treated in step 5 to a sat...

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PUM

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Abstract

The invention discloses a preparation method for a betulinic acid standard substance. The method comprises the following steps: first, collected oriental plane barks are crushed into particles; second, the barks are soaked and washed with clear water, and mud, sand and water-soluble carbohydrate impurities are removed; third, the washed particles obtained from the second step are drained, and soaked and extracted for 3 times with ethanol for 24h per time, and extraction solutions are mixed; fourth, the mixed extraction solution obtained from the third step is subjected to vacuum concentration in water bath at the temperature of 60 DEG C until a saturated solution is obtained, and after cooling, crystallization, filtration and drying, powdery solid is obtained; fifth, the powdery solid obtained from the fourth step is washed with petroleum ether; sixth, the processed powdery solid obtained from the fifth step is dissolved in methanol with water-bath heating until a saturated solution is obtained, insoluble substances are removed after filtration, the filtrated solution is permitted to stand for crystallization in a fume cupboard, and after filtration, needle-cluster shaped betulinic acid crystals are obtained. The prepared betulinic acid standard substance has a purity of being above 98%, the purity is stable, the operation is simple, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of natural products, in particular to a preparation method of a betulinic acid standard product. Background technique [0002] Betulinic acid is a pentacyclic triterpene, which can inhibit the growth of various tumor cells such as melanoma and lymphocytic leukemia cells, and has been widely reported in various reports. Betulinic acid was first found in birch trees and synthesized from betulin extracted from birch trees. Recently, experimental studies have found that the bark of the plane tree plant contains a high proportion of betulinic acid. In the prior art, a method for preparing high-purity betulinic acid disclosed in Chinese patent 200710025418.8 can obtain betulinic acid with a purity of more than 95% as a product, but the purity of the product is unstable and still cannot reach the purity of a standard product. Contents of the invention [0003] In view of the defects in the above-mentioned prior art, the p...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 沈金辉
Owner CHIFCON DRUG DISCOVERY SUZHOU
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