Method for extracting betulinic acid from firmiana bark

A technology of sycamore tree and betulinic acid, which is applied in the field of extracting betulinic acid, can solve the problems of difficult products, complex components, and only 2-3% yield, and achieve the effect of low cost, high efficiency, and simple and easy method

Inactive Publication Date: 2011-10-05
NANJING FORESTRY UNIV
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Problems solved by technology

But usually because the content of betulinic acid in the bark is very little (about 5~8wt%), and bark extracts the composition complex, contains a lot of polar substances, it is difficult to obtain pure product by the way that solvent extracts
[0003] Chinese patent 200710025418.8 discloses a method for preparing high-purity betulinic acid. First, it is extracted 2 to 4 times with ethanol or ethyl acetate, and finally crystallized with water to obtain colorless and transparent crystals of betulinic acid with a purity of more than 95%. Yield is only 1.8-2%
[0005] German patent DE19713768A1 discloses a method for extracting betulinic acid with ethyl acetate and other hydrophobic organic solvents to obtain betulinic acid crystals with higher purity, but it is also achieved in repeated operations of multi-stage extraction and recrystallization, resulting in rate is only 2-3%

Method used

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  • Method for extracting betulinic acid from firmiana bark
  • Method for extracting betulinic acid from firmiana bark
  • Method for extracting betulinic acid from firmiana bark

Examples

Experimental program
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Embodiment 1

[0025] Get 500g of sycamore bark, add 1000mL of clear water, heat and boil for half an hour, filter with suction, add an equal volume of water after removing the filtrate, boil again for 1 hour, and remove the filtrate again. Subsequently, add 600mL of methanol to the boiled bark, soak at room temperature for 24 hours, and concentrate the filtrate obtained by suction filtration at 30°C under reduced pressure, remove the methanol solvent, and obtain betulinic acid crystal powder, which is dried in the presence of phosphorus pentoxide Dry under reduced pressure at room temperature for 24 hours to obtain 28.5 grams of betulinic acid refined product, with a yield of 5.70%, a purity of 95.8%, and a melting point of 315.8°C. The infrared spectrum, hydrogen nuclear magnetic resonance spectrum, carbon nuclear magnetic resonance spectrum, and mass spectrum of the betulinic acid product See Figure 1~4 .

Embodiment 2

[0027] Get 300g of sycamore bark, add 500mL of clear water, heat and boil for 40 minutes, filter with suction, add 350mL of water after removing the filtrate, boil for the second time for 2 hours, and remove the filtrate again. Subsequently, 400 mL of acetone was added to the boiled bark, soaked at room temperature for 26 hours, the filtrate obtained by suction filtration was concentrated under reduced pressure at 40°C, and the acetone solvent was removed to obtain betulinic acid crystal powder, which was dried in the presence of phosphorus pentoxide Dry under reduced pressure at room temperature for 20 hours. 16.3 grams of refined betulinic acid were obtained, with a yield of 5.43%, a purity of 95.9%, and a melting point of 316.5°C.

Embodiment 3

[0029] Take 600g of sycamore bark, add 800mL of water, heat and boil for one hour, filter with suction, remove the filtrate, add 750mL of ethanol directly to the boiled bark, soak at room temperature for 24 hours, filter with suction, and then use a small amount of ethanol Wash the bark, combine the washings, concentrate the resulting combined solution under reduced pressure at 50°C, and remove the ethanol solvent to obtain betulinic acid crystal powder. After air drying, dry under reduced pressure at room temperature for 30 hours in the presence of phosphorus pentoxide. 32.8 grams of refined betulinic acid were obtained, with a yield of 5.46%, a purity of 95.4%, and a melting point of 317°C.

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Abstract

The invention discloses a method for extracting betulinic acid from firmiana bark, which comprises the following steps of: collecting firmiana bark, adding water, boiling, filtering to remove water, adding a hydrophilic organic solvent to the boiled bark, soaking and extracting at room temperature, filtering, collecting the filtrate, concentrating at reduced pressure to volatilize the hydrophilic organic solvent and drying to obtain betulinic acid. The method for extracting betulinic acid from firmiana bark uses hot water extraction for pre-treatment and uses the hydrophilic organic solvent for extraction, thus directly extracting high-purity betulinic acid from firmiana bark, all betulinic acid in firmiana bark is basically extracted, and the method is simple and feasible and has high efficiency and low cost; and the purity of the extracted betulinic acid is more than 95% and the yield reaches 5.7%.

Description

technical field [0001] The invention belongs to the technical field of extracting traditional Chinese medicines, and in particular relates to a method for extracting betulinic acid from the bark of the sycamore family. Background technique [0002] Betulinic acid is a physiologically active substance, which has anti-cancer, anti-infection, anti-inflammation, anti-AIDS and other functions. It is usually prepared by oxidizing betulin or extracting it from the bark of the sycamore family with a solvent. However, usually because the content of betulinic acid in the bark is very small (about 5-8wt%), and the components extracted from the bark are complex and contain many polar substances, it is difficult to obtain a pure product by solvent extraction. [0003] Chinese patent 200710025418.8 discloses a method for preparing high-purity betulinic acid. First, it is extracted 2 to 4 times with ethanol or ethyl acetate, and finally crystallized with water to obtain colorless and tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 任浩大森茂俊
Owner NANJING FORESTRY UNIV
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