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A method for separating and purifying betulinic acid from lotus pod shells

A technology for separation and purification of betulinic acid, applied in organic chemistry, steroids, etc., can solve the problems of low technical content, waste of lotus resources, and lack of attention, and achieve simple process operation, save time, and reduce the use of reagents Effect

Active Publication Date: 2021-09-28
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is the agricultural waste generated during the processing of lotus seeds, which is currently only used for animal feed, or even randomly thrown on the roadside or ditch as waste, rotten and mildewed, or directly buried and incinerated; even if it is used, the method It is also relatively elementary and low in technical content, which not only causes environmental pollution, but also is a great waste of lotus resources
At present, there are only "sporadic" reports on the chemical components and medicinal effects of lotus pod shells at home and abroad, and they have not been paid attention to.

Method used

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  • A method for separating and purifying betulinic acid from lotus pod shells
  • A method for separating and purifying betulinic acid from lotus pod shells

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The raw material of the lotus pod shell is crushed, weighed 1kg, added 10L of 70% ethanol aqueous solution, pretreated in the flash extractor for 30min, then refluxed for 2h, obtained the extract by filtration, and added a mass fraction of 20% to the extract % sodium hydroxide solution adjusted to PH=8, concentrated to alcohol content of 10%; the concentrated solution was acid-adjusted, adjusted to pH=2 with hydrochloric acid, heated to reflux for 30 minutes, filtered after cooling, and the filtrate was treated with 20% sodium hydroxide The pH of the solution was adjusted to 10, and after standing for 10 hours, the precipitate was obtained by centrifugation, and the supernatant was discarded; low-polar petroleum ether was added to the precipitate for elution, and the fat-soluble substances in the precipitate were removed; 3 times the mass of methanol is thermally dissolved, and 10% activated carbon is added to the above dissolved solution, adsorbed at 60°C for 1h, filter...

Embodiment 2

[0031]The raw material of the lotus pod shell is crushed, weighed 1kg, added 20L of 80% ethanol aqueous solution, pretreated in the flash extractor for 10min, then refluxed for 1h, obtained the extract by filtration, and added a mass fraction of 5 % Potassium hydroxide solution adjusted to PH=10, concentrated to alcohol content of 30%; acid-adjusted the concentrated solution, adjusted to PH=3 with citric acid, heated to reflux for 60 minutes, filtered after cooling, and the filtrate was oxidized with 10% hydroxide The potassium solution was adjusted to PH=10, and after standing for 8 hours, the precipitate was obtained by centrifugation, and the supernatant was discarded; low-polarity n-hexane was added to the precipitate for elution, and the fat-soluble substances in the precipitate were removed; 3 times the mass of methanol is thermally dissolved, and 5% activated carbon is added to the above dissolved solution, adsorbed at 60° C. for 1 hour, filtered, and the filtrate is col...

Embodiment 3

[0033] The raw material of the lotus pod shell is crushed, weighed 1kg, added 15L of 60% ethanol aqueous solution, pretreated in the flash extractor for 20min, then refluxed for 1.5h, and the extract was obtained by filtration, and the mass fraction was added to the extract. After adjusting PH=9 with 15% sodium bicarbonate solution, concentrate to alcohol content of 20%; adjust acidity of the concentrated solution, adjust solution PH=4 with formic acid, heat and reflux for 60 minutes, filter after cooling, and filter the filtrate with 15% sodium carbonate The pH of the solution was adjusted to 11, and after standing for 10 hours, the precipitate was obtained by centrifugation, and the supernatant was discarded; low-polarity cyclohexane was added to the precipitate for elution, and the fat-soluble substances in the precipitate were removed; continue to add 3 times the mass of methanol is thermally dissolved, and 10% activated carbon is added to the above dissolved solution, adso...

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Abstract

The invention discloses a method for separating and purifying betulinic acid from lotus pod shells, which comprises the steps of extracting and concentrating lotus pod shells, acid-dissolving and alkali-precipitating, degreasing and decolorizing, and crystallizing. Discard the supernatant; add low-polar petroleum ether to the precipitate for eluting, remove the fat-soluble substances in the precipitate; continue to add methanol to the precipitate for thermal dissolution, adsorb on activated carbon, filter, collect the filtrate, and concentrate the filtrate; Stir and add water to the decolorized concentrated solution until the solution is slightly turbid, carry out crystallization, and collect the crystals by centrifugation. The invention solves the problems of repeated use of mixed solvents in the prior art, long column chromatography production cycle and low yield, which are unfavorable for industrial production, and quickly realizes the separation of active components and impurities through acid-dissolving and alkali-precipitation, simplifying the process route , can effectively increase the yield of betulinic acid.

Description

technical field [0001] The invention belongs to the technical field of plant effective active ingredient extraction, and in particular relates to a method for separating and purifying betulinic acid from lotus shells. Background technique [0002] Lotus (Nelumbo nucifera), family and genus: Nymphaeaceae, Nelumbo, perennial aquatic plant, herbaceous plant, has a planting history of more than 2,000 years in my country. At present, my country has more than 800 varieties of lotus, mainly distributed in Fujian, Zhejiang, Hubei, Hunan, Jiangsu, Anhui and Jiangxi. In addition to its ornamental value, lotus can also be used for food, drinking, medicine and packaging. The whole body of the lotus can be used everywhere. The lotus leaf can be used to treat upset heat, blood in the stool and metrorrhagia, etc.; the lotus seed heart can be used to treat insomnia and dreaminess, blood heat and vomiting blood, etc.; Eat aquatic vegetables. Lotus is rich in alkaloids, flavonoids, glycosi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 吴磊吴静谢传奇胡居吾熊伟李国群曹明源
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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