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Method for separating and purifying ursolic acid from rosemary

A technology of separation and purification, ursolic acid, applied in the direction of organic chemistry, steroids, etc., to achieve the effect of short time-consuming, low cost, simple and safe method

Inactive Publication Date: 2019-12-10
湖南先伟阳光生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the defective that extracts ursolic acid technology existence in the existing rosemary, the purpose of the invention is to improve a kind of method that separates and purifies ursolic acid from rosemary, and this method utilizes solubility in the separation and purification process The difference is that the pickling step is added. This step can effectively remove impurities that are more polar than ursolic acid and similar to ursolic acid. It has a great purification effect on the subsequent acid precipitation step and can reduce the number of recrystallizations. , obtain high-purity ursolic acid through the synergistic effect of each step

Method used

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  • Method for separating and purifying ursolic acid from rosemary
  • Method for separating and purifying ursolic acid from rosemary

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0028] A method for isolating and purifying ursolic acid from rosemary, the steps comprising:

[0029] 1) Take 200g of dried rosemary leaves, heat and reflux them with 1000ml 85% ethanol-water solution twice, extract 1.5h each time, filter to get 1900ml filtrate ①; concentrate the filtrate ① under reduced pressure to 150ml, add 600ml water, place Cool; filter to obtain 60g of filter cake ①, and stir the filter cake ① with 300ml of 3% acetic acid-50% ethanol-water solution for 1h;

[0030] 2) Filtrate to obtain 50g filter cake ②, filter cake ② reflux extraction with 400ml 3% sodium bicarbonate-80% ethanol aqueous solution for 1.5h; filter to obtain 400ml filtrate ②, add 1.2g activated carbon to the filtrate ② for decolorization for 30min;

[0031] 3) filter to get 400ml filtrate 3., add 3% phosphoric acid-water solution to filtrate 3. until precipitate no longer occurs, suction filter to get filter cake 3., filter cake 3. carry out crystallization treatment with ethanol-water s...

experiment example 2

[0033] A method for preparing ursolic acid from rosemary, the steps comprising:

[0034] 1) Take 200g of dried rosemary leaves, heat and reflux them with 1200ml 90% ethanol-water solution for 2 extractions, extract for 1 hour each time, and filter to obtain 2200ml filtrate①; Concentrate the filtrate① under reduced pressure to 140ml, add 420ml of water, place to cool Filter to get 68g filter cake ①, filter cake ① is stirred 50min with 800ml 2% citric acid-80% ethanol-water solution;

[0035] 2) Filter to obtain 60g filter cake ②, filter cake ② was extracted with 540ml 5% sodium carbonate-90% ethanol-water solution for 50min under reflux; filter to obtain 540ml filtrate ②, filtrate ② was decolorized with 1g activated carbon for 40min;

[0036] 3) filter to get 540ml filtrate ③, add 3% acetic acid-water solution to the filtrate until no precipitate occurs, suction filter to get filter cake ③, filter cake ③ is crystallized with ethanol-water solution again, the crystallization con...

experiment example 3

[0038] A method for preparing ursolic acid from rosemary, the steps comprising:

[0039]1) Take 200 g of dried rosemary leaves, heat and reflux them with 1600 ml of 80% ethanol aqueous solution for 3 times, extract for 1 hour each time, and filter to obtain 4600 ml of filtrate ①; concentrate the filtrate ① to 320 ml under reduced pressure, add 760 ml of water, and let it cool; Filter to get 50g filter cake ①, and stir the filter cake ① with 500ml 2% acetic acid-60% ethanol-water solution for 1h;

[0040] 2) Filter to obtain 60g of filter cake ②, filter cake ② with 600ml 2% sodium hydroxide-90% ethanol-water solution for reflux extraction for 1h; filter to obtain 600ml of filtrate ②, filtrate ② plus 3g of activated carbon for decolorization for 30min;

[0041] 3) filter to get 600ml filtrate ③, add 3% hydrochloric acid-water solution to the filtrate until the precipitate no longer occurs, and suction filter to get the filter cake ③, and the filter cake ③ is crystallized with et...

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Abstract

The invention provides a method for separating and purifying ursolic acid from rosemary, wherein the method comprises the following steps: 1) taking dried rosemary leaves, carrying out reflux extraction on the dried rosemary leaves by an ethanol-water solution, and filtering to obtain a filtrate 1; concentrating the filtrate 1 under reduced pressure, adding water, and standing for cooling; filtering to obtain a filter cake 1, and stirring the filter cake 1 with an acid-ethanol-water solution; 2) filtering to obtain a filter cake 2, and carrying out reflux extraction on the filter cake 2 by analkali-ethanol-water solution; and filtering to obtain a filtrate 2, and adding activated carbon into the filtrate 2, and decolorizing; and 3) filtering to obtain a filtrate 3, adding an acid-water solution into the filtrate 3 until no precipitate appears, carrying out suction filtration to obtain a filter cake 3, and repeatedly crystallizing the filter cake 3 by an ethanol-water solution. According to the method, a pickling step is added in the separation and purification process by utilizing different dissolvability, impurities with polarity larger than that of ursolic acid and similar to that of ursolic acid can be effectively removed in the pickling step, a great purification effect is achieved on the subsequent acid precipitation step, the recrystallization frequency can be reduced, and high-purity ursolic acid is obtained.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction of effective plant components, and in particular relates to a method for separating and purifying ursolic acid from rosemary. Background technique [0002] Rosemary is a perennial evergreen shrub of the family Lamiaceae, which is native to Europe and the Mediterranean coast of northern Africa. Its flowers and leaves can extract natural antioxidants and rosemary essential oil. The antioxidant components contained in rosemary mainly include ursolic acid, rosmarinic acid, carnosic acid, carnosol, etc. [0003] Ursolic acid is a pentacyclic triterpenoid compound in free form or combined with sugar to form glycosides, which exists in natural plants. Studies have shown that ursolic acid has anti-inflammatory, anti-bacterial, anti-cancer, sedative, hypoglycemic, anti-diabetic functions, and because of its obvious anti-oxidation function, it is widely used as raw materials in medicine a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 罗伟姚慧
Owner 湖南先伟阳光生物科技有限公司
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