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Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf

A technology of loquat leaves and ursolic acid, applied in the directions of steroids, organic chemistry, etc., can solve the problems of small preparation amount, high safety requirements, toxic solvents, etc., and achieve the effect of increasing added value

Inactive Publication Date: 2011-03-16
桂林安和药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no ultrasonic extraction equipment in production, and this method is noisy, easy to damage hearing, and is not conducive to labor safety and protection
Due to the need for high pressure at room temperature and ultra-high pressure extraction, there are unsafe factors in the production process, requiring explosion-proof workshops and high-pressure-resistant equipment, which not only requires a large investment, but is also not easy to implement in production
[0011] It is widely reported in the literature that petroleum ether, chloroform, acetone and other toxic, flammable and explosive solvents are used in the separation of ursolic acid, which are not easy to control in production and have extremely high safety requirements.
Moreover, these solvents are toxic, harmful to humans, and easy to volatilize, which greatly increases production costs.
There are also reports in the literature that ursolic acid is prepared by thin layer preparation and silica gel chromatography separation, but on the one hand, the amount of preparation is very small, on the other hand, the production cycle is extremely long, and it needs to be eluted or developed with toxic and harmful solvents, which belongs to the laboratory The separation and preparation method cannot be realized in production at all
[0012] 2. The extraction technology is not perfect enough:
[0014] 3. The purity is not high:
[0015] At present, most of the ursolic acid products reported in the literature can be realized in production, the content is 92%~97%, and there are rare reports with more than 98%

Method used

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  • Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf
  • Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf
  • Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf

Examples

Experimental program
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Effect test

Embodiment 1

[0039] The process of separating and extracting ≥98% ursolic acid from loquat leaves includes the following steps:

[0040] (1) Cut into shreds: Take 800kg of fresh or sun-dried loquat leaves and cut into shreds with a medicine cutter, with a width of 0.5-2.0cm;

[0041] (2) Alcohol extraction and filtration: Put the shredded loquat leaves into 6cm 3 In the extraction tank, extract with 80% ethanol solution for 3 times. The amount of extraction solvent added is 6, 4, 6 times the weight of the medicinal material, that is, 4800L for the first time, 3200L for the second time, and 4800L for the third time. Extraction time It is 2.0, 1.5, 0.5h, and the extraction temperature is 70℃~80℃. Filter, combine the first two filtrates, and the third filtrates extract as the first extraction of the next batch of materials, and discard the residue;

[0042] (3) Concentrated precipitation: the first 2 combined filtrate was concentrated under vacuum to a material-liquid ratio of 1:0.7~1.2, that is, t...

Embodiment 2

[0056] Repeat Example 1 according to the same steps as described, but: step (2) is to extract 3 times with 85% ethanol; step (5) is to add 10 to 14 times the weight of the precipitate with 85% ethanol solution under constant stirring; Step (6) wash with 85% ethanol until the color of the liquid is extremely light; Step (12) add 85% ethanol with a concentration of 15 times the precipitation weight.

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Abstract

The invention discloses a process for extracting greater than or equal to 98% of ursolic acid from loquat leaf, which is characterized by the following steps: taking fresh loquat leaves or loquat leaves dried in the sun as a raw material, slicing, extracting with alcohol and filtering, concentrating and precipitating, centrifuging and filtering, dissolving in alcohol and filtering, purifying by ion exchange resin, neutralizing and concentrating, washing and drying, refining by silica gel, discoloring and filtering, concentrating and precipitating, crystallizing and vacuum drying. The invention has the advantages: (1) establishing a standard production line and associated equipment for industrial production of the ursolic acid, searching for a feasible process route, and realizing mass production of high-quality ursolic acid products; (2) solving the problem of purity of the current ursolic acid, wherein the content of the ursolic acid achieves greater than 98% of an HPLC level by analysis and detection; and (3) improving the added value of the loquat leaf and changing wastes into valuables.

Description

Technical field [0001] The invention relates to the extraction of ursolic acid, in particular to a process for separating and extracting ≥98% ursolic acid from loquat leaves. Background technique [0002] Ursolic acid, also known as ursolic acid and ursolic acid, is a pentacyclic triterpene compound of α-aromatic alcohol type. White, prismatic crystals (absolute ethanol), fine needle-like crystals (dilute ethanol). The melting point is 285℃~287℃, and the specific rotation [α]D is 25±67.5° (C=1, in 1mol / L sodium hydroxide). Ursolic acid is a ursane type pentacyclic triterpene, molecular formula C 30 H 48 O 3 , Molecular weight 456.68, its structural formula is as follows: [0003] [0004] Ursolic acid has significant hepatoprotective and anti-hepatitis effects. The clinical manifestations can significantly and rapidly reduce alanine aminotransferase, serum aminotransferase, reduce jaundice, increase appetite, anti-fibrosis and restore liver function. It has the characteristics o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 唐克军蒋红刚曾润清
Owner 桂林安和药业有限公司
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