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Preparation method of corosolic acid as blood sugar reducing active ingredient

The technology of an active ingredient, corosolic acid, is applied in the field of preparation of corosolic acid, an active ingredient for hypoglycemia, and it can solve the problems of high loss rate of corosolic acid, high viscosity, high content of water-soluble impurities, and high total production cost. problems, to achieve the effect of simple pretreatment and posttreatment, high sample recovery rate, and less solvent consumption

Inactive Publication Date: 2017-09-26
CHANGSHA BROAD OCEAN BIO SCI & TECHN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the separation and preparation of corosolic acid often use repeated column chromatography and other methods, and the lack of fast and simple methods limits its application.
[0005] Chinese patent application 200710009556.7, Chen Jianfeng et al. reported the method for the separation and preparation of corosolic acid from loquat leaves. Under alkaline conditions, filter while hot to remove impurities and decolorize with activated carbon. The loquat leaf extract is enriched and purified with macroporous adsorption resin for corosolic acid. The content of sexual impurities is very high, which seriously limits the adsorption capacity and selectivity of macroporous adsorption resins to corosolic acid, resulting in a small total yield of corosolic acid, high production costs, and high purity of corosolic acid prepared. low
[0006] Chinese patent 200810071064.5, Chen Jianfeng reported a method for extracting corosolic acid from plants, which includes boiling water-soluble substances to remove impurities, alkaline organic solvent extraction of total triterpene acids and macroporous adsorption resin for corosolic acid Enrichment and purification steps, macroporous adsorption resin chromatography in this method also has the problems of small total yield of corosolic acid and high total production cost

Method used

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  • Preparation method of corosolic acid as blood sugar reducing active ingredient
  • Preparation method of corosolic acid as blood sugar reducing active ingredient
  • Preparation method of corosolic acid as blood sugar reducing active ingredient

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Take the dried Evodia rutaecarpa and grind it, add methanol according to the ratio of liquid to material ratio of 1:10, and conduct ultrasonic extraction for 20 minutes under the condition of ultrasonic power of 600W and 40°C for 3 times, concentrate the extract under reduced pressure, recover methanol, get the extract;

[0032] (2) The above-mentioned extract is dissolved in a sodium hydroxide solution of pH=10, and after being fully stirred evenly, it is left to stand, filtered, and insoluble matter is removed, and after the solution is neutralized by 1mol / L hydrochloric acid, an equal amount of ethyl acetate is added to extract 3 Once, collect the ethyl acetate extract, concentrate and recover the solvent, and obtain the crude extract;

[0033] (3) The above crude extract was separated by TBE-300A high-speed countercurrent chromatography. The specific steps are: prepare a two-phase solvent system of n-hexane, ethyl acetate, methanol and water in a separatory fun...

Embodiment 2

[0035] (1) Take the dried Evodia rutaecarpa and crush it, add 80% ethanol according to the ratio of liquid to material ratio 1:8, and conduct ultrasonic extraction for 20 minutes under the conditions of ultrasonic power 600W and 40°C, extract 3 times, concentrate the extract under reduced pressure, and recover methanol to obtain extract;

[0036] (2) The above extract is dissolved in a sodium hydroxide solution with a pH of 10, stirred well, left to stand, filtered to remove insoluble matter, and the solution is neutralized by 0.5mol / L sulfuric acid, then extracted by adding an equal amount of ethyl acetate 3 times, collect the ethyl acetate extract, concentrate and recover the solvent, and obtain the crude extract;

[0037] (3) The above crude extract was separated by TBE-300A high-speed countercurrent chromatography. The specific steps are: prepare a two-phase solvent system of n-hexane, ethyl acetate, methanol, and water in a separatory funnel, mix them in a volume ratio o...

Embodiment 3

[0039] (1) Grind the dried Evodia rutaecarpa, add 60% methanol according to the ratio of liquid to material ratio of 1:12, and conduct ultrasonic extraction for 20 minutes under the condition of ultrasonic power of 600W and 40°C for 3 times, concentrate the extract under reduced pressure, and recover methanol to obtain extract;

[0040] (2) The above-mentioned extract is dissolved in a sodium hydroxide solution of pH=10, and after being fully stirred evenly, it is left to stand, filtered, and insoluble matter is removed, and after the solution is neutralized by 0.4mol / L phosphoric acid, an equal amount of ethyl acetate is added to extract 3 times, collect the ethyl acetate extract, concentrate and recover the solvent, and obtain the crude extract;

[0041] (3) The above crude extract was separated by TBE-300A high-speed countercurrent chromatography. The specific steps are: prepare a two-phase solvent system of n-hexane, ethyl acetate, methanol, and water in a separatory funnel...

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Abstract

The invention discloses a method for separating and preparing corosolic acid as a blood sugar reducing active ingredient from Eleutherococcus evodiaefolius. The method comprises the following steps: (1) after pulverizing the Eleutherococcus evodiaefolius, carrying out ultrasonic extraction on the pulverized Eleutherococcus evodiaefolius to obtain extracting liquid, and concentrating the extracting liquid to obtain an extract; (2) dissolving the extract in a sodium hydroxide solution, removing undissolved substances, after neutralizing the solution via acid, extracting the solution with ethyl acetate, collecting an ethyl acetate extracting solution, and concentrating a recycling solvent to obtain a crude extract; and (3) separating the crude extract by high speed counter-current chromatography, carrying out online detection by using an ultraviolet detector, collecting fraction components, concentrating under reduced pressure, crystalizing and drying to obtain the corosolic acid. The corosolic acid is prepared by the method. The method has the advantages that the extracting rate is high, an operation process is simple, energy consumption is low, the preparation method is pollution-free, the recycling rate is high, the quality is good, the activity of physiological activators is protected, and the like. Industrial amplification is facilitated.

Description

technical field [0001] The invention belongs to the field of natural organic chemistry, and relates to a preparation method of plant insulin corosolic acid, a hypoglycemic active ingredient. Background technique [0002] Corosolic acid, 2α-hydroxyursolic acid, trade name: phytoinsulin, is a triterpenoid compound present in plants such as Lagerstroemia indica, loquat, and nasturtium. Corosolic acid is a white amorphous powder, soluble in petroleum ether, benzene, chloroform and other organic solvents, insoluble in water, soluble in hot ethanol and methanol. Under anhydrous conditions, there will be a color reaction or fluorescence. Corosolic acid belongs to α-aryl-type or ursane-type pentacyclic triterpenoids, and its basic skeleton is the pentacyclic core of polyhydropine. Corosolic acid can exist freely in plants or in the form of saponins. In plants, it often exists together with its isomer maslinic acid, which has similar structure and chemical properties and is diffi...

Claims

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Application Information

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IPC IPC(8): C07J63/00A61P3/10
CPCC07J63/008
Inventor 邹亲朋戴玲刘向前
Owner CHANGSHA BROAD OCEAN BIO SCI & TECHN CO LTD
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