Method for extracting iridoid active site and monomer from eucommia bark

A technology for iridoids and active parts, which is applied in the field of extracting iridoid active parts and monomers from Eucommia ulmoides, can solve the problems of rough processing technology, low technological content, cumbersome operation, etc., and improve product purity and production efficiency. Efficiency, saving organic reagents, and improving product quality

Inactive Publication Date: 2008-09-10
JISHOU UNIVERSITY
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AI Technical Summary

Problems solved by technology

There are shortcomings such as low yield, complex process, cumbersome operation, and high cost, and there are no research reports suitable for large-scale production
Although there are many varieties of eucommia products in China, their technological content is low, their processing techniques are rough, and most of them are repeated at a low level, and the comprehensive utilization rate of raw materials is low (for example, the utilization rate of leaves is less than one-thirtieth).
[0004] Previous studies failed to provide a feasible method for obtaining the active site of eucommia iridoids. For the simultaneous extraction and separation of various iridoid monomers from various raw materials (especially leaves and seeds) of eucommia , has not yet been reported

Method used

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  • Method for extracting iridoid active site and monomer from eucommia bark

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) The ulmoides bark is dried, crushed, and sieved, preferably the fresh bark of ulmoides ulmoides. Weigh 20 kg of the treated bark of Eucommia, adopt conventional extraction, add 70% ethanol-water solution as the extractant at a liquid-solid ratio of 15 times, extract at 60°C for 2 hours, and repeat 3 times. Filter the extract, concentrate, and adjust the pH to 1.5-4.5 with hydrochloric acid;

[0024] (2) Use n-butanol to extract, collect the extract, cool the concentrated solution to -10~-20°C, then place it in a freeze dryer and cool it to -45~-65°C, vacuum degree ≤ 20Pa, time 24~48 hours Low-temperature vacuum drying to obtain 480.5 grams of iridoid active parts, with a total iridoid compound content of 53.20%;

[0025] (3) 2.5000 grams of iridoid active sites are dissolved, separated by preparative high-performance liquid chromatography, and the used column packing is C 18 or C 8 , the particle size is 5-50 μm, and the mobile phase is ethanol-water system for g...

Embodiment 2

[0029] (1) Eucommia leaves are dried, crushed, and sieved, and it is better to pick Eucommia leaves in November. Weigh 500 grams of treated Eucommia leaves and use ultrasonic extraction, add 50% ethanol at a liquid-solid ratio of 18 times, ultrasonically extract for 30 minutes at a temperature of 60° C. and a frequency of 80 KHz, and repeat the treatment 3 times. Filter and concentrate the extract;

[0030] (2) Adsorption and elution with a weakly polar adsorbent, concentration of the eluent, and low-temperature vacuum drying using the method of Example 1, to obtain the iridoid active site (content: 51.21%);

[0031] (3) Dissolving 2.5000 g of the iridoid active site, using HPLC preparative chromatography to separate (the method is the same as in Example 1), and collecting GPA, GP, and AU fractions respectively;

[0032] (4) Concentrate and freeze-dry the above fractions respectively to obtain powdered GPA461 mg, GP51 mg and AU410 mg. High-performance liquid chromatography a...

Embodiment 3

[0034](1) Eucommia seeds are dried, crushed and sieved. The processed eucommia seeds are weighed, and the linolenic acid is firstly extracted with supercritical carbon dioxide to obtain the seed meal. Weigh 200 grams of eucommia seed meal, extract by microwave, add 25% ethanol to microwave for 35 seconds at a liquid-solid ratio of 40 times, and repeat the treatment 4 times. Filter and concentrate the extract, and adjust the pH to 1.5-4.5 with hydrochloric acid;

[0035] (2) extracted with ethyl acetate and n-butanol, collected the extract, and dried in vacuum at low temperature using the method of Example 1 to obtain the iridoid active site (content: 51.11%);

[0036] (3) 2.5000 grams of iridoid active sites were dissolved, and the method of Example 1 was used for separation by high-performance liquid chromatography, and GPA, GP, and AU fractions were collected respectively;

[0037] (4) The above fractions are concentrated and freeze-dried respectively to obtain 55 mg of po...

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Abstract

The invention discloses a method for extracting active sites of iridoid, and extracting monomer geniposidic acid (GPA), geniposide(GP) and aucubin(AU) from eucommia, wherein raw materials are extracted by taking the eucommia(husk, leaf or seed) as materials and utilizing the conventional leaching method, the ultrasonic extraction method or the microwave extraction method, and an extracting solution is preliminarily purified by methods such as the solvent extraction and the adsorption separation of special adsorbents, etc., and thus the active sites of the iridoid(the total content of the iridoid is no less than 50 percent) is obtained, and GPA, GP and AU undergo the separation, low temperature condensation, refrigeration and drying by using the preparation high pass filter technique and taking an alcohol-water solution as the mobile phase to obtain monomers of GPA, GP and AU, contents of which are all no less than 90 percent. The preparation method disclosed by the invention utilizes novel process of the extraction and separation, and can simultaneously prepare a plurality of monomer products of the eucommia, and provides scientific foundations for the comprehensive development and utilization of the eucommia; moreover, the whole process does not use solvents harmful to human bodies, thereby realizing the green preparation.

Description

technical field [0001] The invention relates to a method for treating iridoids (iridoids) compounds in Eucommia ulmoides Oliv. and its active monomers geniposidic acid (GPA), geniposide (GP) and peach A method for preparing phyllobulin (aucubin, AU). Background technique [0002] Eucommia ulmoides is a perennial deciduous tree in the Eucommia family Eucommia genus endemic to my country. It is a precious Chinese medicinal material, which has the functions of nourishing the liver and kidney, strengthening bones and muscles, anti-abortion and lowering blood pressure. The chemical composition of Eucommia ulmoides is very complex, and one of the most promising active parts is iridoids, including geniposide (GPA), geniposide (GP) and aucubin (AU ), etc., they exist in Eucommia bark, Eucommia leaves and Eucommia seeds (samara). Studies have shown that iridoids have excellent effects such as prevention and treatment of high blood pressure, refreshing, anti-fatigue, enhancing immun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04A61K36/46
Inventor 彭密军张敏周春山彭胜
Owner JISHOU UNIVERSITY
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