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Method for separating and purifying aucubin from leaves of eucommia ulmoides oliv with NKA-2 macroporous adsorption resin

A technology of aucubin and NKA-2, which is applied in the field of green chemical technology, can solve the problems of high equipment cost, low purity and yield, and difficult separation, and achieve operation and product safety, advanced technology, and environmental friendliness Effect

Inactive Publication Date: 2012-10-03
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the macroporous adsorption resins used for the separation and purification of aucubin mainly include S-8 resin and HZ-820 resin, but the yield and purity of separation and purification are not good
[0008] Eucommia ulmoides leaves contain many types of compounds with great difference in polarity (from polar to non-polar); there are many isomers in the same type of compounds, and their differences are small, so it is difficult to separate, some of which are heat sensitive Strong, but also easy to oxidize, isomerize and decompose
Obviously, although the above-mentioned extraction, separation and purification method of Eucommia leaf aucubin can prepare Eucommia leaf aucubin extract with a certain purity and yield, due to the limitation of technical means and the use of a large amount of toxic Organic solvents or chemical preparations make the product obviously have defects such as poor safety or low purity and yield, high equipment cost, and insufficient product quality and market competitiveness.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The cleaned NKA-2 macroporous adsorption resin was selected as the separation and purification resin of Eucommia aucubin, and the above-mentioned crude extract of aucubin was prepared with 60% volume concentration and neutral pH value of edible ethanol to a concentration of 0.3 mg / mL solution. 3.0 BV of the solution is passed through a separation column equipped with NKA-2 macroporous adsorption resin at a flow rate of 3.0 BV / h for adsorption and separation. After the adsorption is saturated, it is washed with 2 BV of distilled water at a flow rate of 1.5 BV / h until it is colorless. Then use 2.0BV of edible ethanol with a volume concentration of 50% to elute aucubin at a flow rate of 3.0BV / h, collect the eluate, concentrate the eluate at -0.07MPa, 50°C, and recover edible ethanol , vacuum freeze-drying to obtain purified aucubin extract, the measured yield of aucubin was 82.02%, and the purity was 50.37%.

Embodiment 2

[0023] The cleaned NKA-2 macroporous adsorption resin was selected as the separation and purification resin of Eucommia aucubin, and the above-mentioned crude extract of aucubin was prepared with 50% volume concentration and neutral pH value of edible ethanol to a concentration 0.2 mg / mL solution. Pass 2.5 BV of the solution through a separation column equipped with NKA-2 macroporous adsorption resin at a flow rate of 2.0 BV / h for adsorption and separation. After the adsorption is saturated, first wash it with 1 BV of distilled water until colorless at a flow rate of 1 BV / h. Then use 1.5 BV of edible ethanol with a volume concentration of 40% to elute aucubin at a flow rate of 2.0BV / h, collect the eluate, concentrate the eluate at -0.05MPa, 45°C, and recover edible ethanol , freeze-dried in vacuum to obtain purified aucubin extract, the measured yield of aucubin was 77.11%, and the purity was 49.3%.

Embodiment 3

[0025] The cleaned NKA-2 macroporous adsorption resin was selected as the separation and purification resin of Eucommia aucubin, and the above-mentioned crude extract of aucubin was prepared with 70% volume concentration and neutral pH value of edible ethanol to a concentration of 0.4 mg / mL solution. Pass 3.5 BV of the solution through a separation column equipped with NKA-2 macroporous adsorption resin at a flow rate of 4.0 BV / h for adsorption and separation. After the adsorption is saturated, first wash it with 3 BV of distilled water at a flow rate of 2 BV / h until it is colorless. Then use 2.5 BV of edible ethanol with a volume concentration of 60% to elute aucubin at a flow rate of 4.0 BV / h, collect the eluate, concentrate the eluate at -0.09MPa, 55°C, and recover edible ethanol , vacuum freeze-drying to obtain purified aucubin extract, the measured yield of aucubin was 78.06%, and the purity was 48.73%.

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Abstract

The invention discloses a method for separating and purifying aucubin from leaves of eucommia ulmoides oliv with an NKA-2 macroporous adsorption resin, which comprises the following steps: extracting the crude extract of aucubin from leaves of eucommia ulmoides oliv with neutral eatable alcohol, and separating and purifying the crude extract of aucubin with the NKA-2 macroporous adsorption resin to obtain an aucubin extract. According to the method, the aucubin is extracted and separated with the eatable alcohol safely and non-toxically, so that not only aucubin extracts of different purities can be industrially produced safely and efficiently, but also the safe, convenient, rational and economic high-value utilization of eucommia ulmoides oliv resources and the industrial production of a series of products are implemented, and furthermore, an environment-friendly chemical production idea and an economy circulation policy are fully reflected.

Description

Technical field: [0001] The invention relates to a green chemical technology for separating and purifying aucubin from eucommia leaves, in particular to a green separation and purification method for separating and purifying aucubin from eucommia leaves by using NKA-2 macroporous adsorption resin. Background technique: [0002] Eucommia Ulmoides Olive is a deciduous tree of Eucommia ulmoides. my country has a very wide area suitable for the growth of Eucommia, and the land that can be used to plant Eucommia reaches 10 million hm 2 Above, the current national cultivation area of ​​Eucommia is about 350,000 hm 2 , accounting for more than 95% of the total planting area of ​​Eucommia ulmoides in the world, and has unique resource advantages. Our country can produce 4 million tons of leaves every year. [0003] The chemical name of aucubin (aucubin, AU) is β-D-glucopyranoside, which is an iridoid glycoside compound with a bitter taste. Liver, anti-tumor, anti-bacterial, anti-...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 肖文军崔丽龚志华
Owner HUNAN AGRICULTURAL UNIV
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