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Method for producing chlorogenic acids from fresh eucommia leaves

A technology of Eucommia eucommia chlorogenic acid and Eucommia eucommia fresh leaves, applied in chemical instruments and methods, separation/purification of carboxylate, preparation of carboxylate, etc. The effect of improved extraction rate, efficient extraction, and green production concept

Inactive Publication Date: 2014-08-13
HUNAN WORLD WELLBEING BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Jiang Xinyi compared and analyzed the traditional Soxhlet extraction method and ultrasonic extraction method. The test showed that the content measured by the ultrasonic extraction method was higher than that measured by the traditional Soxhlet extraction method; Liu Zonglin used the water extraction method to determine through orthogonal experiments Extraction frequency, time and pH value of active ingredients such as chlorogenic acid and quercetin in Eucommia ulmoides; Cheng Dejun used chloroform to degrease eucommia leaf powder, extracted chlorogenic acid with ethanol ultrasound, and then properly extracted and removed impurities, and established two A method for the production of thin-layer chromatography to separate and purify chlorogenic acid in Eucommia ulmoides leaves; Wang Hongwu used lead salt precipitation, acidified, extracted with ethyl acetate, and finally recrystallized to obtain pure chlorogenic acid; Qian Hua et al. The adsorption rate, adsorption speed and desorption rate of chlorogenic acid were compared comprehensively with porous resins. The results showed that AAS had the largest adsorption capacity, but it was difficult to be eluted; NKA-9 had a larger adsorption capacity and was easy to Desorbed, the elution peak is more concentrated, and the separation effect is better; NKA-Ⅱ has a larger adsorption capacity and is easier to be eluted, but the elution peak is gentle and not concentrated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Implementation example 1 Weigh 10 kg of fresh leaves of Eucommia ulmoides picked in May, beat with a beater, add 40L of pure water with a pH of 7 at 40°C, extract under ultrasonic conditions with a frequency of 20kHz for 30min, and filter to obtain a crude extract of eucommia chlorogenic acid; Add 400g chitosan to the crude extract of eucommia chlorogenic acid while stirring, mix and flocculate; then use 400g activated carbon to decolorize for 10min to obtain the sample solution of eucommia chlorogenic acid. Adsorb through the chromatography column of HPD826 resin until the adsorption is saturated; then wash with 1BV of distilled water at a flow rate of 1BV / h until colorless, and then use 20%, 40%, 60%, 80%, 95% volume concentration of 2BV respectively The edible ethanol was eluted step by step at a flow rate of 1BV / h, the eluent was collected separately, the eluent was concentrated at -0.05MPa and 45°C, the edible ethanol was recovered, and vacuum-dried at -0.05MPa and ...

Embodiment 2

[0023] Implementation Example 2 Weigh 10 kg of fresh leaves of Eucommia ulmoides picked in June, beat with a beater, add 60 L of pure water with a pH of 5 at 50 ° C, extract under ultrasonic conditions with a frequency of 30 kHz for 60 minutes, and filter to obtain a crude extract of eucommia chlorogenic acid. Add 600g chitosan while stirring and mix, after flocculation, then add 600g gac decolorization and obtain sample solution after 20min; This sample solution of 6.0BV is adsorbed by the chromatographic column of HPD826 resin with the flow rate of 2.5 BV / h, to Adsorption saturation; then wash with 2BV of distilled water at a flow rate of 2BV / h until colorless, and then use 20%, 40%, 60%, 80%, and 95% of the volume concentration of 2BV of edible ethanol step by step at a flow rate of 2BV / h Elution, collect the eluate separately, concentrate the eluate at -0.07MPa, 50°C, recover edible ethanol, vacuum-dry at -0.07MPa, 50°C, and obtain the purity of 28.35%, 91.25%, 98.81%, resp...

Embodiment 3

[0024] Implementation Example 3 Weigh 10kg of Eucommia fresh leaves picked in August, beat with a beater, add 80L of pure water with a pH of 4 at 60°C, extract for 90min under ultrasonic conditions with a frequency of 40kHz, add 800g of chitosan while stirring to mix, After flocculation, add 800g of activated carbon to decolorize for 30min to obtain the sample solution; 8.0BV of the sample solution is adsorbed through the chromatography column of HPD826 resin at a flow rate of 3.0 BV / h until the adsorption is saturated; then 3BV of distilled water is used to Rinse at a flow rate of 3BV / h, then use 20%, 40%, 60%, 80%, and 95% of the volume concentration of 2BV of edible ethanol to elute step by step at a flow rate of 3BV / h. Concentrate at -0.09MPa and 55°C, recover edible ethanol, and vacuum-dry at -0.09MPa and 60°C to obtain chlorogenic acid products with a purity of 24.36%, 87.43%, 97.81%, 84.67%, and 58.69%, respectively. The recovery rate was 93.75%.

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Abstract

The invention provides a method for producing chlorogenic acids from fresh eucommia leaves. The method comprises the following steps: firstly, pulping the fresh eucommia leaves so as to obtain eucommia leaf pulp; then adding purified water to the eucommia leaf pulp, and carrying out ultrasonic-assisted extraction so as to obtain eucommia chlorogenic acid crude extracting liquid; flocculating the eucommia chlorogenic acid crude extracting liquid by using chitosan, and decolorizing the eucommia chlorogenic acid crude extracting liquid by using activated carbon so as to obtain eucommia chlorogenic acid loading liquid; and finally adsorbing the eucommia chlorogenic acid loading liquid by using a chromatographic column, and carrying out stepwise elution so as to obtain eucommia chlorogenic acids with different purities. The method has the advantages that the purified water is used for safe nontoxic extraction, separation and purification so as to obtain the eucommia chlorogenic acids, the lost of effective components in an eucommia leaf harvesting aftertreatment process is effectively avoided, the high-effective extraction of the the eucommia chlorogenic acid is realized, the production cost of the eucommia chlorogenic acid is aslo greatly reduced, and the idea of green environment-friendly protection and energy-saving and consumption reducing production is fully embodied.

Description

technical field [0001] The invention relates to a method for producing chlorogenic acid, in particular to a method for producing chlorogenic acid from fresh leaves of Eucommia ulmoides. Background technique [0002] Eucommia ( Eucommia Ulmoides Olive ) is a plant of the genus Eucommia in the family Eucommia, a deciduous tree. my country has a very wide area suitable for the growth of Eucommia, and the land that can be used to plant Eucommia is more than 10 million hectares. At present, the cultivation area of ​​Eucommia in China is about 350,000 hectares, accounting for more than 99% of the total planting area of ​​Eucommia in the world. It has unique resource advantages. It can produce 4 million tons of leaves. [0003] Chlorogenic acid( Chlorogenic acid , referred to as CA) belongs to the phenylpropanoid compounds, is a class of organic acids containing carboxyl and o-diphenol groups, chemical name 3-caffeoylquinic acid. Chlorogenic acid widely exists in higher dicotyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/56C07C67/62
CPCC07C67/48C07C69/732
Inventor 盛达成肖文军刘家波冯林
Owner HUNAN WORLD WELLBEING BIOTECH
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