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Extraction method of high-purity chlorogenic acid

An extraction method and technology of chlorogenic acid, which are applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems affecting the economic development value of chlorogenic acid products, and the instability of chlorogenic acid extraction and purification processes , Increase production energy consumption and cost, etc., to achieve the effect of reducing environmental governance costs, ensuring energy efficiency and product quality, and low production costs

Inactive Publication Date: 2013-10-02
GUANGXI JINHAO BIO TECH
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The main disadvantages of this method are: (1) the method adopts directly soaking honeysuckle leaves and eluting the soaking liquid to obtain chlorogenic acid, because the solubility of chlorogenic acid in water at 25°C is about 4%, and the chlorogenic acid in honeysuckle leaves at normal temperature The amount of acid soluble in soaking liquid is few, causes the waste of chlorogenic acid resource in honeysuckle leaf, directly affects the extraction amount of product, thereby reduces the economic value of chlorogenic acid resource development in honeysuckle leaf; (2) this method successively through three times of soaking, Purified water and ethanol are eluted twice, and the production steps are 7 steps in total. The extraction purity of the obtained chlorogenic acid is between 35% and 95%. The instability of acid extraction and purification process affects the quality of chlorogenic acid products and directly affects the economic development value of chlorogenic acid products; (3) in the production process, it only takes 10-14 hours to stand still in various steps, and the elution method used The additive ethanol is food grade, which further increases the production energy consumption and cost
美国专利US4872987、德国专利DE3603574和DE3239219、欧洲专利EP1405566、国际专利申请WO2006093114和WO2006080333、日本专利JP4145049、JP4145048、JP2005263632、JP2006174746、JP2007031392和JP2007322823等公开的制备高纯度绿原酸的技术方案均是在粗 On the basis of the above, modern separation methods are further adopted, such as macroporous adsorption resin adsorption separation, ion exchange column separation, polyamide or dextran gel chromatography, etc. for further refining of chlorogenic acid; Chinese patents CN1398845, CN1762972, CN1616403 , CN1687008, CN1524843, and CN1435406 disclosed chlorogenic acid refining methods all adopt column chromatography separation, and the adsorption filler involved includes macroporous adsorption resin, ion exchange resin and polyamide, in view of the phenolic hydroxyl group contained in chlorogenic acid is easy to oxidize, The enolate bond is easy to hydrolyze and the intramolecular ester group is easy to migrate. Although chromatography can prepare chlorogenic acid with higher purity, it cannot achieve efficient separation. Oxidation and isomerization of chlorogenic acid make the yield decrease, and this The cost of the method is high and the production intensity is limited; the refining methods of chlorogenic acid disclosed in Chinese patents CN1616402, CN1746149, CN1740137, CN1425643, CN1273964 and CN1273964 all use solvent extraction and column chromatography, that is, use solvent extraction to obtain the crude product before using Column chromatography refining, this method can obtain higher purity chlorogenic acid, but the extraction agent ethyl acetate used in the solvent extraction process has high water solubility and high residue in water, which affects the purity of chlorogenic acid products and increases the degree of water pollution , and the method steps are cumbersome, the solvent recovery consumes a lot of energy, the production cost is high, and it is not suitable for industrial scale-up

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  • Extraction method of high-purity chlorogenic acid
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  • Extraction method of high-purity chlorogenic acid

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Embodiment 1

[0032] A method for extracting high-purity chlorogenic acid, the specific steps of the method are as follows:

[0033] Step 1 Honeysuckle preparation and pretreatment

[0034] Wash the honeysuckle with clean water, put it in an oven, first dry it in an oven at 50°C for 30 minutes, and then pass it through a 20-mesh sieve after being pulverized by a pulverizer. Put down the honeysuckle raw material, and then grind it in a corundum mortar for 30 minutes, pass through a 200-mesh sieve, and return the honeysuckle raw material that has not been sieved to the mortar to continue grinding. The honeysuckle material that is sieved is the pretreated honeysuckle raw material;

[0035] Step 2 Enzyme Treatment

[0036] After step one is finished, according to the quality of honeysuckle raw material after the pretreatment: the quality of enzyme: the ratio of the volume of water is the ratio of 1g: 0.04g: 40ml, and described enzyme is the composite of cellulase, ligninase and cex enzyme. En...

Embodiment 2

[0048] A method for extracting high-purity chlorogenic acid, the specific steps of the method are as follows:

[0049] Step 1 Eucommia leaf preparation and pretreatment

[0050] Wash the eucommia leaves with clean water, place them in an oven, and dry them in an oven at 60°C for 30 minutes, then pass them through a pulverizer and pass through a 20-mesh sieve. Collect the eucommia leaf raw material under the sieve, and then grind it in a corundum mortar for 30 minutes, pass through a 200-mesh sieve, and return the eucommia leaf raw material that has not been sieved to the mortar for further grinding. The eucommia leaf material under the sieve is the pretreated Eucommia leaf raw material;

[0051] Step 2 Enzyme Treatment

[0052] After step 1 is finished, according to the quality of eucommia leaf raw material after pretreatment: the quality of enzyme: the ratio of the volume of water is the ratio of 1g: 0.04g: 40ml, and described enzyme is cellulase, ligninase and cex enzyme ...

Embodiment 3

[0059] A method for extracting high-purity chlorogenic acid, the specific steps of the method are as follows:

[0060] Step 1 sunflower seed preparation and pretreatment

[0061] Wash the sunflower seeds with clean water, place them in an oven, and dry them in an oven at 55°C for 30 minutes, then pass them through a grinder and pass through a 20-mesh sieve, return the sunflower leaves that have not been screened to the grinder and grind them again , collect the sunflower seed raw material under the sieve, and then grind it in a corundum mortar for 30 minutes, pass through a 200-mesh sieve, and return the sunflower seed raw material that has not been sieved to the mortar for further grinding. The sunflower seed material under the sieve is the pretreatment After sunflower seed raw material;

[0062] Step 2 Enzyme Treatment

[0063]After step 1 is finished, according to the quality of sunflower seed raw material after pretreatment: the quality of enzyme: the ratio of the volume...

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Abstract

The invention relates to an extraction method of high-purity chlorogenic acid, which comprises the steps of raw material preparation and pretreatment, enzyme treatment, ultrasonic treatment, preparation of the chlorogenic acid product, and the like. In the preparation process, an inorganic membrane is used, wherein the support of the inorganic membrane is alumina ceramic or honeycomb ceramic, and the inorganic membrane is an alumina composite microfiltration membrane. The raw material is honeysuckle flower, eucommia, cacao tree, coffee or the like. When the raw material is the honeysuckle flower, the extraction rate of the chlorogenic acid is up to 97.5%, and the purity is up to 99%. The method provided by the invention can simply and quickly obtain stable-quality high-purity high-yield safe reliable chlorogenic acid from the raw material.

Description

technical field [0001] The invention belongs to the technical field of chlorogenic acid extraction, and in particular relates to a method for extracting high-purity chlorogenic acid. Background technique [0002] Chlorogenic acid is an ester formed by caffeic acid and quinic acid, which belongs to phenylpropanoid compounds and is mainly found in plants such as honeysuckle, Eucommia, cocoa and coffee. As an important raw material for drug synthesis, chlorogenic acid has a significant effect on the prevention and treatment of cardiovascular system diseases and diabetes. It is also widely used in food preservation, anti-aging in cosmetics, and obesity prevention. It has broad applications in the fields of medicine and population health. market application prospects. However, chlorogenic acid itself is unstable. During the extraction process from plants, conditions such as high temperature, strong light, and long-term heating can accelerate the hydrolysis of chlorogenic acid an...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/48C07C67/56C07C67/58
Inventor 叶春袁煜昊胡永明李文华刘洪军
Owner GUANGXI JINHAO BIO TECH
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