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Preparation method of high-purity chlorogenic acid

A chlorogenic acid, high-purity technology, applied in the field of preparation of high-purity chlorogenic acid, can solve the problems of reducing the purity of chlorogenic acid, poor impurity removal effect, impurity cannot be completely removed, etc., to reduce energy consumption and save solvents cost, consumption reduction effect

Inactive Publication Date: 2020-04-21
成都乐美天医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned prior art scheme has the following defects: 1. Impurities such as sugar and protein contained in the extract cannot be completely removed, which will reduce the overall purity of the obtained chlorogenic acid; 2. Purification is carried out by macroporous resin adsorption, washing The removal speed is fast, but the impurity removal effect is not good

Method used

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

Examples

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Effect test

Embodiment 1

[0034] The invention discloses a preparation method of high-purity chlorogenic acid, which comprises the following steps:

[0035] S1. Pretreatment: Take 10g of honeysuckle medicinal material, pulverize, pass through a 100-mesh sieve, add 150g of pure water, stir evenly, and soak for 4 hours;

[0036] S2. Extraction: add hydrochloric acid to adjust the pH value to 3, heat to 50°C for extraction, filter, add 150g of pure water again, heat to 50°C for extraction, filter, and combine the filtrates to obtain 300ml of primary extract;

[0037] S3. Purification: Put the primary extract obtained in S2 directly on a polyamide column, use eluents with 10vol%, 20vol%, 30vol%, and 40vol% ethanol concentrations for gradient elution, and collect eluents with 20vol% ethanol concentrations. Deliquification and eluted fractions are obtained to obtain a secondary extract;

[0038] S4. Extraction: Concentrate the secondary extract in S3 to 60ml to obtain a tertiary extract, add 250ml of ethyl ...

Embodiment 2

[0041] The invention discloses a preparation method of high-purity chlorogenic acid, which comprises the following steps:

[0042] S1. Pretreatment: take 10g of honeysuckle medicinal material, pulverize, pass through a 100-mesh sieve, add 200g of pure water, stir evenly, and soak for 3 hours;

[0043] S2. Extraction: add hydrochloric acid to adjust the pH value to 3, heat to 50°C for extraction, filter, add 200g of pure water again, heat to 50°C for extraction, filter, and combine the filtrates to obtain 400ml of primary extract;

[0044] S3. Purification: Put the primary extract obtained in S2 directly on a polyamide column, use eluents with 10vol%, 20vol%, 30vol%, and 40vol% ethanol concentrations for gradient elution, and collect eluents with 20vol% ethanol concentrations. Deliquification and eluted fractions are obtained to obtain a secondary extract;

[0045] S4. Extraction: Concentrate the secondary extract in S3 to 50ml to obtain a tertiary extract, add 200ml of ethyl ...

Embodiment 3

[0048] The invention discloses a preparation method of high-purity chlorogenic acid, which comprises the following steps:

[0049] S1. Pretreatment: Take 10g of honeysuckle medicinal material, pulverize, pass through a 100-mesh sieve, add 250g of pure water, stir evenly, and soak for 2 hours;

[0050] S2. Extraction: add hydrochloric acid to adjust the pH value to 3, heat to 50°C for extraction, filter, add 250g of pure water again, heat to 50°C for extraction, filter, and combine the filtrates to obtain 500ml of primary extract;

[0051] S3. Purification: Put the primary extract obtained in S2 directly on a polyamide column, use eluents with 10vol%, 20vol%, 30vol%, and 40vol% ethanol concentrations for gradient elution, and collect eluents with 20vol% ethanol concentrations. Deliquification and eluted fractions are obtained to obtain a secondary extract;

[0052] S4. Extraction: Concentrate the secondary extract in S3 to 45ml to obtain a tertiary extract, add 180ml of ethyl ...

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Abstract

The invention relates to a preparation method of high-purity chlorogenic acid. The method comprises the following steps: S1, taking a honeysuckle medicinal material, crushing, adding into 15-25 timesby weight of pure water, and soaking for 2-4 hours; S2, adding hydrochloric acid to adjust the pH value to 3-4, heating to 45-60 DEG C, extracting twice, and filtering to obtain a first-stage extracting solution; S3, directly loading the first-stage extracting solution obtained in the step S2 on a polyamide column, performing gradient elution by adopting an eluent containing 10-40 vol% of an extracting agent, and collecting the fractions to obtain a second-stage extracting solution; S4, concentrating the second-stage extracting solution obtained in the step S3 to 8-20% of the original volume of the first-stage extracting solution so as to obtain a third-stage extracting solution, adding ethyl acetate according to a volume ratio of the third-stage extracting solution to the ethyl acetate of1:(3.5-4.5), extracting twice, and combining filtrates to obtain a fourth-stage extracting solution; and S5, concentrating the fourth-stage extracting solution obtained in the step S4 under reduced pressure until the volume of the fourth-stage extracting solution is 75-88% of the original volume of the fourth-stage extracting solution, and refrigerating and crystallizing to obtain the chlorogenicacid. The method has the advantages that impurities are removed to a large extent, and the purity of chlorogenic acid is effectively improved.

Description

technical field [0001] The invention relates to the technical field of chlorogenic acid extraction, in particular to a preparation method of high-purity chlorogenic acid. Background technique [0002] Chlorogenic acid is a phenylpropanoid substance synthesized by plants in the process of aerobic respiration. Honeysuckle is a raw material commonly used to extract chlorogenic acid at present. The main active ingredients in honeysuckle are organic acids mainly composed of chlorogenic acid and flavonoids mainly composed of luteolin. In addition, there are some sugars, macromolecules such as proteins. Chlorogenic acid has strong pharmacological activity. Studies have shown that it has pharmacological effects on the digestive system, blood system and reproductive system. It has a significant inhibitory effect on Staphylococcus aureus, hemolytic streptococcus, Shigella, and typhoid bacillus; it has a significant effect on leukocyte feeding syndrome caused by radiotherapy and chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C69/732C07C67/56
CPCC07C67/48C07C67/56C07C2601/14C07C69/732
Inventor 张光兰
Owner 成都乐美天医药科技有限公司
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