Method for extracting isoferulic acid from radix clematidis

A technology of isoferulic acid and extraction method, applied in the field of extraction, can solve the problems such as the decline of effective components ferulic acid and isoferulic acid, the increase of the cost of removing acid, the cumbersome extraction process, etc., to achieve true and reliable results, process safety, good repeatability

Inactive Publication Date: 2019-11-08
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in recent years, with the sharp rise in prices, the local cohosh has been plundered and collected, and now the wild cohosh resources have been depleted day by day. It is found in the research report on the impact of the artificial cultivation that the main active components of ferulic acid and isoferulic acid in Cimicifuga have decreased. Therefore, it is of great significance to study the extraction and separation of isoferulic acid from other plants.
And isoferulic acid is one of the active ingredients in Clematis clematis, and there is no report on extracting isoferulic acid from Clematis clematis at present
At the same time, the existing method for extracting isoferulic acid from Cimicifuga is generally required to add ethanol-water mixed solution to soak for 12 hours, and then add appropriate amount of hydrochloric acid to extract by ultrasonic or decocting. This extraction method takes a long time and the extraction process is cumbersome. And adding acid reagents (in order to inhibit acid hydrolysis), increasing the cost of subsequent acid removal

Method used

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  • Method for extracting isoferulic acid from radix clematidis
  • Method for extracting isoferulic acid from radix clematidis
  • Method for extracting isoferulic acid from radix clematidis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] S1. Extraction method: crush Clematis clematis, pass through a 60-mesh sieve to obtain Clematis clematis powder, and pack it into a bag for later use; weigh 10 g of Clematis clematis powder and add 150 mL of ethyl acetate solution, heat and reflux at 60 ° C for extraction, and the extraction time is 120min, the number of extractions is 2 times, the 2 extracts are combined and filtered, the filtered extract is added to a rotary evaporator to concentrate under reduced pressure, the concentrated water temperature is 60 ° C, and the speed is 5 files to obtain the crude extract of isoferulic acid ;

[0043] S2. Detection

[0044] (1) Dilute the isoferulic acid standard with the mobile phase to prepare the standard solution. The specific configuration steps are as follows:

[0045] Accurately weigh 20 mg of isoferulic acid standard substance, place it in a 25mL volumetric flask, dilute with mobile phase, shake well, and set the volume to the mark to obtain a standard solutio...

Embodiment 2

[0055] S1. Extraction method: crush Clematis clematis, pass through a 60-mesh sieve to obtain Clematis clematis powder, and pack it into a bag for later use; weigh 10 g of Clematis clematis powder and add 150 mL of ethyl acetate-acetic acid solution, heat and reflux at 60 ° C to extract, extract The time is 120min, the number of extractions is 2 times, the 2 extracts are combined and filtered, and the filtered extract is added to a rotary evaporator to concentrate under reduced pressure, the concentrated water temperature is 60°C, and the speed is 5 gears to obtain crude isoferulic acid. Extract;

[0056] S2. Detection

[0057] The detection method is the same as in Example 1.

[0058] S3. Separation and purification: Weigh 2g of the extract obtained from S1, add 30ml of 40% methanol-water solution to dissolve, centrifuge at 4200r / min for 30min, take the supernatant, separate and purify by semi-preparative HPLC, and semi-preparative HPLC Chromatography is reversed-phase chro...

Embodiment 3

[0061] S1. Extraction method: crush Clematis clematis, pass through a 40-mesh sieve to obtain Clematis clematis powder, and pack it into a bag for later use; weigh 10 g of Clematis clematis leaf powder, add 100 mL of ethanol-formic acid aqueous solution, and extract under reflux at 80 ° C. The extraction time is 60min, the number of extractions is 2 times, the 2 extracts are combined and filtered, the filtered extract is added to a rotary evaporator to concentrate under reduced pressure, the concentrated water temperature is 60 ° C, and the speed is 5 files to obtain the crude extract of isoferulic acid ;

[0062] S2. Detection

[0063] The preparation method of standard solution and need testing solution is with embodiment 1;

[0064] The standard solution and the test solution were analyzed by HPLC respectively. HPLC chromatographic conditions: the chromatographic column is Venusil XBPC18; the mobile phase is acetonitrile-0.5% acetic acid aqueous solution (26:74, V / V); the ...

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Abstract

The invention discloses a method for extracting isoferulic acid from radix clematidis. The extraction method comprises the following steps: crushing the radix clematidis, performing sieving by a 40-80-mesh sieve, weighing radix clematidis powder, adding the weighed radix clematidis powder into an organic solvent, wherein a mass-to-volume ratio of the radix clematidis powder to the organic solventis 1 g:(10-20) mL, performing heating reflux extraction, wherein the extraction temperature is 60-100 DEG C, the extraction time is 30-120 min and the extraction times are 1-3 times, merging the extraction liquids, performing filtration, and performing concentration on the filtered extraction liquid to dryness to obtain crude isoferulic acid extract. The method provided by the invention has the advantages of simple operation, good repeatability and good stability; and only ethyl acetate, ethanol, glycerin, lactic acid, citric acid, glacial acetic acid, formic acid, methanol and acetonitrile are used in the processes of extraction, separation and purification, organic solvents such as chloroform and benzene which are harmful to the environment and human bodies are not used, so that the method is safe, green and environmentally friendly in the whole process, and opens up a novel way to obtain the isoferulic acid.

Description

technical field [0001] The invention relates to an extraction method, in particular to a method for extracting isoferulic acid from Clematis clematis. Background technique [0002] Clematis chinensis Osbeck., Clematis chinensis Osbeck., Clematis manshurica Rupr., and Clematis manshurica Rupr. are the dry roots and rhizomes of Clematis chinensis Osbeck., Clematis manshurica Rupr. Pulse spasm, flexion and extension disadvantage. The chemical components in Clematis are complex, mainly including triterpenoid saponins, flavonoids, coumarins, alkaloids and small molecular organic acids, among which organic acids include ferulic acid, isoferulic acid, vanillic acid, etc. Modern According to pharmacological studies, organic acids have anti-inflammatory, detoxification, analgesic and other pharmacological effects. The content of isoferulic acid in Clematis is higher than that of other organic acids. [0003] Isoferulic acid, molecular formula C 10 h 10 o 4 , The pure product is...

Claims

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Application Information

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IPC IPC(8): C07C59/64C07C51/48C07C51/42
CPCC07C51/42C07C51/48C07C59/64
Inventor 张海江许晨新郑海东马婷婷戴宁付欣欣
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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