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A method for extracting high-purity chlorogenic acid from aerial parts of honeysuckle

A technology of aerial parts and honeysuckle, applied in chemical instruments and methods, separation/purification of carboxylic acid esters, preparation of carboxylic acid esters, etc., can solve the problem of low purity of the extraction rate of chlorogenic acid, and achieve low cost and clean The effect of deconcentration and simple process

Active Publication Date: 2016-08-24
山东禾本堂生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After testing, the extraction rate and purity of the chlorogenic acid obtained by the above enzymatic extraction are not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take the leaves of honeysuckle, crush, take 50g of coarse powder, add 1.0L 70% ethanol aqueous solution (0.5-1mol / L hydrochloric acid to adjust pH2.5), reflux for 1h, filter while hot, and repeat the extraction of medicine residue once. The sub-filtrates were combined to obtain 1.85L of the extract. Take 1.5L of the extract and concentrate to 300mL, mix with the unconcentrated extract, and let stand for 8h. The lower layer of the solution has obvious dark green precipitates. Vacuum filtration to obtain the filtrate is further concentrated. To dry powder, add 300-400mL of deionized water to dissolve the dry powder and adjust pH 3 with 1M hydrochloric acid aqueous solution (calculated as chlorogenic acid content 5.4mg / mL), which is the loading solution of macroporous adsorption resin column chromatography. Take 500mL of AB-8 macroporous adsorption resin, firstly pretreat the AB-8 macroporous adsorption resin (column diameter of 5.5cm, column length of 25cm) according to the...

Embodiment 2

[0019] Take 50g of the crude powder of honeysuckle, add 1.0L of 70% ethanol / dilute hydrochloric acid aqueous solution (0.5-1mol / L hydrochloric acid to adjust pH4), reflux and extract for 2h, filter, repeat extraction of medicine residue once, suction filter, combine the two filtrates , Get the total extract 1.8L, take 1.5L of the extract and concentrate to 200mL, mix it with the unconcentrated extract, let stand for 8h, filter with suction to remove the dark green precipitate, collect the filtrate, and further concentrate to dry powder, add 300 -400mL of distilled water was dissolved, and the solution was adjusted to pH 3.5 with 0.5mol / L dilute hydrochloric acid solution, the chlorogenic acid content in the solution was 4.0mg / mL, and then subjected to X-5 macroporous adsorption resin resin column chromatography. Take 500mL of X-5 macroporous adsorption resin, firstly pretreat the X-5 macroporous adsorption resin (column diameter: 5.5cm, column length: 25cm) according to the inst...

Embodiment 3

[0021] Take 50g of the coarse powder of honeysuckle above ground, add 500mL of deionized water, heat to 45°C, adjust pH3 with 0.5mol / L, add 10mg of cellulase (enzyme activity 300), enzymatically hydrolyze for 2h. After the enzymolysis is completed, add 20mg of acid protease (enzyme activity 1000), enzymolysis for 2h, after enzymolysis is completed, the temperature is raised to 80°C to inactivate the enzyme for 30min. Reflux the filtered residue with 800mL deionized water at 82°C for 1.5h, repeat the water extraction once, filter with suction, and combine the three filtrates to obtain a total of 2.0L of the filtered filtrate. The extraction liquid is concentrated to a dry powder. Use deionized water for this dry powder. 350mL was dissolved, and then 1.0mol / L hydrochloric acid was used to adjust the pH to 2.5. The concentration of chlorogenic acid in the solution was 6.0mg / mL. The solution was further separated and purified by a macroporous adsorption resin. First, pack 500mL of ...

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Abstract

The invention discloses a method of extracting chlorogenic acid with high purity from a honeysuckle above ground part, and belongs to the technical field of traditional Chinese medicine extraction of active ingredients. The method takes the honeysuckle above ground part as raw materials, and the chlorogenic acid with high purity can be acquired through the following steps that step 1,reflux extraction are conducted twice by 60-80% of ethanol solutions at the PH of 2 to 5, or the reflux extraction are conducted twice by adding cellulases and acid proteinases into acid water at the PH of 2 to 5 at the temperature of 40-60 DEG C; step 2, extracting solutions acquired in step 1 are concentrated according to a certain proportion and stay 4-12 hours at indoor temperature, and precipitated sediments are removed by suction filtration; step 3, the filter liquor needs to be concentrated until no alcohol taste exists, and then attenuated with the acid water; further depuration is conducted through macroreticular resins, and chlorogenic acid with the purity higher than 90% can be acquired. Chlorogenic acid acquired through the method is in high purity, and the method is simple, green and environmental friendly, low in cost, and suitable for being applied in the industrial production.

Description

Technical field [0001] The invention belongs to the technical field of extracting active ingredients of traditional Chinese medicine, and specifically relates to a method for extracting high-purity chlorogenic acid from the aerial part of honeysuckle. Background technique [0002] Honeysuckle, the scientific name Lonicera japonica Thurb, is a plant of the genus Lonicera japonica. It has the functions of clearing away heat and detoxifying, dissipating heat from the cool breeze, anti-virus, protecting the liver and promoting gallbladder. The main chemical constituents in honeysuckle are chlorogenic acid, isochlorogenic acid, flavonoids, linalool, divinyl alcohol, etc. Modern research generally believes that the biologically active ingredients of honeysuckle are chlorogenic acid compounds, and the quality of honeysuckle is often evaluated by the content of chlorogenic acid. [0003] Chlorogenic acid is an organic acid containing carboxyl groups and ortho-diphenolic hydroxyl groups. I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/48C07C67/56
CPCC07C67/48C07C67/56C07C2601/14C07C69/732
Inventor 王彩芳潘宣张呈瑞
Owner 山东禾本堂生物科技有限公司
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