Method for extracting chlorogenic acid and hederagenin from honeysuckle flower

A technology of hedera saponin and chlorogenic acid, which is applied in the separation/purification of carboxylic acid esters, organic chemistry, fermentation, etc., and can solve unfavorable industrial production, low yield of chlorogenic acid, pollution of chlorogenic acid, etc. problems, to achieve the effect of benefiting the purification of chlorogenic acid, mild conditions, and improving the utilization rate

Inactive Publication Date: 2012-05-09
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of chlorogenic acid is not high and the purity is low by the water extraction lime milk precipitation method; the supercritical fluid extraction method is expensive and is not conducive to industrial production; the membrane separation method has a certain limit on the pore size; the lead salt precipitation uses toxic heavy metals , polluted by chlorogenic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Grind honeysuckle, take 1kg, put it into an extraction tank, add 15kg90% ethanol solution and heat to 55°C for extraction for 2 hours, filter the liquid with suction, add 10kg90% ethanol solution to extract once, extract the extract under reduced pressure and recover the ethanol solution to obtain a concentrated solution, Add 4L water to the concentrated solution, add 1L SPD-100 macroporous resin column for adsorption, the flow rate is 1L / h, after the adsorption is completed, the water washing sugar reaction is negative, and then eluted with 7L 60% ethanol solution, collect the eluent and recover ethanol under reduced pressure, Add 1L of water saturated n-butanol to extract 5 times, recover n-butanol, and add appropriate amount of water to adjust pH4 with hydrochloric acid to get the concentrated solution, add 5g of cellulase, enzymolyze at 55°C for 30h, filter the concentrated enzymolyzed solution, and the solid Reflux with 500ml of absolute ethanol to dissolve and filt...

Embodiment 2

[0021] Grind honeysuckle, take 1kg, put it into an extraction tank, add 15kg of 70% ethanol solution and heat to 70°C for extraction for 1 hour, filter the liquid with suction, add 15kg of 70% ethanol solution to extract twice, extract the extract under reduced pressure and recover the ethanol solution to obtain a concentrated solution, Add 1L of water to the concentrate to disperse, add 1L of AB-8 macroporous resin column for adsorption, the flow rate is 2kg / h, after the adsorption is completed, the sugar reaction of washing with water is negative, then elute with 5L of 80% ethanol solution, collect the eluate and recover ethanol under reduced pressure, Add 4L of water-saturated n-butanol to extract 4 times, recover n-butanol, add appropriate amount of citric acid to the concentrated solution to adjust pH5, add 5g of cellulase to enzymatically hydrolyze at 40°C for 24 hours, filter the concentrated enzymatic hydrolyzate, and use 600ml for solids Reflux the absolute ethanol to ...

Embodiment 3

[0023] Grind honeysuckle, take 1 kg, put it into an extraction tank, add 12 kg of 80% ethanol solution and heat to 60°C for extraction for 1 hour, filter the liquid with suction, add 15 kg of 80% ethanol solution to extract twice, extract the extract under reduced pressure and recover the ethanol solution to obtain a concentrated solution, Add 2L of water to the concentrate to disperse, add 1L of LSA-21 macroporous resin column for adsorption, the flow rate is 1kg / h, after the adsorption is completed, the reaction of sugar washing with water is negative, then elute with 6L of 70% ethanol solution, collect the eluate and recover ethanol under reduced pressure, Add 5L of water-saturated n-butanol to extract 3 times, recover n-butanol, add appropriate amount of water and adjust the pH to 4 with sulfuric acid, add 2g of β-glucosidase at 50°C for 48h, concentrate the enzymolysis solution and filter, use 500ml of solid matter Reflux the absolute ethanol to dissolve, place the crystal...

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PUM

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Abstract

The invention relates to a method for extracting chlorogenic acid and hederagenin from honeysuckle flower. The method is characterized by comprising the following steps of: smashing the honeysuckle flower; extracting with a 70-90 percent ethanol solution; recovering ethanol from an extracting solution under reduced pressure; adding water into a concentrated solution for dispersing; adding into a macroporous resin column for adsorbing; eluting with a 40-70 percent of ethanol solution; recovering ethanol from an eluent and adding n-butyl alcohol for extracting; recovering n-butyl alcohol; adjusting the pH of the concentrated solution to 4-7, and adding a biological enzyme for performing enzymolysis; concentrating a hydrolysate; and filtering to obtain a solid and a filtrate; and purifying the solid and the filtrate respectively to obtain a hederagenin product and a chlorogenic acid production. The method has simple process operation and high raw material utilization ratio, and is suitable for industrial production.

Description

Technical field: [0001] The invention belongs to the technical field of natural product separation, and in particular relates to a method for extracting chlorogenic acid and hedera saponin from honeysuckle. Background technique: [0002] Chlorogenic acid, molecular formula C 16 h 18 o 9 , 3-Caffeoylquinic acid, the hemihydrate is needle crystal (water), and becomes an anhydrous compound at 110°C. Soluble in water, ethanol and acetone, very slightly soluble in ethyl acetate. [0003] Hedera saponin, the molecular formula is C 30 h 48 o 4 , (3beta, 4alpha)-3,23-dihydroxyolean-12-ene-28-acid, soluble in ethanol, methanol, acetic acid, hydroxide alkali solution, insoluble in water, ether, benzene, chloroform and petroleum ether. [0004] Honeysuckle is the dried flower bud of Lonicerae Lonicerae, which has the effect of clearing away heat and detoxification, and dispersing wind-heat. It is used for carbuncle and furuncle, sore throat, erysipelas, pyretic toxin, bloody d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P33/00C07C69/732C07C67/48
Inventor 李法庆杨成东刘东锋
Owner 苏州宝泽堂医药科技有限公司
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