Method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme

A honeysuckle leaf, catalytic activation technology, applied in organic chemistry, separation/purification of carboxylic acid esters, etc., can solve the problem of chlorogenic acid extraction and purification process instability, affecting the economic development value of chlorogenic acid products, and increasing production energy consumption. and cost issues, to achieve the effect of ensuring extraction energy efficiency and product quality, reducing environmental treatment costs, and low production costs

Inactive Publication Date: 2013-05-08

王星敏

7 Cites 11 Cited by

AI-Extracted 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 ...

Abstract

The invention discloses a method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme, belonging to the technical field of chlorogenic acid extraction. According to the method, the solid waste of Lonicera japonica leaves, used as raw material, is prepared into the target product by the simple processes of treatment on Lonicera japonica leaves, enzymatic hydrolysis, ultrasonic wave synergistic digestion and chlorogenic acid preparation. The raw material used in the method provided by the invention is cheap and easily available, and the method has the characteristics that the waste is fully used, the prepared chlorogenic acid product is high in extraction ratio and purity and complete in biological activity, energy consumption in production process is low, the production equipment is hardly corroded, the consumption of organic solvent is low, environment protection is facilitated, and so on. The method provided by the invention can be widely used for extracting natural products, such as chlorogenic acid, isochlorogenic acid and Ginnol, from the solid waste of Lonicera japonica leaves, and effectively realizes the resource utilization of the Lonicera japonica leaves.

Application Domain

Carboxylic acid esters separation/purification

Technology Topic

ChemistryDigestion +11

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Examples

Experimental program(5)
Effect test(1)

Example Embodiment

[0020] Example 1

[0021] The specific steps of an enzyme-catalyzed activation method for extracting chlorogenic acid from honeysuckle leaves are as follows:

[0022] (1) Raw material pretreatment

[0023] Wash the honeysuckle leaves, dry them, place them in an oven, bake them in an oven at 100°C for 60 minutes, then take them out, pulverize them with a pulverizer, and sieve them through a 60 mesh molecular sieve to obtain honeysuckle leaves with a particle size of less than 60 meshes. Use a plastic bag Divide and spare.

[0024] (2) Enzymatic hydrolysis reaction

[0025] After the completion of step (1), the volume ratio of the mass of the solid waste of honeysuckle leaf after pretreatment in step (1): the mass of enzyme: water is 1:0.1:25. The enzyme is ligninase: cellulase in a mass ratio of 1:2. Add the compound enzyme and water to the raw materials pretreated in step (1). After stirring, adjust the pH of the system to 4 with sulfuric acid solution, and then place the pH-adjusted mixture in a shaker. After enzymatic hydrolysis and activation were carried out at a water bath temperature of 45°C for 11 hours, the filtrate and filter residue were collected by suction filtration with a suction filter pump. The collected filter residue is the honeysuckle leaf enzymatically activated base material, and the collected filtrate is discharged after treatment reaches the standard.

[0026] (3) Ultrasonic collaborative extraction

[0027] After step (2) is completed, first transfer the honeysuckle leaf enzymatically activated base material obtained in step (2) into a 250ml extraction container, and then follow the quality of the honeysuckle leaf solid waste pretreated in step (1) : The ratio of the volume of the ethanol solution is 1:12. Add the ethanol solution to the extraction vessel, stir and mix uniformly, and ultrasonicate for 30 minutes at an ultrasonic power of 100W and a temperature of 30°C, and then use a suction filter to perform suction filtration. Collect the filtrate and filter residue. The filter residue is collected as a raw material for preparing the adsorption material; the filtrate is transferred to a centrifuge tube, and the centrifuge is centrifuged for 10 minutes at a centrifuge speed of 3000 r/min, and then the upper centrifuge clear liquid and the centrifuge residue are collected. The collected supernatant centrifugal liquid is obtained as an extract containing chlorogenic acid; the collected centrifugal residue is used as the raw material for preparing the adsorption material.

[0028] (4) Preparation of chlorogenic acid products

[0029] After step (3) is completed, first take 1 ml of the chlorogenic acid-containing extract obtained in step (3), and measure the concentration of chlorogenic acid by a spectrophotometer. Under the condition that the detection wavelength is 329nm and the volume solubility of the ethanol solution is 62.5%, the chlorogenic acid solution of the centrifuged supernatant collected in step (3) is determined. Then place the centrifugal clear liquid collected in step (3) in a rotary evaporator, under a vacuum pressure of 0.2Mpa and a temperature of 50°C, under reduced pressure and concentration to a viscous form to obtain crude chlorogenic acid. Then, according to the ratio of the mass of crude chlorogenic acid: the volume of ethanol is 1:5, the crude chlorogenic acid and the ethanol solution are added to the extraction vessel, and the mixture is uniformly dissolved. Finally, through a rotary evaporator, under a vacuum pressure of 0.2Mpa and a temperature of 50°C, vacuum concentration is repeated 3 times to obtain a chlorogenic acid product. The extraction rate of chlorogenic acid is as high as 97.0%, and the purity is as high as 92.2%.

Example Embodiment

[0030] Example 2

[0031] An enzyme-catalyzed method for extracting chlorogenic acid from honeysuckle leaves is the same as that in Example 1, wherein:

[0032] In step (1), the honeysuckle leaf mesh number is 160 meshes, the oven temperature is 110°C, and the drying time is 30 minutes.

[0033] In step (2), the volume ratio of the mass of honeysuckle leaf solid waste: the mass of enzyme: water is 1:0.05:5, and the mass ratio of the enzyme is ligninase:cellulase is 1:0.5. The pH value of the system is adjusted to 8 with hydrochloric acid solution, and the temperature of the water bath is 65°C. Enzymatic hydrolysis activates honeysuckle leaf base material for 2h.

[0034] In step (3), the mass ratio of the pretreated honeysuckle leaf solid waste: ethanol solution volume ratio is 1:8. The ultrasonic power is 40W, the ultrasonic temperature is 55°C, the ultrasonic time is 10min; the centrifugal speed of the filtrate is 4000r/min, and the centrifugal time is 5min.

[0035] In step (4), the detection wavelength of the spectrophotometer is 325nm, and the volume concentration of the ethanol solution is 50%. The suction pressure is 0.6Mpa and the concentration temperature is 30°C. The ratio of the quality of crude chlorogenic acid to the volume of ethanol is 1:2, the extraction rate of chlorogenic acid is 90.9%, and the purity is 88.5%.

Example Embodiment

[0036] Example 3

[0037] An enzyme-catalyzed method for extracting chlorogenic acid from honeysuckle leaves is the same as that in Example 1, wherein:

[0038] In step (1), the honeysuckle leaf mesh number is 20 meshes, the oven temperature is 85°C, and the drying time is 90 minutes.

[0039] In step (2), the volume ratio of the mass of the pretreated honeysuckle leaf solid waste: the mass of enzyme: water is 1:0.3:30, and the mass ratio of the enzyme is ligninase: cellulase is 1: 3. Use hydrochloric acid solution to adjust the pH of the system to 3 and the temperature of the water bath to 20°C. Enzymatic hydrolysis activates honeysuckle leaf base material for 14h.

[0040] In step (3), the mass ratio of the honeysuckle leaf enzymatic hydrolysis activation base material: the volume ratio of the ethanol solution is 1:15. The ultrasonic power is 200W, the ultrasonic temperature is 25°C, the ultrasonic time is 45min; the centrifugal speed of the filtrate is 2500r/min, and the centrifugal time is 15min.

[0041] In step (4), the detection wavelength of the spectrophotometer is 335nm, and the volume concentration of the ethanol solution is 65%. The suction pressure is 0.1Mpa and the concentration temperature is 60°C. The ratio of the quality of crude chlorogenic acid to the volume of ethanol is 1:10, the extraction rate of chlorogenic acid reaches 93.2%, and the purity reaches 91.0%.

PUM

Property	Measurement	Unit
Particle size	<= 60.0	mesh

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Classification and recommendation of technical efficacy words

Reduce mass transfer resistance
Improve permeability

Method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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