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Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf

A technology of chlorogenic acid and eucommia leaves, which is applied in the field of preparing high-purity chlorogenic acid and total flavonoids, can solve the problems of many types of reagents, large solvent consumption, cumbersome process, etc., and achieve high target component content and product quality The effect of stability and simple process flow

Active Publication Date: 2010-06-23
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has the following disadvantages: the pretreatment of this process uses petroleum ether to degrease, the amount of petroleum ether is 2 to 3 times that of the raw material, and the solvent consumption is large, but generally it is impossible to achieve the desired effect in a short time, and at the same time it needs to add biological compound Enzyme impregnation for 24 to 36 hours, which makes the whole production cycle longer; at the same time, the process includes pretreatment, extraction, concentration, acid extraction, alkali neutralization, acid precipitation, recrystallization and other steps, and in some steps, biological Composite enzymes, reducing complex enzymes, etc., have many and cumbersome process steps, and involve many types of reagents and large quantities, which are not suitable for industrial production
This process is mainly completed by ultrasonic pretreatment and high temperature extraction, ultrafiltration, ethyl acetate extraction, D-140 resin separation and other steps. The patent mainly has the following shortcomings: (1) ultrasonic pretreatment before extraction, the process is cumbersome, The cost is high, and it is difficult to realize industrially; (2) chlorogenic acid is a heat-sensitive component, and high-temperature extraction is prone to decomposition. According to the extraction conditions of the CN1273964A patent, the recovery rate of chlorogenic acid is only 60% at 100 ° C for 80 to 120 min; (3) There are many steps in the patented process, and methods such as ultrafiltration, precipitant precipitation, and macroporous resin are used. The process is complicated, the equipment cost is high, the operation is cumbersome, and there are still problems such as unreasonable temperature selection during extraction. Therefore, it is difficult to realize industrial production

Method used

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  • Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf
  • Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf
  • Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The selection of embodiment 1 extraction process condition:

[0034] (1) Effect of pulverized Eucommia leaves on the extraction rate of chlorogenic acid and total flavonoids

[0035] Experimental method: 5.0kg of eucommia leaves were extracted with 40L of 45% ethanol solution with pH=4, stirred twice at 70°C, the first time was extracted with 25L solvent for 2 hours, and the second time was extracted with 15L solvent for 1 hour. After the solution was concentrated to 4L, it was left to stand for 1.0 hour and centrifuged, and the supernatant was taken to dry, and the extraction rates of chlorogenic acid and total flavonoids were calculated respectively. The results are shown in the table below

[0036]

[0037] It can be seen from the above table that pulverizing Eucommia leaves increases the contact area between the raw material and the extraction solvent, and improves the extraction rate of active ingredients. When Eucommia leaves were crushed into coarse powder, me...

Embodiment 2

[0051] The selection of embodiment 2 separation process

[0052] (1) The influence of the choice of macroporous resin type on the separation effect

[0053] Experimental method: Extract 5kg of eucommia leaf coarse powder with 45% ethanol solution with pH=4 at 70°C for 1.5 hours each time, concentrate the combined extracts to 4L and centrifuge, and take the supernatant as eucommia leaf The extract was determined to have a dry weight of 0.9kg, a mass content of chlorogenic acid of 11.3% and a mass content of total flavonoids of 30.5%. The extract was divided into 7 parts on average, and the macroporous resin was used for static saturated adsorption, and the adsorption capacity and desorption rate of different types of resins for chlorogenic acid and total flavonoids were calculated respectively. Macroporous resin mainly selects non-polar resin XDA-5, LSA-20, D140, polar resin NKA-II, HPD-400, HPD-400A and medium polar resin JD-1 in the method of the present invention.

[0054]...

Embodiment 3

[0059] The process selection of embodiment 3 chlorogenic acid refining process

[0060] (1) The effect of the amount of silica gel on the separation of chlorogenic acid silica gel column

[0061] Experimental method: Take 0.25kg of crude chlorogenic acid (content is 24.5%) and dissolve it with 100ml of methanol, mix the sample with 125g of silica gel and put it on a silica gel column. The amount of silica gel in the silica gel column is 6 to 15 times the dry weight of crude chlorogenic acid, and then Use ethyl acetate as the eluent for elution, collect in sections and then concentrate under reduced pressure. The fractions collected in sections are monitored by HPLC, and the fractions with a content higher than 90% are combined and concentrated to dryness. The result shows that when the amount of silica gel is less than 6 times of the dry weight of the crude product of chlorogenic acid, the crude product of chlorogenic acid is not separated well, and the yield of 90% chlorogeni...

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Abstract

The process of preparing high purity chlorogenic acid and flavonid with eucommia leaf includes the following steps: crushing eucommia leaf and extracting with pH 3-6 alcohol solution of 45 %-55 % concentration; saturation adsorbing the extracted solution with medium polarity JD-1 macroporous resin, and eluting successively with water, 20 %-45 % concentration alcohol solution and 60 %-75 % concentration alcohol solution to obtain crude chlorogenic acid product and flavonid-containing powder separately; eluting the crude chlorogenic acid product in silica gel column with ethyl acetate, acetone,methanol or ethanol, collecting the eluted solution, decompression concentrating, and re-crystallizing the concentrate in acetone or water to obtain refined chlorogenic acid product. The present invention has simple technological process, convenient operation, reuse of the macroporous resin, low comprehensive cost and excellent industrial application foreground.

Description

technical field [0001] The invention relates to a method for extracting and preparing active ingredients by using plants as raw materials, in particular to a method for preparing high-purity chlorogenic acid and total flavonoids from leaves of Eucommia ulmoides. Background technique [0002] Eucommia ulmoides is a traditional Chinese medicinal material with a history of more than 2,000 years in my country. Its functions are to nourish the liver and kidney, strengthen bones and muscles, and prevent miscarriage. At the same time, Eucommia ulmoides has special effects on treating hypertension. Chlorogenic acid and flavonoids are the main active components of Eucommia ulmoides leaves, which have significant physiological activities. Chlorogenic acid is a derivative of caffeoylquinic acid, which has multiple pharmacological effects such as choleretic, antibacterial, antiviral, antihypertensive, increasing white blood cells, and stimulating the central nervous system. It is an imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/48C07C69/732C07D311/22C07B63/00A61K36/46
Inventor 李金华邹小燕葛发欢周锦珂黄裕林周杨祖金
Owner GUANGZHOU HANFANG PHARMA
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