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Removal method for caffeine in folium ginkgo extractives

An extract and technology of ginkgo biloba, applied in the field of removal of harmful substances in ginkgo biloba extract, can solve the problem of low caffeine ginkgo biloba extract, etc., and achieve the effect of low cost and simple process

Active Publication Date: 2019-10-15
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the literature on the refining of Ginkgo biloba extract is mainly aimed at the purification of flavonoids and ginkgolide B in Ginkgo biloba extract, and there are almost no literature reports on the purification of low-caffeine Ginkgo biloba extract.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Add 30L of hydrochloric acid aqueous solution at 15°C and pH=5.7 to 20kg of ginkgo leaf extract, stir at 90r / min for 2h, and centrifuge with a decanter centrifuge with a centrifugal factor of not less than 6000 to obtain 14L of aqueous acid solution I , 26.3kg viscous substance I;

[0020] (2) After vacuum-drying the obtained viscous substance I at 53°C and vacuum degree of -0.085MPa, 17.7kg of Ginkgo biloba extract I was obtained;

[0021] (3) Add 3 times the volume of dichloromethane to the acid aqueous solution I, extract 3 times at 34°C, stand to separate and separate, and carry out organic solvent recovery at 35°C and a vacuum of -0.04MPa for the solvent phase of the lower layer, and the upper layer of water The phases were combined to obtain solution II;

[0022] (4) Add sodium hydroxide solution with a mass fraction of 5‰ to the obtained solution II to adjust the pH value to 9.0, and heat it to 35°C and pass it through a DM-130 macroporous adsorption resin c...

Embodiment 2

[0027] (1) Add 40L of phosphoric acid aqueous solution with a temperature of 10°C and pH=5.8 to 20kg of ginkgo leaf extract, stir at 90r / min for 0.5h, and then centrifuge with a tubular centrifuge with a centrifugal factor of not less than 6000 to obtain 33L of aqueous acid solution 1, 26kg viscous substance I;

[0028] (2) After vacuum-drying the obtained viscous substance I at 53°C and a vacuum degree of -0.08MPa, 17.8kg of Ginkgo biloba extract I was obtained;

[0029] (3) Add 4 times the volume of dichloromethane to the acid aqueous solution I, extract 4 times at 32°C, stand to separate and separate, and carry out organic solvent recovery at 31°C and vacuum degree of -0.04MPa for each lower solvent phase obtained, and the upper layer of water The phases were combined to obtain solution II;

[0030] (4) Add sodium bicarbonate solution with a mass fraction of 5‰ to the obtained solution II to adjust the pH value to 9.5, heat it to 36°C, pass through LSA-10 macroporous adsor...

Embodiment 3

[0035] (1) Add 45L of hydrochloric acid aqueous solution with a temperature of 15°C and pH=6.0 to 20kg of ginkgo leaf extract, stir at 90r / min for 3 hours, and then centrifuge with a disc centrifuge with a centrifugal factor of not less than 6000 to obtain 37L of aqueous acid solution 1, 26.2kg viscous substance I;

[0036] (2) The obtained viscous substance I was vacuum-dried at a temperature of 55°C and a vacuum degree of -0.09MPa to obtain 17.6kg of Ginkgo biloba extract I;

[0037] (3) Solution I was extracted by adding 4 times the volume of dichloromethane at 36°C for 4 times, standing to separate layers, and the solvent phase of the lower layer was collected at 33°C and vacuum degree -0.05MPa for each pass, and the upper layer of the aqueous phase was combined to obtain Solution II;

[0038] (4) Add sodium hydroxide solution with a mass fraction of 5‰ to the obtained solution II to adjust the pH value to 10.0, heat it to 40°C and pass through LSA-20 macroporous adsorpti...

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PUM

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Abstract

The invention discloses a removal method for caffeine in folium ginkgo extractives. The removal method comprises the following steps of: (1) adding acidic aqueous solution of which the pH is 5.7-6.0 at a temperature of 10-15DEG C into folium ginkgo extractives, evenly mixing under a condition of 10-15DEG C, and carrying out centrifugation to obtain a first acidic aqueous solution and a first sticky substance; (2) carrying out vacuum drying on the first sticky substance to obtain a first folium ginkgo extractive with a low caffeine content; (3) adding dichloromethane into the first acidic aqueous solution for extraction for 3-5 times, standing for layering, and combining water on an upper layer to obtain a second solution; (4) regulating the pH value of the second solution to 9.0-10.0, heating the second solution, and enabling the second solution to pass through macroporous adsorption resin, washing a resin column with hot water, analyzing until the pH value is 6.5-7.5, collecting analytic solution, removing solvent residues to obtain a second folium ginkgo extractive with a low caffeine content; and (5) fully evenly mixing the first folium ginkgo extractive and the second folium ginkgo extractive to obtain the folium ginkgo extractive of which the caffeine is removed. The removal method has the advantages of simple technology and low cost and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for removing harmful substances in ginkgo leaf extract, in particular to a method for removing caffeine in ginkgo leaf extract. Background technique [0002] Ginkgo biloba L. is a deciduous tree of the genus Ginkgo in the Ginkgo family, and is a special plant in my country. Ginkgo biloba is an important medicinal part of Ginkgo biloba. Its main active ingredients are flavonoids and lactones. Among them, flavonoids can resist oxidation, improve cardiovascular and cerebrovascular circulation, and have anti-virus, anti-aging, anti-allergic, anti-tumor, Lower cholesterol, regulate the body's immune system and other effects. Ginkgo biloba has been used as medicine for more than 60 years. Ginkgo biloba extract (GBE) is the first-line drug for clinical treatment of cerebrovascular diseases. The effect of dampness and antidiarrheal is mainly used to treat coronary heart disease, cough disease, hyperlipidemia, angina pectoris...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/16A61K127/00
CPCA61K36/16A61K2236/333A61K2236/51A61K2236/53A61K2236/55
Inventor 张玉芬张苹苹张晓芳刘登帅程远欣
Owner CHENGUANG BIOTECH GRP CO LTD
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