KR100331778B1 - The method for extracting for an effect element with in leaf of ginko nut and there's apparatus - Google Patents

Abstract

The present invention relates to a method for effectively extracting flavonoids and ginkgorides from ginkgo biloba and an extracting device thereof. More specifically, the present invention effectively extracts the active ingredient in a short time compared to the conventional extraction method by increasing the specific gravity difference of the solvent and solubility of the sample by chromatographic method, that is, LLC extraction (Liquid-Liquid Chromatography extract method). In addition to the environmentally friendly extraction method and the extraction apparatus that can reduce the amount of use of the organic solvent.

The method includes a step of powdering by freeze drying or hot air drying after removing the residual solvent by the effective extraction method of all the herbal extracts as well as ginkgo leaves by the LLC extraction method.

Ginkgo biloba powder produced by this method has more than 30% of GFG (Ginkgo Flavonol Glycosides) content and excellent extraction of active ingredient compared to the existing 24%.

Description

Method of extracting active ingredient of ginkgo biloba and its extracting device {THE METHOD FOR EXTRACTING FOR AN EFFECT ELEMENT WITH IN LEAF OF GINKO NUT AND THERE'S APPARATUS}

The present invention relates to a method for extracting the active ingredient of ginkgo biloba and its extracting device. More specifically, the present invention improves the specific gravity difference of the solvent and the solubility of the sample by the extraction method using chromatographic extraction method, that is, LLC extraction method (Liquid-Liquid Chromatography extract method) in a short time compared to the conventional extraction method As an effective method of extracting the active ingredient, extracts of all herbal medicines as well as ginkgo biloba extract include the process of extracting the active ingredient by this method to remove residual solvent and then powdering it by lyophilization or hot air drying.

The active ingredients of ginkgo biloba leaves are known to be flavonoid compounds and terpene compounds (bilobalide, ginkgolide A, B, C, D, M, J), and flavonol glycosides and biflavones can be separated. Among them, glycosides of kaempferol, quercetin, and isorhamnetin are shown to be effective.

Since their medicinal components have been used in the treatment of vascular and blood flow disorders in 1965, they have significant effects on reducing cholesterol, expanding coronary arteries, enhancing blood circulation and reducing blood pressure resistance, as well as angina and hypertension of coronary heart disease. The treatment effect has been recognized and developed in Korea and abroad. Currently, researches on anti-cancer, hangover removal, tinnitus and AIDS treatment are also in progress.

In addition, ginkgoride was first isolated in 1967 by Nakanishi, Japan, and its structure was confirmed, and it was a competitive reaction with platelet-activating factor, resulting in asthma, bronchitis, senile dementia, allergies, heart disease, shock symptoms, rheumatic diseases, Although it is usefully used for other circulatory diseases, the amount of ginkgo biloba leaves is extremely small, and a method of effectively extracting and separating it has also been studied.

Korean Patent Publication No. 94-3054 discloses a process of distilling a ginkgo leaf extract aqueous solution into a methyl ethyl ketone single solvent using an ultrasonic extractor to obtain a flavonicoside, dissolving it in ethanol, and then passing an ion exchange resin. It describes a method for producing a high concentration of flavonol glycoside extract from the ginkgo leaf consisting of,

After filling ginkgo leaf powder in a column in Korean Patent Application Publication No. 91-19635, the mixture was passed through ether, exo acids, ethyl acetate-acetone mixtures in turn at room temperature, and passed through lower alcohol through the extract of flavonoid compound, and then purified by ethanol. Then, the inorganic salts were mixed to separate the organic layer, and the dried product was dried under reduced pressure and dried in anhydrous lower alcohol. The resulting mixture was adsorbed and separated by silica gel, washed with chloroform or dichloromethane and eluted again as anhydrous lower alcohol. A method for extracting flavonoids from ginkgo biloba powders is disclosed,

The conventional methods of extracting ginkgo biloba are the method of extracting the active ingredient by refining many times with many organic solvents, and there is a concern that a small amount of organic solvent may remain in the final product, as well as extraction required to go through various processes. Excess ginkgo leaf extract powder is very expensive due to excessive burden of facility cost and loss of active ingredient through multi-stage process due to the installation of the facility, and price burden on finished products is now a problem. As a result, they are in charge of the deficit of the trade balance.

In order to solve the above problems, the present invention by introducing the extraction method using the LLC device in extracting the active ingredient of ginkgo biloba by developing a method that can complete the extraction in a short time and at the same time save their time It was confirmed that the content of the active ingredient is a very excellent method compared to the existing extraction method and also completed the present invention in terms of the use of domestic agricultural products.

As a result, an object of the present invention is to reduce the amount of organic solvent used and extract and separate a large amount of active ingredients by extraction using chromatographic methods to increase the amount of active ingredients and to extract the active ingredients of ginkgo biloba leaves which are environmentally friendly, and their extraction apparatus. The purpose is to provide.

1 is a detailed view of the LLC extraction apparatus of the present invention

Explanation of symbols in the drawings

(1) motors (2) low specific solvent outlets and water outlets (3) sample entrances

(4) Solvent recycling (5) Low specific solvent inlet (MEK inlet)

(6) Heavyweight solvent inlet (MEK inlet) (7) Heavyweight solvent inlet (water outlet)

(8) impellers (9) glass tubes

C: Controller P: Pump

In order to achieve the above object, the present invention is the primary and secondary extraction of 100Kg ginkgo leaf pulverized with about 3-7 times methanol and then concentrated the filtrate under reduced pressure to remove the toxic substances with chloroform 3-4 times The aqueous layer was collected, filtered and concentrated under reduced pressure, and the aqueous layer was directly put into the LLC extractor and extracted with methyl ethyl ketone {MEK (Methyl Ethyl Ketone)} to quickly and effectively separate the active ingredients of ginkgo biloba. The content of Flavonol Glycosides) is generally about 10-12%, whereas it is about 17-19 ± 1.8% in this method, and it is 29 ± 1.2% when powdered after hot air or lyophilization after ethanol treatment. It is a very high yield extraction method compared to the standard value of 24% ginkgo leaf extract powder by the method of.

In addition, when extracting the solvent to MEK by the extraction method using LLC extractor in the ratio of 1: 0.8, 1: 1, 1: 1.5, 1: 2, 1: 3, the content of GFG was 11.652, 16.938, 17.518, 17.836, 18.102, 14.642% were measured and the sample and solvent input ratio was 1: 1-2, more preferably, 1: considering the maximum extraction effect while minimizing the amount of solvent used. The ratio of 1.5 is the most effective (see Table 1).

Table 1.Comparison of GFG Content by Addition Ratio of Sample and Extraction Solvent (MEK) in LLC Extraction

Sample to extractant ratio GFG content (%) Sample (Water Layer) Extraction Solvent (MEK Layer) 111111 321.510.80.5 14.64218.10217.83617.51816.93811.652

Extraction method of ginkgo leaf extract powder by LLC method of the present invention

The present invention will be described in detail by way of examples.

Example 1 (Ginkgo Leaf Extract Extraction Method)

To extract the active ingredient by crushing ginkgo biloba, 100 g of crushed ginkgo biloba leaves were extracted first and second with about 3-7 times methanol, and the filtrate was concentrated under reduced pressure. To remove the components, purified water and chloroform were added, and the solvent was extracted three times. Among them, the aqueous layer was separated, filtered and concentrated, and this was put into the LLC extractor as a sample, and purified water was added to the upper part and MEK was added to the lower part, and the solvent was circulated twice and extracted for 4-6 hours while operating the impeller. Among them, the MEK layer was taken, filtered and extracted twice with ethanol, and then the ethanol layer was concentrated under reduced pressure by filtration, stored in a deep freezer, lyophilized or hot air dried, and then ground to powder. This is a drying method widely used in the food or pharmaceutical industry has been confirmed as a non-hazardous method in the human body.

Example 2 (ratio of sample and solvent when extracting active ingredient of ginkgo biloba using LLC device)

The ratio of sample and extractant (MEK) to the LLC extractor is 1: to establish the conditions of use of the sample and extractant (MEK) containing purified water to obtain the maximum extract of the active ingredient when extracting the active ingredient by the LLC device. 0.5, 1: 0.8, 1: 1, 1: 1.5, 1: 2, 1: 3 in the ratio of GFG content was compared and examined (see Table 1).

As shown in Table 1, the more the amount of MEK extractant was used, the higher the content of GFG was. However, when comparing the effect of solvent use with the amount of extraction, the GFG content was 12.806%, which was the highest in the ratio of 1: 2. Considering the efficiency of use, the ratio of 1: 1.5 is more preferable in view of the reduction of the use of the extraction solvent.

Therefore, in the present invention, the ratio between the sample containing purified water and the extraction solvent (MEK) used in the LLC extraction apparatus is 1: 1.5-2, and more preferably, the maximum extraction effect is 1: while reducing the amount of solvent used. 1.5.

Example 3 (Check the GFG content of the ginkgo leaf extract powder extracted by the present invention)

In extracting ginkgo biloba, the GFG content of each extract was measured in the order of solvent extraction. As a result, as shown in Table 2, the MEK extract in the LLC extractor, the most important process of ginkgo leaf extraction, showed a 17.967% increase in the GFG content. Compared with the existing method, the method showed an increase in GFG content by using LLC extractor. The GFG content after freeze-drying or hot-air drying after ethanol extraction of this concentrate was measured to be 30.28%. An increase in GFG content of about 1.25 times greater than% was shown.

The rapid increase of GFG content in the extraction of the active ingredient of ginkgo biloba by LLC extraction method increased the separation coefficient by increasing the phase seperation by the impeller as solvent extraction was continuously circulated, and the amount of extraction was increased. This method minimizes the loss in the extraction process, and it is an environmentally friendly method because the solvent extraction method is simple, but the amount of solvent used is small and the recovery rate is minimized to minimize the amount of solvent used.

Table 2. Changes in GFG Content of Ginkgo Leaf Extract Extracts

sample GFG content (%) Methanol concentrate 3.578 Water layer after chloroform treatment 5.509 MEK Concentrate (LLC Treatment) 17.967 Ethanol Concentrate 23.324 Ginkgo leaf extract powder 30.284

Brief description of the drawings is as follows.

1 shows an LLC extraction apparatus, (1) motor, (2) low specific solvent outlet and water outlet, (3) sample inlet, (4) solvent recirculation pipe, (5) low specific solvent inlet (MEK inlet) ), (6) high specific solvent inlet (MEK inlet), (7) high specific solvent inlet (water outlet), (8) impeller, (9) glass tube, C: controller, P: pump.

LLC extraction apparatus of the present invention has a motor (1) is configured on the top and the lower body is formed of a body (9), which is operated by the motor (1) a plurality of formed inside the body of the glass An impeller 8, an inlet (water outlet) 7 connected to an upper portion of the glass tube 9 to inject a high specific solvent, and an inlet for injecting a low specific solvent from the lower portion of the glass tube 9 (MEK inlet) (5), a sample inlet (3) for injecting a sample into the middle portion of the glass tube (9), and an outlet and a water layer outlet (2) formed at an upper portion of the glass tube (9) to discharge a low specific gravity solvent And, LLC (Liquid-Liquid Chromatography) extraction device for extracting the active ingredient from the ginkgo leaf, characterized in that it comprises a solvent recycle pipe (4) and other pumps, controllers and valves connected to the inlet.

The LLC extraction method is the same as the conventional method in that a solvent is used to extract and separate a substance by using a specific gravity difference, but the method according to the present invention increases the theoretical number of separation by using the physical properties to the maximum. It is a device that can extract the active ingredient more effectively. As shown in Fig. 1, the separation coefficient was increased by mounting a large amount of impeller 8 so as to make the best use of the specific gravity difference of the solvent and the physical properties of the sample. It is a device (5) is designed to extract the most effective ingredient of ginkgo leaf extract.

The present inventors study that the number of impellers in the LLC extraction apparatus is 4-8, and the extraction time is very long when the number of impellers is small and the mixing of solvents is unbalanced when the number of impellers is large. When the six is confirmed that the most effective extraction effect was completed the present invention.

The extraction device consists of a glass (9).

In general, the most influential factors in extraction in solvent extraction methods are interfacial tension, solubility of solutes, and emulsion formation.In this extraction method, these factors are considered to improve or eliminate separation barriers as much as possible. As the scope of application of the method, extraction of expensive compounds, separation of compounds with similar boiling points, compounds with high boiling points, azeotropic compounds, especially heat sensitive compounds, etc. can be effectively used.

The present invention as described above is an environmentally friendly extraction method that can effectively reduce the amount of use of the organic solvent as well as effectively extract the active ingredient in a short time compared to the conventional extraction method by increasing the specific gravity difference of the solvent and the solubility of the sample.

This method has the effect of efficiently extracting the active ingredient from the extract of all herbal medicines as well as ginkgo leaves by the LLC extraction method.

Claims (6)

In the method of extracting the active ingredient from the ginkgo biloba, the ginkgo biloba extract is extracted with methanol and ethanol, the toxic substance is removed with chloroform, and the active ingredient (flavonoid compound and terpene compound) is extracted with methyl ethyl ketone solvent using LLC extraction. After the purification, filtration, concentrated with methanol or ethanol and then lyophilized or hot-air dried to extract the active ingredient from the ginkgo leaf comprising the step of powdering. The method of claim 1, pulverizing ginkgo biloba leaves and extracted with primary and secondary methanol to extract the active ingredient, the filtrate is concentrated under reduced pressure, to remove ginkgoric acid (toxic ginkgoric acid) contained in the ginkgo leaves In order to extract the solvent three times by adding purified water and chloroform, the aqueous layer is separated, filtered and concentrated. The liquid is added to a LLC (Liquid-Liquid Chromatography) extractor, and purified water and methyl ethyl ketone (MEK) are added to operate the impeller. After circulating the solvent three times while extracting for 4-6 hours, the MEK layer was taken, filtered and extracted with ethanol two or three times, and the ethanol layer was concentrated under reduced pressure by filtration and stored in a deep freezer. Method of extracting the active ingredient from the ginkgo leaf, characterized in that the lyophilized, or hot-air dried and then pulverized to powder. According to claim 1, In order to increase the GFG content in the extraction of the active ingredient of the ginkgo biloba, solvent extraction is continuously circulated to increase the phase separation by increasing the phase separation by the impeller to increase the extraction amount, and also extraction A method of extracting an active ingredient from ginkgo biloba, characterized by minimizing the amount of solvent generated and minimizing the amount of solvent used in the extraction process. The method of extracting an active ingredient from ginkgo biloba leaves according to claim 1, wherein the extract is powdered from ginkgo biloba, including those produced by the LLC extraction method alone or in a continuous process. The method according to claim 1, wherein the ratio of the sample and the extraction solvent (MEK) used in the LLC extraction method in the extraction is a solvent ratio applied in a ratio of 1: 1 to 2. In the extracting device for extracting the active ingredient from the ginkgo leaf, the motor (1) is configured on the upper part and the body (9) made of glass is formed at the lower part of the body, which is operated by the motor (1) A plurality of impellers 8 formed therein, an inlet (water outlet) 7 connected to the upper portion of the glass tube 9 to inject a high specific solvent, and a low specific solvent in the lower portion of the glass tube 9 An inlet (MEK inlet) 5, a sample inlet 3 for injecting a sample into the middle portion of the glass tube 9, an outlet for discharging a low specific gravity solvent formed on the glass tube 9, and LLC (Liquid-Liquid Chromatography) extraction device for extracting the active ingredient from the ginkgo leaf, characterized in that it comprises a water outlet (2), the solvent recycle pipe (4) and other pumps, controllers and valves connected to the inlet.