KR102499774B1 - Method for preparing excipient for tableting comprising green tea residue and method for preparing green tea tablet using the same - Google Patents

Abstract

The present invention comprises the steps of (a) extracting dried green tea leaves with an extraction solvent to obtain a green tea extract, and separating the residue to prepare a primary residue; (b) preparing a re-extract and a secondary residue by re-extracting the primary residue with an extraction solvent; and (c) preparing an excipient powder for tableting by pulverizing the re-extract and the secondary residue. By this, the generation of waste during tablet manufacturing is fundamentally prevented from occurring, and the process and costs associated with waste disposal are prevented, and since the catechin contained in the residue is included in the green tea tablet, the content of catechin can be increased.

Description

Manufacturing method of tableting excipient containing green tea residue and manufacturing method of green tea tablet using the same

The present invention relates to a method for manufacturing an excipient for tableting containing green tea residue and a method for manufacturing a green tea tablet using the same, and more particularly, to a method for manufacturing a green tea tablet containing green tea residue that can be used as an excipient without discarding the residue generated after green tea extraction It relates to a method for manufacturing an excipient for tableting and a method for manufacturing a green tea tablet using the same.

Green tea contains catechin, caffeine, amino acids, fiber, pectin, vitamins, inorganic salts, and the like, and contains various physiologically active substances that are effective in antioxidation, antimutagenic and antitumor action, and inhibition of cholesterol elevation by these components.

Catechin belongs to the flavan-3-ols of the flavonoid group, and is a kind of polyphenol, which is an astringent component of green tea. It is derived from tea (Camellia sinensis) and is included in white tea, green tea, black tea, and oolong tea. However, in the case of black or oolong tea, more than half of catechins are reduced during fermentation. Polyphenols in tea leaves include free catechins with a mild bitter taste, ester catechins with a bitter and astringent taste, and combined catechins with strong bitter and weak astringent tastes. The major catechins include epigallocatechingallate (EGCG), epigallocatechin (EGC), epicatechingallate (ECG), and epicatechin (EC).

Catechin has various effects such as suppression of carcinogenesis, arteriosclerosis, inhibition of blood pressure increase, prevention of blood clots, antiviral, antiobesity, antidiabetic, antibacterial, detoxification, anti-inflammatory, prevention of tooth decay, prevention of dry mouth, and normalization of intestinal flora. The antioxidant action of catechins and the ability to remove free radicals, which are fundamental factors in aging, have a stronger active oxygen removal effect than vitamins C and E, and have cardiovascular protective effects such as oxidation of low density lipoprotein due to their antioxidant action. has been reported Catechins have been shown to stop or slow the production and initiation of undesirable cell populations and to block those that empirically cause DNA damage.

For easy intake of such catechins, there is a method of tableting green tea extract by tableting. However, in the tableting process, the residue after green tea extraction is entirely discarded, requiring an additional waste treatment process, additional processing costs due to the additional use of excipients such as dextrin and lactose, and the use of catechins contained in the residue. There was a problem that couldn't be solved.

Korean Patent Registration No. 10-1630853 Korean Registered Patent Publication No. 10-0673605

An object of the present invention is to solve the above problems, by using the residue remaining after preparing the green tea extract to prepare an excipient for tableting, and using this for tableting of green tea tablets, the generation of waste is fundamentally prevented, resulting in waste treatment It is an object of the present invention to provide a method for manufacturing an excipient for tableting, which increases the content of catechin, and a method for manufacturing a green tea tablet including the same, without the process and cost being incurred and since the catechin contained in the residue is included in the green tea tablet.

According to one aspect of the present invention,

(a) extracting dried green tea leaves with an extraction solvent to obtain a green tea extract, and separating a residue to prepare a primary residue; (b) preparing a re-extract and a secondary residue by re-extracting the first residue with an extraction solvent; and (c) preparing an excipient powder for tableting by pulverizing the re-extract and the secondary residue.

The extraction solvent in step (a) may be at least one selected from water, lower alcohol having 1 to 4 carbon atoms, acetone, ethyl acetate, chloroform, butyl acetate, 1,3-butylene glycol, hexane, and diethyl ether. .

The extraction solvent may be an aqueous solution of ethanol at a concentration of 30 to 75%.

The extraction solvent used in the re-extraction of step (b) is selected from water, lower alcohol having 1 to 4 carbon atoms, acetone, ethyl acetate, chloroform, butyl acetate, 1,3-butylene glycol, hexane, and diethyl ether It may be one or more.

The extraction solvent used for the re-extraction may be hot water at 60 to 100 ° C.

Re-extraction in step (b) may be performed by reflux extraction.

Sugars included in the primary residue may be extracted by re-extraction in step (b).

The powdering of step (c) may be performed according to any one method selected from spray drying, vacuum distillation and freeze drying.

According to another aspect of the present invention,

An excipient for tableting comprising the green tea residue prepared according to the above method is provided.

According to another aspect of the present invention,

(1) extracting dried green tea leaves with an extraction solvent to obtain a green tea extract, and separating the residue to prepare a primary residue; (2) preparing a decaffeinated green tea extract by removing caffeine from the green tea extract; (3) preparing a concentrated green tea extract by concentrating the decaffeinated green tea extract; (4) preparing green tea extract powder by pulverizing the green tea extract; and (5) preparing a green tea tablet by tableting the green tea extract powder and an excipient for tableting containing the green tea residue prepared according to any one of claims 1 to 7. A manufacturing method is provided.

The catechin content of the dried green tea leaves in step (1) may be 8 to 13 wt%.

In step (2), caffeine may be removed by treatment with an ion exchange resin or ultrasonication while the green tea extract is mixed with an extraction solvent.

The ultrasonic treatment may be performed for 10 to 20 minutes.

In step (2), caffeine may be removed by adding ethyl acetate or methylene chloride while the green tea extract is mixed with the extraction solvent.

Concentration in step (3) may be performed according to vacuum concentration or centrifugal concentration.

The green tea extract powder of step (4) may have an average particle size of 20 to 23 μm.

The powdering of step (4) may be performed according to any one method selected from spray drying, vacuum distillation and freeze drying.

In step (5), the tableting excipient and the green tea extract powder may be mixed in a weight ratio of 3:7 to 7:3 and compressed into tablets.

In step (5), a lubricant may be additionally included for tableting.

The catechin content of the green tea tablet of step (5) may be 30 to 35 wt%.

According to another aspect of the present invention,

A green tea tablet prepared according to the above method is provided.

The method for manufacturing an excipient for tableting containing green tea residue and a method for manufacturing a green tea tablet using the same of the present invention is to prepare an excipient for tableting using the residue remaining after preparing the green tea extract, and using the residue for tableting green tea tablet, thereby producing waste The generation of catechin is fundamentally prevented from occurring, and the content of catechin can be increased because the catechin contained in the residue is included in the green tea tablet.

1 is a flowchart showing a method of manufacturing a green tea tablet and a method of manufacturing an excipient for tableting according to the present invention.

Since the present invention can apply various transformations and have various embodiments, specific embodiments will be illustrated in the drawings and described in detail in the detailed description. However, it should be understood that this is not intended to limit the present invention to specific embodiments, and includes all transformations, equivalents, and substitutes included in the spirit and scope of the present invention. In describing the present invention, if it is determined that a detailed description of related known technologies may obscure the gist of the present invention, the detailed description will be omitted.

1 is a flow chart sequentially showing a method of manufacturing an excipient for tableting containing green tea residue of the present invention and a manufacturing process of a green tea tablet using the method. Hereinafter, a method for preparing an excipient for tableting containing the green tea residue of the present invention will be described with reference to FIG. 1 .

First, dry green tea leaves Extraction with an extraction solvent to obtain a green tea extract, the residue ( residue ) by separating the first order residue Prepare (step a).

As the extraction solvent, water, lower alcohol having 1 to 4 carbon atoms, acetone, ethyl acetate, chloroform, butyl acetate, 1,3-butylene glycol, hexane, diethyl ether and the like may be used.

Preferably, the extraction solvent may be a 30 to 75% aqueous ethanol solution, more preferably 50 to 75% concentration, and even more preferably 60 to 75% ethanol solution.

The term 'extract' used herein has a meaning commonly used in the art as a crude extract, but may also include a fraction obtained by further fractionating the extract in a broad sense.

Next, the first residue Re-extract with extraction solvent re-extract and Secondary residue Prepare (step b).

As the extraction solvent used for the re-extraction, water, lower alcohol having 1 to 4 carbon atoms, acetone, ethyl acetate, chloroform, butyl acetate, 1,3-butylene glycol, hexane, diethyl ether and the like may be used.

Preferably, the extraction solvent used in the re-extraction may be 60 to 100 ° C hot water, more preferably 70 to 95 ° C hot water, and even more preferably 80 to 90 ° C hot water.

The re-extraction is preferably performed by reflux extraction.

Sugars included in the primary residue are extracted by the re-extraction, and the binding agent function may be further improved. In some cases, this step may be omitted and the primary residue may be immediately pulverized to prepare an excipient, but in this case, tableting may not be performed properly due to insufficient binder components.

Finally, remind re-extract and Secondary residue powdered for driving An excipient powder is prepared (step c).

The powdering may be carried out by spray drying, distillation under reduced pressure, freeze drying, etc., preferably by spray drying.

The present invention provides an excipient for tableting manufactured according to the method for preparing an excipient for tableting containing the green tea residue described above.

Hereinafter, with reference to FIG. 1, a method for manufacturing the green tea tablet of the present invention will be described.

First, dry green tea leaves Extraction with an extraction solvent to obtain a green tea extract, the residue ( residue ) by separating the first order residue Prepare (step 1).

Since step 1 is performed in the same way as step a in the above-described method for manufacturing an excipient for tableting, reference will be made to that part for specific details.

The green tea extract may have a catechin content of 8 to 13 wt%.

Next, by removing the caffeine component from the green tea extract decaf Green tea extract is prepared (step 2).

Caffeine may be removed by treatment with an ion exchange resin or ultrasonic treatment in a state where the green tea extract is mixed with an extraction solvent. At this time, the ultrasonic treatment is preferably performed for 10 to 20 minutes.

Alternatively, caffeine may be removed by adding ethyl acetate or methylene chloride while the green tea extract is mixed with the extraction solvent, but the scope of the present invention is not limited thereto and other known decaffeination methods may be used.

After, above decaf Green tea extract is concentrated to prepare a green tea concentrated extract (step 3).

Concentration may be performed according to vacuum concentration or centrifugal concentration.

Next, the green tea concentrate extract powdered Green tea extract powder is prepared (step 4).

The green tea extract powder may have an average particle size of 20 to 23 μm.

The powdering may be carried out by spray drying, distillation under reduced pressure, freeze drying, etc., preferably by spray drying.

Finally, the green tea of the present invention described above residue including for driving The excipient and the green tea extract powder as materials By concluding green tea tablet Prepare (step 5).

The green tea tablet may have a catechin content of 30 to 35 wt%. The reason for this is that the content of catechins is greatly increased because catechins included in the excipient are additionally included in the catechins included in the green tea extract.

In addition, the present invention provides a green tea tablet prepared according to the above-described green tea tablet manufacturing method.

Hereinafter, preferred embodiments are presented to aid understanding of the present invention, but the following examples are merely illustrative of the present invention, and various changes and modifications are possible within the scope and spirit of the present invention. It is obvious to those skilled in the art, It goes without saying that these variations and modifications fall within the scope of the appended claims.

Example One

(1) Green tea extraction and residue obtained

Green tea leaves (Osulloc Farm, Jeju Special Self-Governing Province) were used after being dried in the shade at room temperature. 680 kg of the prepared green tea leaves were prepared, 10,200 L of a 70% concentration ethanol aqueous solution was added, heated, and extracted for 1 hour after reaching 70° C., followed by filtration to separate the green tea extract and residue.

(2) Preparation of green tea extract

After treating the green tea extract with decaffeination, a concentrated extract obtained by removing the solvent by a vacuum concentrator was obtained, and then powdered by spray drying.

(3) residue re-extraction and preparation of excipient powder

3400 kg of hot water was added to the residue, followed by reflux extraction at 86° C. to extract sugars from the residue to obtain a re-extract and residue mixture, and the re-extract and residue mixture were spray-dried and pulverized to prepare an excipient powder.

(4) Green tea tablet manufacturing

The green tea extract powder obtained in step (2), the excipient powder obtained in step (3), silicic anhydride as a lubricant, and magnesium stearate were mixed in a weight ratio of 55:44:0.5:0.5, and the size was 15 mm in diameter and 7 mm in thickness, and the tableting pressure was 500 kgf. A green tea tablet was prepared by tableting. The total weight of the green tea produced was 198.6 kg, and the yield was 29.2%.

comparative example One

A green tea tablet was prepared in the same manner as in Example 1, except that the residue re-extraction process was omitted and the powdered residue was used as an excipient. The total weight of the prepared green tea tablet was 202.4 kg, and the yield was 29.8%.

comparative example 2

Green tea tablets were prepared in the same manner as in Example 1, except that dextrin was used as an excipient instead of the excipient powder obtained in step (3). The total weight of the prepared green tea tablet was 180 kg and the yield was 26.5%. In addition, about 500 kg of residue generated after extracting green tea was disposed of, and the disposal cost was 75,000 won per ton.

[Test Example]

test example 1: Catechin content analysis

100 ml of a 50% methanol aqueous solution was added to 0.5 g of each crushed sample of the tablets prepared according to Example 1, Comparative Example 1 and Comparative Example 2, and sonicated for 20 to 30 minutes. The extracted sample was filtered through a 0.45 μm membrane filter. Analysis was performed by HPLC (high performance liquid chromatography), and the injection amount of each sample was 10 μl, and the gradient method was used.

As a result of the analysis, the catechin content was 24.3% in the sample of Example 1, 24.1% in Comparative Example 1, and 19.6% in Comparative Example 2, indicating that the green tea tablet using the residue as an excipient had a relatively high catechin content.

test example 2: of the tablet Property evaluation

Hardness, disintegration time, and friability were evaluated for the tablets prepared according to Example 1, Comparative Example 1 and Comparative Example 2. Hardness was measured according to United States Pharmacopoeia (USP) Chapter 1217 (tablet breaking force), disintegration time was measured according to United States Pharmacopoeia (USP) Chapter 701 (Disinteration), and friability was measured according to United States Pharmacopoeia (USP) Chapter 1216 (tablet friability) After performing the wear test according to, the wear degree was measured according to the following formula, and the results are summarized in Table 1 below.

[ceremony]

Friction (%) = (Weight of 20 initial tablets (mg) - Weight of 20 tablets after wear test (mg))/Weight of 20 initial tablets ⅹ 100 (%)

evaluation items Hardness (kp) Wear and tear (%) Disintegration time (minutes) Example 1 9.7 0.5 4.6 Comparative Example 1 6.5 1.8 3.2 Comparative Example 2 10.2 0.4 4.9

According to Table 1, the tablet of Example 1, while using green tea residue as an excipient, did not show a significant difference from the tablet of Comparative Example 2 using conventional dextrin as an excipient in hardness, friability, and disintegration time evaluation. However, the tablet of Comparative Example 1 using the non-re-extracted residue as an excipient showed relatively low hardness and high friability. These results indicate that the hardness of the tablet of Example 1 was increased because the sugars contained in the residues were extracted during the re-extraction process of the residues, and the re-extracts containing the extracted sugars were included in the excipients and acted as binders.

Although the embodiments of the present invention have been described above, those skilled in the art can add, change, delete, or add components within the scope not departing from the spirit of the present invention described in the claims. The present invention can be variously modified and changed by the like, and this will also be said to be included within the scope of the present invention.

Claims (11)

(a) extracting dried green tea leaves with an extraction solvent to obtain a green tea extract, and separating a residue to prepare a primary residue;
(b) preparing a re-extract and a secondary residue by re-extracting the first residue with an extraction solvent; and
(c) preparing an excipient powder for tableting by pulverizing the re-extract and the secondary residue; According to claim 1,
The extraction solvent in step (a) or (b) is 1 selected from water, lower alcohol having 1 to 4 carbon atoms, acetone, ethyl acetate, chloroform, butyl acetate, 1,3-butylene glycol, hexane, and diethyl ether A method for producing an excipient for tableting comprising green tea residue, characterized in that more than one species. According to claim 1,
The powdering of step (c) is a method for producing an excipient for tableting, characterized in that carried out according to any one method selected from spray drying, vacuum distillation and freeze drying. An excipient for tableting comprising the green tea residue prepared according to any one of claims 1 to 3. (1) extracting dried green tea leaves with an extraction solvent to obtain a green tea extract, and separating the residue to prepare a primary residue;
(2) preparing a decaffeinated green tea extract by removing caffeine from the green tea extract;
(3) preparing a concentrated green tea extract by concentrating the decaffeinated green tea extract;
(4) preparing green tea extract powder by pulverizing the green tea extract; and
(5) preparing a green tea tablet by tableting the green tea extract powder and an excipient for tableting containing the green tea residue prepared according to any one of claims 1 to 3; manufacturing method. According to claim 5,
In step (2), caffeine is removed by adding ethyl acetate or methylene chloride while the green tea extract is mixed with the extraction solvent. According to claim 5,
The green tea extract powder of step (4) is a method for producing a green tea tablet, characterized in that the average particle size is 20 to 23㎛. According to claim 5,
The powdering of step (4) is a method for producing a green tea tablet, characterized in that carried out according to any one method selected from spray drying, vacuum distillation and freeze drying. According to claim 5,
In step (5), the tableting excipient containing the green tea residue and the green tea extract powder are mixed in a weight ratio of 3:7 to 7:3 and tableted. According to claim 5,
The method for producing a green tea tablet, characterized in that the catechin content of the green tea tablet of step (5) is 30 to 35 wt%. A green tea tablet prepared according to claim 5.

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