KR20190142082A - Method of preparing green tea extract containing high phenolic acid compound - Google Patents

Abstract

The present invention relates to a method for extracting green tea and a green tea extract prepared thereby. More specifically, the green tea extract can be prepared at low cost and high yield using a shaking extraction. The green tea extract of the present invention contains a large amount of catechin compounds and polyphenol compounds. In particular, the phenolic acid compound is contained at a higher content than products prepared by other extraction methods. The green tea extract can be useful in various fields, such as medicine, health food and cosmetics.

Description

Method of preparing green tea extract containing high phenolic acid compound {Method of preparing green tea extract containing high phenolic acid compound}

The present invention relates to a method for producing green tea extract.

Green tea is a long-established beverage made from the leaves and leaves of Camellia sinensis, which belongs to Teaceac and Camellia, and has been a favorite food in East Asia for a long time.

Green tea contains 75 to 80% of the fresh leaves and the rest contains solid polyphenol compounds (flavanols, flavandiols, flavonoids, phenolic acid). Most of these polyphenolic compounds are commonly known as catechins. In addition, it contains various vitamins, alkaloids (caffeine, etc.), pigments, 28 kinds of amino acids including deanine and glutamic acid, minerals, various enzymes (polyphenoloxidase, etc.), organic acids and carbohydrates. Green tea contains a lot of catechin compounds compared to ordinary plants, and unlike other plants, it is associated with various physiological activities. Until now, various research results of green tea catechin compounds have been reported, and in particular, anti-cancer, antioxidant, antibacterial, anti-viral, anti-allergic, blood pressure increase suppression, blood cholesterol lowering effect, caries prevention and the like have been reported.

However, most of the methods for extracting the active ingredient from green tea were performed through various extraction methods such as hot water extraction, solvent extraction, ultrasonic extraction, and supercritical extraction. Such extraction methods have problems such as low yield, stability, and high cost. Therefore, low cost, high efficiency extraction technology is needed.

Green tea-derived catechin compounds mostly exist in free form, but some of them exist in the form of bonds in cell walls. Green tea also contains phenolic acid compounds such as gallic acid, ferulic acid, and sinapic acid. Most of them are very hard in bound form on the green tea cell wall, and the extraction methods that are commonly used, that is, hot water or solvents, are not easily eluted during extraction. There is a need for the development of a new technology that can extract all the useful components present in the cell wall in free and bound form.

If a new extraction technology, that is, green tea is applied in combination with temperature and shaking, the green tea-derived functional ingredients are eluted with a large amount of catechin compounds or phenolic acids due to the destruction of the cell walls, thereby extracting them at low cost and high efficiency. In particular, the extraction of green tea using agitation can increase the catechin compound rather than hot water extraction, as well as obtain a green tea extract containing a lot of phenolic acid compounds. Among phenolic acids, phenolic acid-derived gallic acid compounds are expected to be extracted more than twice.

Korean Patent Registration No. 1548131

An object of the present invention is to provide a method for producing a green tea extract having a low cost, high extraction yield, in particular, a high extraction yield of a phenolic acid compound using a shaking extraction method.

1. First step of grinding green tea leaves to obtain green tea powder; A second step of adding hot water to the green tea powder and shaking for 5 to 25 minutes at a frequency of 0.5 to 5 Hz at a frequency of 0.5 to 5 Hz at a temperature of 50 to 90 ° C. to obtain a green tea mixture; And a third step of obtaining the green tea extract by filtering the green tea mixture through a filter paper.

2. The method according to the above 1, wherein the horizontal moving frequency per second is the frequency per second of the horizontal reciprocating motion, manufacturing method of green tea extract.

3. The method of 1 above, wherein the horizontal movement frequency per second is 0.833 to 3.33 Hz, the method of producing green tea extract.

4. according to the above 1, wherein the green tea powder is obtained by passing the crushed green tea leaves through a 30 to 50 mesh sieve, a method for producing green tea extract.

5. according to the above 1, wherein the hot water is 50 to 90 ℃ distilled water, the production method of green tea extract.

The present invention provides a method for producing green tea extract with low cost and high yield, and the green tea extract prepared according to the present invention contains a large amount of catechin compound and polyphenol compounds. In particular, compared to the general green tea extraction method can produce a green tea extract with a high content of phenolic acid, the extract according to the present invention can be utilized in various fields, such as pharmaceuticals and health functional food, cosmetics.

One embodiment according to the manufacturing method of the green tea extract of the present invention is a first step of obtaining green tea powder by grinding the dried green tea leaves; A second step of adding hot water to the green tea powder and shaking for 5 to 25 minutes at a frequency of 0.5 to 5 Hz at a frequency of 0.5 to 5 Hz at a temperature of 50 to 90 ° C. to obtain a green tea mixture; And a third step of obtaining the green tea extract by filtering the green tea mixture through a filter paper.

One embodiment of the present invention comprises a first step of obtaining a green tea powder by grinding the dried green tea leaves.

To obtain green tea powder, the green tea leaves undergo a sufficient drying process before grinding. Grinding can be used without limitation as long as it is a known grinding method.

The green tea powder may be obtained by passing crushed dry green tea leaves through a 30 to 50 mesh sieve, and preferably, may be performed with a 35 to 45 mesh sieve, but is not limited thereto.

When using a mesh sieve smaller than 30 mesh sieve in the first step, it is difficult to elute the active ingredients in the green tea extract, when using a mesh sieve larger than 50 mesh sieve, the extraction yield does not show a significant difference.

Next, an embodiment of the present invention is a second step of obtaining a green tea mixture by adding hot water to the obtained green tea powder, shaking for 5 to 25 minutes at a frequency of 0.5 to 5 Hz horizontal movement per second at a temperature of 60 to 80 ℃; It includes.

In one embodiment of the present invention, the hot water may be water of an appropriate temperature,

For example, the temperature of the hot water may be 50 to 90 ° C, preferably 60 to 80 ° C, but is not limited thereto. Extraction effect through shaking in the above temperature range can be maximized. If the hot water temperature is less than 50 ℃ useful components may not be sufficiently eluted, if the hot water is above 90 ℃ useful components may be destroyed.

Water used as hot water is not particularly limited, but may be, for example, distilled water, but is not limited thereto.

In the present invention, agitation is distinguished from agitation, in which agitation means mixing the contents of the container by rotating it by using a stirrer or the like, whereas in the case of agitation, the contents are moved by moving the container itself. It means mixing.

In one embodiment of the invention, the horizontal movement may comprise a horizontal reciprocating motion.

In one embodiment of the present invention, when the horizontal movement is a horizontal reciprocating motion, the frequency of the horizontal movement per second may be the frequency per second of the horizontal reciprocating motion.

In one embodiment of the present invention, the horizontal moving frequency per second may be 0.5 to 5 Hz, preferably 0.833 to 3.33 Hz, but is not limited thereto.

In one embodiment of the present invention, when the horizontal movement is a horizontal reciprocating motion, one reciprocating distance may be 5 mm to 600 mm, preferably 10 mm to 300 mm, but is not limited thereto.

If the shaking horizontal movement is less than the frequency per second or the range of the reciprocating distance, the useful components of the green tea may not be sufficiently eluted, if larger than that may not be good in terms of efficiency.

As a condition of the shaking, the temperature may be 50 to 90 ° C., preferably 60 to 80 ° C., but is not limited thereto.

If the shaking performance temperature is less than 50 ° C, useful components may not be sufficiently eluted, and if it is above 90 ° C, useful components may be destroyed.

The shaking time may be 5 minutes to 25 minutes, preferably 10 minutes to 20 minutes. However, it is not limited thereto.

If the shaking time is less than 5 minutes, the components to be eluted may not be sufficiently eluted, and if it exceeds 25 minutes, the flavor may be bad, or the color of the extract may be dark, which may not be suitable for the consumer's taste. People may be oxidized to reduce the content.

Furthermore, when the shaking performance temperature is greater than 90 ° C. and the shaking performance time is greater than 25 minutes, a large amount of useful components may also be destroyed.

Next, according to an embodiment of the present invention, a third step of obtaining a green tea extract by filtering the green tea mixture obtained after shaking through a filter paper.

The filter paper in the third step may be used commercially available filter paper, for example, Whatman No. 1 filter paper may be used, but is not limited thereto.

In one embodiment of the present invention, the green tea mixture may be filtered and then further cooled. Cooling may be accomplished by leaving at room temperature, but is not limited thereto.

The room temperature may be 20 to 30 ° C, preferably 23 to 27 ° C, but is not limited thereto. If cooling takes place above 30 ° C., the components of the green tea extract may be destroyed or oxidized.

According to the method for producing green tea extract of the present invention, the extraction yield of the active substance contained in green tea is good.

The green tea extract prepared by the method of the present invention has a high content of a catechin compound or a phenolic acid compound.

In the case of the extraction method of the previously known green tea, in particular, the extraction yield of the phenolic acid compound is not a good method, while the green tea extract according to the present invention is very good extraction yield for the phenolic acid compound.

The catechin compound contained in the green tea extract may be included without limitation if it is a catechin compound included in green tea, for example, epigallocatechin gallate ((-)-Epigallocatechin gallate), catechin ((-)-catechin) , Gallocatechin gallate ((-)-gallocatechin gallate), epigallocatechin ((-)-epigallocatechin), gallocatechin ((-)-gallocatechin), epicatechin gallate ((-)-epicatechin gallate), catechin gallate Eight catechin compounds, such as rate ((-)-catechin gallate). However, it is not limited thereto.

In addition, the phenolic acid compound contained in the green tea extract may be included without limitation if the phenolic acid compound contained in green tea, for example, gallic acid (gallic acid), ferulic acid (ferulic acid), cinapic acid (sinapic acid) And phenolic acid compounds such as, but are not limited thereto.

The catechin compound and phenolic acid compound of green tea are known to have various activities such as anti-inflammatory, antioxidant, antibacterial, anti-aging, body fat decomposition, detoxification, and anti-diabetic, and these activities are already well known. Omit.

Hereinafter, Examples 1 to 7, using the shaking extraction method of the present invention, Comparative Examples 1 to 6 using the hot water extraction method, Comparative Examples 7 to 12 using the stirring extraction method, the temperature and time of shaking were changed in order to explain the present invention in detail. The comparative example 13 and the experimental example which compared these are demonstrated in detail.

Example  -Shake extraction method of the present invention

One. Example  One

The green tea dry leaves were ground and passed through a 40 mesh sieve to obtain green tea powder. 1 g of the obtained green tea powder was poured into 100 ml of distilled water (temperature 60 ° C.) contained in a conical flask, and then shaken for 10 minutes at a frequency of 60 ° C. and a shaking horizontal reciprocating motion of 1.66 Hz in a constant temperature bath for 10 minutes. Thereafter, green tea extract was obtained after filtration through Whatman No. 1 filter paper and cooling at room temperature (25 ° C.).

2. Example  2

It carried out similarly to Example 1, but set it as 70 degreeC instead of the temperature of 60 degreeC.

3. Example  3

It carried out similarly to Example 1, but set it as 80 degreeC instead of the temperature of 60 degreeC.

4. Example  4

It carried out similarly to Example 1, but set it as 20 minutes instead of 10 minutes.

5. Example  5

It carried out similarly to Example 1, but set it as temperature 70 degreeC and time 20 minutes instead of temperature 60 degreeC and time 10 minutes.

6. Example  6

It carried out similarly to Example 1, but made temperature 80 degreeC and time 20 minutes instead of temperature 60 degreeC and time 10 minutes.

7. Example  7

It carried out similarly to Example 1, but set it as time 25 minutes instead of time 10 minutes.

Comparative example  - Hydrothermal  Extraction

One. Comparative example  One

The green tea dry leaves were ground and passed through a 40 mesh sieve to obtain green tea powder. 1 g of the obtained green tea powder was poured into 100 ml of distilled water (temperature 60 ° C.) contained in a conical flask, followed by extraction for 10 minutes, filtered through Whatman No. 1 filter paper. After cooling at room temperature (25 ° C.), green tea extract was obtained.

2. Comparative example  2

The same process as in Comparative Example 1, but the temperature 60 ℃ Instead it was 70 ℃.

3. Comparative example  3

It carried out similarly to the comparative example 1, but set it as 80 degreeC instead of the temperature of 60 degreeC.

4. Comparative example  4

It carried out similarly to the comparative example 1, but set it as 20 minutes instead of 10 minutes.

5. Comparative example  5

It carried out similarly to the comparative example 1, but was made into temperature 70 degreeC time 20 minutes instead of temperature 60 degreeC and time 10 minutes.

6. Comparative example  6

It carried out similarly to the comparative example 1, but made temperature 80 degreeC time 20 minutes instead of temperature 60 degreeC and time 10 minutes.

Comparative example  - Stirring  Extraction

One. Comparative example  7

The green tea dried leaves were ground and passed through a 40 mesh sieve to obtain green tea powder. 1 g of the obtained green tea powder was poured into 100 ml of distilled water (temperature 60 ° C.) contained in a conical flask and stirred in a constant temperature water bath at a temperature of 60 ° C., 100 rpm for 10 minutes, and then Wattman No. 1 ( Whatman No.1) The green tea extract was obtained after filtration through filter paper and cooling at room temperature (25 ° C).

2. Comparative example  8

In the same manner as in Comparative Example 7, the temperature is 60 ℃ Instead it was 70 ℃.

3. Comparative example  9

It carried out similarly to the comparative example 7, but set it as 80 degreeC instead of the temperature of 60 degreeC.

4. Comparative example  10

It carried out similarly to the comparative example 7, but set it as 20 minutes instead of 10 minutes.

5. Comparative example  11

It carried out similarly to the comparative example 7, but set it as temperature 70 degreeC time 20 minutes instead of temperature 60 degreeC and time 10 minutes.

6. Comparative example  12

It carried out similarly to the comparative example 7, but made temperature 80 degreeC time 20 minutes instead of temperature 60 degreeC and time 10 minutes.

concussion Comparative example

One. Comparative example  13

It carried out similarly to Example 1, but set it as temperature 95 degreeC and time 35 minutes instead of temperature 60 degreeC and time 10 minutes.

Experimental Example  -Analysis of Contents of Catechin Compounds and Phenolic Acid Compounds in Green Tea Extracts According to Extraction Methods

Table 1 shows the content of the catechin compound of the green tea extract according to the extraction method, Table 2 shows the content of the phenolic acid compound.

As can be seen in Table 1, Examples 1 to 7 can be seen to show a higher catechin compound content than Comparative Examples 1 to 12, the shaking extract method to produce a green tea extract with a higher content of catechin compound than the hydrothermal extraction method or stirring extraction method I could see that.

In addition, when comparing the catechin compound content of Examples 1 to 7 and Comparative Example 13, it was found that the shake temperature and shaking time were out of the range of shaking temperature of 95 ° C and shaking time of 35 minutes.

In addition, in the content of the total phenolic acid compound in Table 2, Example 6 showed a higher phenolic acid content than Comparative Examples 6 and 12, through which the shaking extraction method has a higher phenolic acid content than the hot water extraction method and stirring extraction method It can be seen that the green tea extract can be prepared.

In addition, in Table 2, Example 6 shows a higher phenolic acid content than Comparative Example 13, indicating that the extraction efficiency is deteriorated when the shaking temperature is 95 ° C. and the shaking time is 35 minutes out of the range of shaking temperature and shaking time of the present invention. Could.

Therefore, the green tea extract according to the present invention was confirmed to contain a higher content of phenolic acid compounds than other extraction methods.

EGCG C GCG ECG GC EGC CG Example 1 (shaking, 60 ° C., 10 minutes) 24.4 ± 3.7cd 19.5 ± 0.5bc 6.9 ±
0.1c 52.7 ±
4.0b 0.9 ± 0.2c 24.3 ±
1.2b 7.5 ±
0.0cd Example 2 (shaking, 70 ° C., 10 minutes) 27.9 ± 0.4c 16.9 ± 0.5c 6.4 ±
0.3c 52.3 ±
4.8b 1.0 ± 0.2bc 24.0 ±
2.7b 7.4 ±
0.1cd Example 3 (shaking, 80 ° C., 10 minutes) 30.9 ± 3.5b 21.0 ± 2.7bc 7.1 ±
1.4bc 61.1 ±
2.3a 1.1 ± 0.9bc 31.2 ±
4.3ab 7.8 ±
0.2b Example 4 (shaking, 60 ° C., 20 minutes) 37.4 ± 0.3ab 20.7 ± 2.2bc 6.6 ±
0.3c 59.1 ± 3.7ab 0.9 ± 0.0c 28.9 ±
0.5ab 7.7 ±
0.0bc Example 5 (shaking, 70 ° C., 20 minutes) 32.1 ± 1.3b 22.3 ± 4.1b 8.8 ±
0.1b 59.4 ± 1.4ab 2.1 ± 0.1b 29.6 ±
1.8ab 7.6 ±
0.1bc Example 6 (shaking, 80 ° C., 20 minutes) 39.2 ± 1.2a 27.9 ± 5.3a 11.9 ±
2.7a 63.7 ±
1.3a 3.6 ±
0.4a 34.2 ±
3.0a 7.8 ±
0.3b Example 7 (shaking, 60 ° C., 25 minutes) 40.5 ±
0.9a 23.6 ±
0.8b 7.8 ±
0.4bc 62.5 ±
2.0a 1.3 ±
0.1bc 30.2 ±
0.3ab 9.2 ±
0.5a Comparative Example 1 (hot water, 60 ° C., 10 minutes) 10.8 ± 2.3g 9.3 ± 0.3e 6.1 ±
0.0d 21.6 ±
3.6f 0.5 ± 0.0e 9.0 ±
0.3 g 7.2 ±
0.0d Comparative Example 2 (hot water, 70 ° C., 10 minutes) 11.3 ± 1.4f 8.6 ± 0.8e 6.0 ±
0.1d 23.4 ±
3.6f 0.5 ± 0.0e 9.9 ±
1.2 g 7.2 ±
0.1d Comparative Example 3 (hot water, 80 ° C., 10 minutes) 12.9 ± 2.7f 10.5 ± 2.3d 6.1 ±
0.2d 26.8 ±
3.4e 0.6 ± 0.0d 12.2 ±
1.5f 7.2 ±
0.1d Comparative Example 4 (hot water, 60 ° C., 20 minutes) 11.0 ± 2.6fg 10.3 ± 0.2d 6.1 ±
0.0d 25.3 ±
3.1e 0.6 ± 0.0d 12.3 ±
0.1f 7.3 ±
0.0cd Comparative Example 5 (hot water, 70 ° C., 20 minutes) 13.5 ± 1.0f 10.0 ± 0.5d 6.0 ±
0.0d 27.7 ±
1.5e 0.6 ± 0.0d 13.2 ±
0.2e 7.3 ±
0.0cd Comparative Example 6 (thermal water 80 ° C., 20 minutes) 15.3 ± 2.5f 11.1 ± 1.4d 6.1 ±
0.4d 28.0 ±
4.8e 0.8 ± 0.3c 14.2 ±
0.7e 7.2 ±
0.1d Comparative Example 7 (stirring, 60 ° C., 10 minutes) 16.8 ±
2.6f 13.5 ±
1.8c 6.2 ±
0.2d 36.5 ±
2.9d 0.8 ±
0.1c 18.6 ±
1.6cd 7.1 ±
0.3d Comparative Example 8 (stirring, 70 ° C., 10 minutes) 20.1 ±
3.9d 12.1 ±
2.3cd 6.1 ±
0.1d 38.9 ±
4.6cd 0.6 ±
0.1d 19.2 ±
2.1bc 7.2 ±
0.1d Comparative Example 9 (stirring, 80 ° C., 10 minutes) 21.8 ±
4.5d 14.6 ±
2.7c 6.0 ±
0.2d 40.2 ±
3.9cd 0.8 ±
0.2c 20.3 ±
2.1bc 7.3 ±
0.4cd Comparative Example 10 (stirring, 60 ° C., 20 minutes) 20.5 ±
2.8d 13.4 ±
2.8c 6.2 ±
0.1d 45.6 ±
5.6c 0.8 ±
0.1c 17.6 ±
3.2d 7.0 ±
0.3d Comparative Example 11 (stirring, 70 ° C., 20 minutes) 18.5 ±
3.2de 14.6 ±
3.9c 6.0 ±
0.3d 48.4 ±
2.6bc 0.7 ±
0.1c 20.3 ±
2.5bc 7.1 ±
0.5b Comparative Example 12 (stirring, 80 ° C., 20 minutes) 19.5 ±
6.7de 15.5 ±
4.1bc 6.1 ±
0.3d 45.6 ±
6.3c 0.7 ±
0.3c 21.6 ±
3.6bc 7.1 ±
0.1d Comparative Example 13 (shaking, 95 ° C., 35 minutes) 20.6 ±
1.6d 15.3 ±
2.0c 6.3 ±
1.9cd 49.2 ±
1.3bc 0.8 ±
0.2c 22.5 ±
3.2bc 7.0 ±
0.1d

1.mg/g dry weight

2. The figures represent the mean ± standard deviation.

3. Lowercase letters a through g in the upper right of the data indicate that the data are statistically significantly different from each other (p <O.05).

4.EGCG (Epigallocatechin Gallate), C (Catechin), Gallocatechin GCG (Gallate), ECG (Epigallocatechin), GC (Galocatechin), EGC (Epicatechin Gallate), CG (Catechin Gall) Rate).

Garlic acid
(gallic acid) Sinapic Acid
(sinapic acid) Ferulic acid
(ferulic acid) Total phenolic acid
(total phenolic acid) Example 6
(Shaking, 80 ° C, 20 minutes 10.2 ± 0.6a 0.5 ± 0.0a 0.7 ± 0.0a 11.4 ± 0.5a Comparative Example 6
(Hot water 80 ° C, 20 minutes) 6.6 ± 0.6b 0.4 ± 0.1a 0.5 ± 0.0c 7.6 ± 0.5c Comparative Example 12 (stirring, 80 ° C., 20 minutes) 7.9 ± 0.9b 0.4 ± 0.1ab 0.5 ± 0.1b 9.1 ± 0.3bc Comparative Example 13 (shaking, 95 ° C., 35 minutes) 8.5 ± 0.6a 0.4 ± 0.1ab 0.6 ± 0.3a 9.5 ± 0.8b

1.mg/g dry weight

2. The figures represent the mean ± standard deviation.

3. Lowercase letters a and b in the upper right of the data indicate that the data are statistically significantly different from each other (p <O.05).

In the above described exemplary embodiments of the present invention by way of example, the scope of the present invention is not limited only to the specific embodiments as described above, those skilled in the art to the scope described in the claims of the present invention It will be possible to change accordingly.

Claims (5)

A first step of grinding green tea leaves to obtain green tea powder;
Adding a hot water to the green tea powder and shaking the mixture for 5 to 25 minutes at a frequency of 0.5 to 5 Hz at a frequency of 0.5 to 5 Hz at a temperature of 50 to 90 ° C. to obtain a green tea mixture; And
And a third step of obtaining the green tea extract by filtering the green tea mixture through a filter paper.
The method of claim 1, wherein the horizontal moving frequency per second is a frequency per second of horizontal reciprocating motion.
The method of claim 1, wherein the horizontal moving frequency per second is 0.833 to 3.33 Hz.
The method of claim 1, wherein the green tea powder is obtained by passing crushed green tea leaves through a 30 to 50 mesh sieve.
The method of claim 1, wherein the warm water is 50 to 90 ℃ distilled water, the method of producing green tea extract.