KR940000775B1 - Method for extracting smell removing component from green tea - Google Patents

Abstract

The method for extracting of odor eliminating components from green tea comprises; pulverizing dried green tea into 20-100 mesh size; adding extraction solvent to pulverized green tea powder; stirring and press juicing; centrifuging juicy solution; picking up supernatant; filtering precipitated ordor eliminating components in supernatant; concentrating filtered odor eliminating components. Also, the extraction method comprises; adding mixed extraction solvent with 40-60 % glycerin and water in green tea powder; reflux-distillating at 30-100 deg.C for 20 min. - 2 hrs..

Description

How to extract deodorant from green tea

1 is a comparative graph of each deodorant effect on the CH ₃ SH of the glycerin, water extraction solvent used in the present invention in Experimental Example 3 of the present invention.

2 is a graph comparing the deodorizing effect of the glycerin-water extract and the conventional solvent extract of CH ₃ SH in Experimental Example 3 of the present invention.

The present invention relates to a method for extracting deodorant from green tea, and more specifically, by using glycerin and water as extracting solvent, flavonoids, chlorophyll, etc. A room for extracting deodorant from green tea, which is useful for foods such as gum, candy, etc. by increasing the extraction yield and lowering the content of tannin and caffeine, which are bitter and astringent components. It's about the burr.

Recently, as the national income is improved and life is stabilized, interest in the bad breath which has become a local obstacle of social life is gradually increasing. Moreover, Koreans tend to prefer foods with strong odors such as garlic and kimchi, and research on how to effectively remove bad breath caused by meals is urgently needed.

Here, bad breath refers to the smell of exhalation (呼氣) coming out through the mouth to the people around you unpleasant. Such bad breath consists of volatile sulfur compounds produced by the degradation of epithelial, connective tissue, plant residues, oral bacteria, etc. in the saliva of protein in the saliva as protein resources. The main component of these sulfur compounds is methyl mercaptam (Methyl mercaptam). : CH ₃ SH), hydrogen sulfide (H ₂ S), dimethyl sulfide ((CH ₃ ) ₂ S) and the like, in particular methylmercaptan is known as the main component of the disgusting smell during bad breath.

Among the odors derived from food, the main component of garlic smell is sulfur compound of allyl mercaptan and diallyl disulfide, and the tobacco smell is known as pyridine derivative and amine. .

Flavonoids and chlorophyll are known among the substances that can remove bad breath, and these compounds are usually present in the form of glycosides in combination with sugars in nature. These flavonoid derivatives are As it is a polyphenol, it has chemical properties of phenol and is mass-producible, so it is decomposed from alkali and is ethanol (EtOH), methanol (MeOH), butanol (BuOH), acetone, and dimethyl sulfooxide (Dimethyl sulphoxide). : Soluble in organic solvents such as DMSO) and dimethyl formamide (DMF).

와 -SH, -NH의 중화(中和)반응, 또 유기산과 -NH의 중화반응, 당류의 악취물질의 흡수, 흡착, 용해작용 및 탄닌류의 에스테르(Easter)화와 에스테르교환반응 등의 화학적, 물리적인 작용에 의하여 이루어진다.Deodorizing action of flavonoids in green tea is related to the combination of flavonoids with phenol (pPhenol) and -NH in tannins, condensation of -SH and -NH in flavonoids, polymerization, addition reaction, and amino acid

Chemical reactions such as neutralization of -SH and -NH, neutralization of organic acids with -NH, absorption of odorous substances, adsorption, dissolution and esterification and transesterification of tannins. This is accomplished by physical action.

In addition, chlorophyll, which is present in Chloroplast, together with Carotenes and Xanthophylls, belonging to the Carotenoids, is insoluble in water, but in acetone, ether, benzene, etc. Melts well

Deodorization of chlorophyll is mainly carried out by chemical action, which mainly removes bad breath caused by food, tobacco and metabolism during neutralization and inclusion.

Therefore, among the methods for extracting flavonoids and chlorophyll, which are known to have bad breath removal effects, polar organic solvents such as methanol (MeOH), nucleic acid (Hexane) and chloroform are commonly used to separate and purify pure flavonoids and chlorophyll. On the other hand, extractable solvents that can be used in food manufacturing processes in Korea are mainly limited to water, alcohol, glycerin, propylene glycol (Propyleneglycol: PG), it is difficult to purify pure flavonoids and chlorophyll.

In addition, the conventional method of extracting the deodorant from the green tea generally extracted the deodorant components such as flavonoids and chlorophyll using water and alcohol as the extraction solvent, but tannin (13-20%, dry green tea content ratio) contained in the green tea Tea and caffeine (1.4 ~ 2.5%, dry green tea content ratio) of the bitter and astringent components are extracted a lot, so green tea extract according to this method is difficult to use in confectionery such as gum, Kendy.

In order to solve this problem, the present invention uses an appropriate ratio of glycerin and water as an extraction solvent to increase the extraction yield of deodorant components such as flavonoids and chlorophyll extracted from green tea and to contain less tannin and caffeine. It is an object of the present invention to provide a new method of extracting deodorant from green tea so that the deodorant component can be widely used in the manufacture of the same food.

Hereinafter, the present invention will be described in detail.

The present invention is pulverized dry green tea to 20 ~ 100 mesh size, the extract is added to the pulverized powdered green tea and stirred, and then juiced, the juice is centrifuged to take a supernatant, and then the supernatant is filtered and filtered It is a method of extracting deodorant from green tea by concentrating deodorant, and is characterized in that it is refluxed by adding an extraction solvent mixed with 40 to 60% glycerin and 60 to 40% water to powdered green tea.

In the method of the present invention, centrifugation for 10 minutes to 1 hour at a temperature of 0 ~ 30 ℃, 1,000 ~ 20,000rpm in the winsimal separation of the juice solution, and also by adding a glycerin-water extraction solvent to the powder green tea to reflux distillation In performing, it implements on the conditions of 20 minutes-2 hours at 30-100 degreeC.

Hereinafter, the present invention will be described in more detail.

The method for extracting the deodorant component from the green tea according to the present invention will be described in detail according to the process. Then, the green tea collected from the mountain region in the first step is immediately dried to a moisture content of 2 to 5%. Grind to 20 ~ 100 mesh size using a grinder.

Then, in the second step, 900 g of a mixed solvent of 40 to 60% glycerin and 60 to 40% water was added to 100 g of the powdered green tea ground in the first step, and then heated at a temperature of 30 to 100 ° C. in a Reflux Dkistillator. Distilled under reflux for 20 minutes to 2 hours and then juiced using a juicer to obtain juice.

At this time, the mixing ratio of glycerin-water is preferably 40 to 60%, 60 to 40%. This is because too much glycerin extracts less water-soluble flavonoids, and too much water extracts tannins and caffeine, both bitter and astringent.

In addition, reflux distillation is used, because this method can prevent moisture loss and increase the extraction effect, and the temperature at that time is 30 to 100 ° C, which is a problem of extracting a large amount of tannin and caffeine at too high a temperature, and too This is because the extraction yield may be reduced at low temperatures.

In addition, if the reflux time is too short, the extraction yield of the deodorant is lowered, it is preferable to reflux at least 20 minutes to 2 hours.

In the present invention, the relationship between temperature and time during reflux distillation has a relationship between taste difference and extraction yield according to the composition of green tea extract, and may be extracted by adjusting the conditions appropriately.

In the third step, the juice obtained in the second step is poured into a centrifuge at 0 to 30 ° C and 1,000 to 20,000 rpm, centrifuged for 10 minutes to 1 hour, the supernatant is taken, and then 12 to 36 hours in a refrigerator at 20 ° C or lower. Refrigerate.

In the fourth step, the green tea extract is obtained by removing the precipitates in the refrigerated supernatant stored in the third step using celite filtration.

In the fifth step, the extract obtained in the fourth step is vacuum evaporated to obtain a concentrated solution and commercialize it.

The deodorant component extracted from green tea according to this process has a lower content of tannin and caffeine, which is less bitter and astringent than the deodorant component extracted with water and alcohol, which are commonly used extraction solvents. Since the yield is also high, there is an effect that can be widely applied to the manufacture of favorite food, such as gum and candy having a deodorant function.

In order to confirm this, chlorophyll and flavonoid components, which are known to have a strong bad breath inhibitory effect among green tea active ingredients, are extracted by different solvent extraction methods, and methylmercaptan (CH), which is the main ingredient of bad breath according to various green tea extracts Deodorization effect on ₃ SH) was compared by in vitro experiments.

Hereinafter, the present invention will be described in detail with reference to Examples.

[Preparation of Experimental Materials]

The deodorizing effect of five green tea extracts extracted from green tea (2% water content, 2nd tea), which was directly collected and dried in Dawon, Jeonnam, was measured in July 1989.

The five green tea extracts are green tea flavonoids extracted from methanol and water (9: 1), glycerin and water (1: 1), ethanol and water (1: 1), room temperature water (25 ℃), high temperature water (80 ℃), etc. It is extracted using a solvent.

EXAMPLE

100 g of powdered green tea was added with 900 g of glycerin and water in a ratio of 1: 1, stirred at 75 ° C. for 30 minutes, extracted, cooled at room temperature, and centrifuged at 10,000 rpm for 20 minutes to extract green tea extract as a supernatant. It was refrigerated for one day at below ℃. The extract cooled to 10 ° C. or less was filtered through filter paper and Celite.

The filtered extract was concentrated in vacuo at 65 ~ 70 ℃ using a vacuum concentrator to obtain a green tea extract 380g.

As a result of experiments by varying the mixing ratio of glycerin and water among the above extraction methods, the extraction yield of green tea extract was different (Table 1). In the deodorizing effect experiment, representatives of glycerin and water were 50% each (1: The green tea extract of 1) was tested.

TABLE 1

Comparative Example 1

The dried green tea (water content 2%, 100g) was pulverized to 50 mesh or less using a grinder, and then a solvent containing methanol and water of 9: 1 was added to the ground green tea sufficiently and extracted for 6 hours while stirring at room temperature.

The extracted extract was filtered to obtain a primary filtrate and a primary residue. The primary filtrate was stored in a refrigerator at 10 ° C. or lower for 2 days, and the primary residue was a solvent containing methanol and water 1: 1. Extracted. At this time, the mixture was stirred at room temperature and extracted for 18 hours.

The secondary extract was filtered to obtain a secondary filtrate and a secondary residue. At this time, the secondary residue was discarded and the secondary filtrate was refrigerated at 10 ° C. or lower for 1 day. The cold filtrate and the secondary filtrate were mixed and filtered and concentrated in vacuo to 3/1 of the total volume to remove methanol.

The concentrate obtained at this time was placed in a separatory funnel and extracted and separated several times with chloroform. The supernatant was concentrated in vacuo to give only 72 g of tan-brown flavonoids from which chloroform was completely removed.

Comparative Example 2

To 100 g of powdered green tea, ethanol and water were added at a ratio of 1: 1, and the mixture was refluxed at 78 ° C. for 30 minutes, immediately cooled to room temperature, juiced with a juicer, and the filtrate was centrifuged at 10,000 rpm for 20 minutes. Green tea extract, the supernatant, was refrigerated for 1 day at 10 ℃ or less. After filtering the extract stored below 10 ℃ with filter paper, the filtered precipitate was concentrated under reduced pressure at 50 ℃ using a vacuum concentrator to obtain 31g of green tea extract.

Comparative Example 3

Pure water of room temperature (25 ° C.) was added to 100 g of powdered green tea, which was stirred for 10 minutes, and then juiced using a juicer. The filtrate was refrigerated for one day at 10 ° C. or lower. The extract cooled to 10 ° C. or less was filtered with a filter paper, and the filtered extract was concentrated in vacuo at 65 ° C. using a vacuum concentrator to obtain 26.2 g of green tea extract.

[Comparative Example 4]

Pure water at 80 ° C. is added to 100 g of powdered green tea, followed by stirring extraction for 2 minutes. The extracts were immediately juiced and the filtrate was stored under refrigeration at 10 ° C. for 1 day.

Experimental Example 1

in vitro experiment

Five extracts extracted from green tea by the Examples and Comparative Examples 1 to 4 were taken in each of 8g each to make 40ml of water, dissolved well, and then placed in a 100ml volumetric flask and heated in a 36 ° C water bath. Stir for a minute and leave.

Then, ₃ ml of CH ₃ SH gas was taken into the above volumetric flask, and 0.3 m of the gas was injected into GC (Gas Chromatography). The reaction was continued for 10 minutes, 15 minutes, and CH ₃ SH was reacted with deodorant in water. At 30 minutes, 45 minutes, and 60 minutes, 0.3 ml of the sample was taken from the upper space of the volumetric flask and injected into GC to determine the amount of CH ₃ SH remaining. The blank test of the deodorizing effect on glycerin and water, green tea extraction solvents, was also performed in the same manner as above.

Gas Chromatography (Shim) with Flame Photometric Detector (FPD) to measure the residual amount of methylmercaptan after odor addition

adzu-9A) was used, and the column was TCEP (25%, 1,2,3-Tris (2-Cyano ethxy) Propane, L = 3m, ψ = 1/8 inch) and the conditions of GC Is shown in Table 2 below.

TABLE 2

Experimental Example 2

Determination of Caffeine and Tannins

Caffeine Quantitative Analysis

The caffeine content of green tea extract was measured by injection into HPLC under the conditions shown in Table 3 according to the HPL method of Blauch et al.

TABLE 3

Tannin Quantitative Analysis

Tannin content of green tea extract was measured according to the Association of Official Analytical Chemist (AOAC) method.

Experimental Example 3

Deodorization effect of various substances by in vitro experiment

[Glycerine and water]

The results of experiments on the deodorizing effect of glycerin and water remaining in the green tea extract on CH ₃ SH by a blank test are shown graphically in FIG. 1, which shows a high viscosity glycerin (viscosity: 6.05 Chen / 50% solution, 20 in ℃) is in yongmaeeun glycerin indicate the remaining amount of the 10 minutes, when 98%, 15 minutes when 95%, 30 minutes when 70% to 90%, and 45 minutes, when 88%, 60 minutes when CH ₃ SH deodorizing effect is very appeared less to water is 10 minutes, when 89.7%, 15 minutes when 86.4%, 30 minutes when 72.4% 45 minutes, when 567%, 60 minutes when CH ₃ SH remaining in the 56.4% As it shows a small amount of deodorizing effect, the deodorizing effect of glycerin and water is almost negligible.

[Comparison of Yield and Deodorization Effect of Green Tea Extract by Solvent]

Compared with 100 g of dry powder green tea, the amount of extract extracted using a solvent usable for food, 380 g of glycerin-water extraction (5% green tea extract content, 56.5% glycerin, 38.5% moisture, 1.42 refractive index), ethanol-water extraction 31g (TS 50%), 26.2g (TS 50%) of extracting room temperature water, 40g (TS 50%) of extracting hot water were obtained, the extraction yield of these four green tea extracts are shown in Table 4. , The yield of glycerin-water extract was obtained 10 times higher than the extraction yield of ethanol-water and other methods.

TABLE 4

The results of the deodorant effect on the five green tea extracts including pure green tea flavonoids are shown in the graph at 2 degrees. The ethanol-water extract extracted using ethanol and water as 1: 10%, 15 minutes, when viewed the CH ₃ SH residual amount of 8.6%, 30 minutes when 3.1% and 2.2% when 45 minutes elapsed time by 2.4%, 60 minutes showed a superior deodorizing effect using an organic solvent of methanol and water and chloroform the pure green tea flavonoid extract extracted for 10 minutes, when 11.2%, 15 minutes when 10.4%, 30 minutes when 3.9%, 45 minutes when 2.9%, 60 minutes when strong show ₃ SH residual amount of CH 2% Deodorant effect was shown.

In addition, the deodorizing effect of the glycerin-water extract extracted using glycerin and water according to the present invention 1: 15.0% after 10 minutes, 14.6% after 15 minutes, 4.6% after 30 minutes, 3.1 after 45 minutes %, CH ₃ SH remaining amount of 2.1% after 60 minutes showed a very good deodorant effect.

On the other hand, the deodorant effect on high water (80 ℃) extract was 19.5% after 10 minutes, 16.3% after 15 minutes, 6.4% after 30 minutes, 5.3% after 45 minutes, 3.4% after 60 minutes ₃ SH residual amount, deodorant effect on room temperature water (25 ℃) extract was 30.5% after 10 minutes, 29.3% after 15 minutes, 20.3% after 30 minutes, 19.6% after 45 minutes, 60 minutes The deodorizing effect was lowest with 18.9% CH ₃ SH remaining. From these results, Glycerin-water extract showed more than 10 times higher extract deodorization effect than ethanol-water extract.

In addition, there was a difference in the extraction yield and composition of green tea extract depending on the difference between the mixture ratio of glycerin and water (40-60%), but there was no significant difference in the deodorizing effect.

Experimental Example 4

Comparison of Caffeine and Tannin Contents of Green Tea Extracts

Caffeine and tannin content of glycerin-water extract, ethanol-water extract, room temperature water extract, and hot water extract in green tea extracts were measured and shown in Table 5. The caffeine and tannin content of the green tea bitter and astringent taste components were used. According to the present invention, the glycerin-water extract according to the present invention, which has a high yield of extraction more than 10 times, is low in caffeine 0.6% and tannin 3.7% per unit weight of extract, compared to other extracts. This was very little. The ethanol-water extract and the hot water extract were relatively high in caffeine and tannins, and the taste was much bitter.

TABLE 5

Chlorophyll and flavonoids, which are known to have a strong bad breath inhibitory effect among the active ingredients of green tea from green tea through the above-described examples, comparative examples and experimental examples, were extracted by different solvent extraction methods, and bad breath according to various green tea extracts Deodorization effect on the main component methylmercaptan (CH ₃ SH) was compared by in vitro experiments. As a result, the ethanol-water extract with high deodorizing effect and the hot water extract have strong bitterness and astringent taste among green tea extracts extracted with a solvent usable for food, but the use of preference food is limited, but the glycerin-water extract of the present invention is very In addition to the deodorant effect, the bitter and astringent taste is relatively small, and the extraction yield is more than 10 times, so it can be easily used for favorite foods such as gum and candy.

Claims (1)

Dry green tea is pulverized with 20 ~ 100 mesh cree, add extractive solvent to the pulverized powdered green tea, stir, extract, extract, extract juice, take supernatant and filter small amount of deodorant precipitated in the supernatant. In the method of extracting the deodorant component from the green tea consisting of concentrating the filtered deodorant component, 20 minutes at 30-100 ° C by adding an extraction solvent in which 40-60% glycerin and 60-40% water are added to powdered green tea. Method for extracting deodorant components from green tea, characterized in that distilled reflux for 2 hours.

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