JPH0241165A - Deodorant containing tea leaf ingredients and method for producing the same - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a deodorant containing a tea leaf component, which contains tannin as a main deodorant active ingredient and is substantially free of caffeine. By combining a method of extracting active ingredients such as tannins as a deodorant with a solvent and a method of extracting and removing caffeine from tea leaves with a fluid in a supercritical state, we have created a tea leaf ingredient containing substantially no caffeine. The present invention relates to a method for producing a deodorant.

The tea leaf component-containing deodorant described above does not substantially contain caffeine, and therefore can be safely used for deodorizing foods such as mouth fresheners, candies, and chewing gums.

[Description of prior art]

Conventional methods for deodorizing or deodorizing include, for example, methods of masking bad odors with aromatic substances such as camphra oil, methods of oxidizing and decomposing odorous substances with oxidizing agents such as potassium permanganate, and methods of rendering odorless by using zinc sulfate. , aluminum sulfate,
A method of fixing bad odors such as ammonia and hydrogen sulfide using metal salt fields such as iron sulfate, and a method of neutralizing odorous substances and making them odorless using neutralizing agents such as salts, nitric acid, sodium hydroxide, and sodium carbonate. , a method of adsorbing bad odors with activated carbon, etc. has been used. However, all of these methods are often subject to significant limitations depending on the intended use, and have not been sufficiently developed in the food field in particular. So far, deodorants and deodorizers containing as an active ingredient thermal extracts of fresh or dried leaves of plants of the Camellia family or Lauraceae family using an alcohol-based organic solvent, a ketone-based organic solvent, water, or a mixed solvent thereof. (Tokuko Sho No. 58-1809
No. 8) A component obtained by extracting green tea with an organic solvent such as an alkyl ketone and then heating and saponifying it with an aqueous solution of caustic alkali, or a component obtained by heating and saponifying green tea with an aqueous solution of a caustic alkali and then using an organic solvent such as an alkyl ketone. A deodorizing agent characterized by containing a component obtained by extraction, or a component obtained by heating green tea with an aqueous caustic alkali solution and an organic solvent such as an alkyl ketone to simultaneously perform saponification and extraction. No. 58-190445) and the like have been proposed. In addition, as an improvement method of the invention disclosed in the above-mentioned Japanese Patent Publication No. 58-18098, which has the disadvantage that its use is restricted depending on the object to be deodorized due to its strong coloring and poor solubility in water, or/and heat-extracting fresh leaves of Lauraceae plants or dried leaves obtained by drying naturally or by heating them with steam or fire using a polyhydric alcohol-based organic solvent or a mixture of two or more of them; A deodorizer obtained by distilling the obtained thermally extracted solution under reduced pressure and separating the active ingredients by silica gel adsorption method (Japanese Patent Laid-open No. 6
No. 0-40059), fresh or dried leaves of plants of the Camellia family and/or Lauraceae family are treated with an alcohol-based organic solvent,
Perform cold extraction or hot extraction with a ketone organic solvent, polyhydric alcohol organic solvent, water or a mixed solvent thereof,
A deodorizer containing the extracted product as an active ingredient by subjecting the extract to a coloring treatment using activated carbon, acid clay, diatom clay, etc. (Japanese Patent Application Laid-Open No. 60-122566) etc. have been proposed.

However, the aforementioned Japanese Patent Publication No. 58-18098,
JP-A No. 58-190445, JP-A No. 60-4
The deodorants and deodorizers disclosed in Publication No. 0059 and Japanese Patent Application Laid-open No. 60-122566, etc. all contain caffeine, which has a stimulant effect on the central nervous system, heart, kidneys, etc., in their final products. For example, when these deodorizers are added to candy, chewing gum, etc. as mouth fresheners or breath odor removers, or as deodorizers added to foods, health problems may occur. It could not necessarily be said that it was a safe deodorizer.

Therefore, the emergence of a high value-added deodorizer/deodorizer that does not contain caffeine, has excellent safety, and has good deodorizing or deodorizing effects has been desired, especially in the food market field.

[Problem to be solved by the invention]

As mentioned above, the purpose of the present invention is to create a new deodorizing agent that solves the problems of conventional deodorizing and deodorizing agents, which include caffeine in the final product and are not necessarily satisfactory in terms of safety. An object of the present invention is to provide a deodorant containing tea leaf components and a method for producing the same.

[Means to solve the problem]

Therefore, in view of the problems of the prior invention mentioned above, the present inventors conducted intensive research with the aim of producing a deodorant that does not substantially contain caffeine. The present invention was finally achieved based on the knowledge that a deodorant with an extremely low caffeine content can be obtained by combining an extraction removal method and a method for extracting the active ingredient as a deodorant using a solvent.

That is, the first invention has 5 to 5 as the main deodorizing active ingredient.
Contains 20% by weight of tannins and has a deodorization rate of at least 8
The present invention relates to a deodorant containing a tea leaf component, which has a caffeine content of 0% or more and 1% by weight or less. Also, the second
The invention is based on (A) a fluid (first component) obtained by bringing tea leaves into a supercritical state from a gas in the presence of water, and a lower aliphatic saturated monohydric alcohol having 1 to 4 carbon atoms; (B) selectively extracting and removing caffeine from the tea leaves by bringing them into contact with a mixed solution of at least one alcohol-based organic solvent (second component) under a supercritical state; (B) a step of selectively extracting and removing caffeine from the tea leaves; The obtained extraction residue is extracted using a solvent, the raw material residue is filtered off from the obtained extraction solution, and the filtrate is concentrated or condensed to dryness to obtain a deodorizing stock solution or deodorant powder. The present invention relates to a method for producing a deodorant containing a tea leaf component, which is characterized by the following.

[Detailed explanation of each requirement of the present invention] There are various types of tea leaves that can be used as raw materials in the present invention, such as fresh leaves of tea plants such as green tea, black tea, oolong tea, and machi tea (also called Paraguayan tea). or its dried product, but green tea is particularly preferred as the type of tea plant.

The deodorant of the present invention contains 5 to 20% by weight of tannin as a main active ingredient having a deodorizing effect. Furthermore, the deodorant of the present invention contains, as active ingredients having a deodorizing effect, in addition to the above-mentioned content of tannins, which are the main components of tea, chlorophyll, flavonoids, amino acids, which are components of tea,
It may also contain organic acids, sugars, etc.

The deodorizer of the present invention has r
The deodorization rate 1 determined by the gas chromatographic analysis results for benzyl mercaptan and trimethylamine, which are malodorous substances, is at least 80% or more, preferably 90% or more, and especially for benzyl mercaptan, it is 80% or more, preferably 90% or more. % or more, and for trimethylamine 90% or more, preferably 95%
The above is desirable.

The deodorizing agent of the present invention has a deodorizing effect not only on the above-mentioned benzyl mercaptan and trimethylamine, but also on mercaptans and amine compounds other than those mentioned above, and other odorous components such as hydrogen sulfide, methyl sulfide, and ammonia. It is also effective against all kinds of other bad odors.

The mechanism of action of the deodorizing effect of the deodorant of the present invention is not clear, but it is probably due to condensation and chelation reactions with chlorophyll, which is a component of tea, or with polyphenol groups such as flavonoids and tannins, which are components of tea. -NI
The bond with the T group, and furthermore, the amino acid (7
) Nll □c (R) HCOOI (and -5H group,
-N) Neutralization reaction with l group, organic acid which is a component of tea and -N
It is thought that the deodorizing effect is exerted by a combination of chemical and physical effects such as neutralization reaction with H groups, or absorption, adsorption, and clathration by sugars, which are components of tea.

In the deodorant of the present invention, the caffeine content determined by the caffeine content measuring method described below is 1% by weight.
The content below is preferably 0.5% by weight or less, and substantially does not contain caffeine.

Next, the production method of the present invention utilizes selective extraction and removal method 1 of caffeine using T supercritical fluid, which was previously proposed by the present inventors and described in Japanese Patent Application No. 118165/1982. It is something.

In the production method of the present invention, the extraction solvent C is a combination of the first component and the second component used for decaffeinating the raw material tea leaves, hereinafter referred to as a mixed solution in this specification. ), the first component, that is, the fluid that brings the gas into a supercritical state during its use, is, for example, Co, which is harmless to health and does not cause chemical changes in the substance.
Gases such as 2, Neo, SF'6, Xe5CF4, methane, ethane, ethylene, acetylene, cyclopropane are suitable, and these gases can be used alone or in mixtures.

The second component to be added to the first component to form the mixed solution may have 1 to 4 carbon atoms, such as methanol, ethanol, propatool, isopropanol, butanol, isobutyl alcohol, 5ec-butyl alcohol, etc.
Lower aliphatic saturated monohydric alcohols are suitable and can be used alone or in admixture with one another.

The selection of the first and second components as a mixed solution depends on the selected application conditions, the type of tea plant and the second component, such as having the highest possible selectivity and solubility for caffeine. It is determined by the nature of the first component that is to be used to form a liquid mixed solution. That is,
If the first component has relatively low solubility and/or selectivity for caffeine under the application conditions, the mixed solution for producing the second component is selected to have high selectivity and solubility for caffeine. be.

Decaffeination from the raw material tea leaves is carried out by contacting the raw material tea leaves with the above mixed solution in a supercritical state in the presence of water, where "in the presence of water" means, for example, The amount of water that is entrained when the above-mentioned mixed solution in a supercritical state passes through water may be sufficient. Therefore, the water content may be less than the solubility of the first component in the supercritical state under the applied conditions, that is, less than saturation. For example, as will be described later, when carbon dioxide at a temperature of 50 cm and a pressure of 300 kg/cfifG is used as the first component in a supercritical state, which is an embodiment of the decaffeination treatment process of the present invention, Approximately 0.3 g-u2o,/g-Go
□It is sufficient if the water content is below. When the amount of water is low, the extraction of caffeine tends to be incomplete or unsatisfactory. On the other hand, if the amount of water is large, there is a problem that caffeine selectivity is lost and useful substances other than caffeine are extracted at the same time. In addition, methods for adding water to the extraction system to remove decaffeination include a method of humidifying solid tea leaves with water, a method of moistening the first component with water, and a method of adding water to the second component. Either is fine. Alternatively, - a combination of these methods may be used.

By the way, a preferred embodiment of the decaffeination treatment step of the present invention uses moist CO□ (carbon dioxide) gas in a supercritical state as the first component of the mixed solution, and ethanol as the second component of the mixed solution. This is a method for selectively extracting and removing caffeine from fresh green tea leaves or dried green tea leaves.

For dicarbonate as the first component of the mixed solution, the supercritical state with respect to temperature is a temperature higher than 31.6°C, which is the temperature of extraction according to a preferred embodiment of the decaffeination process of the present invention. is 32 to 100°C, preferably 32 to 60°C. When the extraction temperature is lower than 32°C, the amount of caffeine extracted sharply decreases, making the work of the decaffeination treatment method of the present invention extremely uneconomical.
Significantly longer extraction times are required.

The extraction pressure in the decaffeination treatment step of the present invention is such that at least the mixed solution (mixture of the first component and the second component) used in the decaffeination treatment step of the present invention is liquid at the selected composition and application temperature. should be chosen, and the upper limit of the extraction pressure applied in that case is determined solely by economic considerations. That is, when the extraction pressure is high, the extraction speed of caffeine is faster than when the extraction pressure is low, but the device is required to have high pressure resistance, and the equipment is costly. On the other hand, when a low pressure is applied as the extraction pressure, only a small amount of equipment is required, but the extraction speed of caffeine is slower and the extraction time is longer than when a high pressure is used. Therefore, for carbon dioxide as the first component of the mixed solution, the supercritical state 1 in terms of pressure is a pressure higher than 74.3 kg/ci G, which is the pressure of extraction according to the preferred embodiment of the decaffeination process of the present invention. is 75-500 kg/dG, preferably 75-350 kg/cnlG.

Incidentally, the appropriate time for extraction of caffeine in the decaffeination treatment step of the present invention is 2 to 10 hours.

Therefore, the ratio of the amount of the mixed solution to the fresh leaves of the tea plant or its dried material as the raw material should be selected so that the caffeine extraction time is as short as possible within the above range, and a large amount of the mixed solution that would be uneconomical should be avoided. Should.

Further, in the decaffeination treatment step of the present invention, it is desirable to circulate the mixed solution.

Therefore, the flow rate of the mixed solution, and therefore the degree of circulation flow rate of the mixed solution, depends on other selection factors regarding the decaffeination treatment method of the present invention, such as the types of first and second components, operating temperature, operating pressure, and treatment. It depends on the type of tea plant to be used and the desired caffeine extraction time within the range of 2 to 10 hours.

Therefore, for example, in the decaffeination treatment method according to a preferred embodiment of the present invention, the amount of the mixed solution per 1 g of dried raw material tea leaves is 50 to 1.000 g for carbon dioxide gas as the first component. Preferably 100-5
00g, and for the second component ethanol, 0
．． 5 to 50 relatives, preferably 2 to 10d.

Furthermore, the extracted caffeine can be separated by known separation methods, such as adsorption separation of caffeine from the circulating solution using an adsorbent or separation of caffeine from the 1# ring solution by pressure- and/or temperature changes. can be separated from the circulating solution by a method.

Next, the process of extracting the active ingredients of the deodorant of the present invention using a solvent will be explained.

The raw material supplied to this extraction step is an extracted residue obtained by selectively extracting and removing caffeine from the raw tea leaves described above using a supercritical fluid in the presence of water as described above.

The solvent used to extract the active ingredient as a deodorant is:
For example, monoalcoholic organic solvents such as methanol, ethanol, propatool, and isopropanol, polyhydric alcoholic organic solvents such as glycerin and propylene glycol, ketone organic solvents such as acetone, methyl ethyl ketone, cyclohexanone, and isobutylethyl ketone, and water. and mixed solvents thereof, among which ethanol, isopropanol, and cyclohexanone are particularly preferred because they have a high extraction rate of the active ingredient and have a large deodorizing effect of the active ingredient.

Further, in the case of the present invention, it is preferable that the solvent used for extracting the active ingredient as a deodorant is the same as the second component used in the decaffeination treatment step of the present invention, and therefore,
In a preferred embodiment of the present invention, ethanol is particularly suitable.

Extraction of the active ingredient as a deodorant is carried out by cold extraction or thermal extraction using the above-mentioned solvent, but thermal extraction is more preferable. As the extraction method, a standing method, a stirring method, a Soxhlet extraction method, etc. can be applied, but when using thermal extraction, it is necessary to extract sufficiently when hot.

When extracting the active ingredient as a deodorant from the extraction residue, which is the raw material in the extraction process of the present invention, for example, in the case of thermal extraction, the solvent is about 4 to 4 parts by weight per 1 part by weight of the extraction residue. 10 parts by weight, preferably about 4-6
This is done by adding parts by weight and heating to the reflux temperature of the solvent under normal pressure. The extraction time varies depending on the extraction method, type of extraction device, raw materials, etc., but for example, in the case of thermal extraction using a Soxhlet type device, it is approximately 10 to 2 hours.
It is desirable that the time be about 0 hours.

In this way, the active ingredient as a deodorant in the extracted pickle is transferred into the solvent and extracted, so the extraction residue with this solvent is removed by filtration or centrifugation. An extract containing active ingredients as a deodorant is obtained. Therefore, by completely or partially removing the solvent from this extract by distillation or other methods, a dark green to greenish brown powder or solid (hereinafter referred to as deodorizing powder) or its solvent diluted solution (hereinafter referred to as The active ingredients for deodorants are obtained as deodorizing stock solutions.

Note that, as described above, the deodorizing stock solution and deodorant powder are strongly colored and have poor solubility in water, so their use may be restricted depending on the object to be deodorized.

In such a case, the extract containing the active ingredient as a deodorant can be treated with activated carbon, acid clay, diatom top, etc. by the method disclosed in Japanese Patent Application Laid-Open No. 60-122566. After decolorization, the extract contains components that cause coloration and chlorophyll, which is considered to be a water-insoluble component.
By removing the resin and essential oil components, we obtain a deodorant that has good solubility in water, has little coloring, and has a great deodorizing effect against acidic and alkaline malodorous substances such as benzyl mercaptan and trimethylamine. It is also possible.

By the way, as mentioned above, in the manufacturing method of the present invention, first,
Caffeine is selectively extracted and removed from the raw material tea leaves by a decaffeination treatment using a supercritical fluid (a mixed solution of the first component and the second component), and then the extracted residue is used as a deodorizing agent using a solvent. First, the active ingredients are extracted from the raw tea leaves using a solvent as a deodorant, and then this extract is heated with supercritical fluid (the first and second ingredients). There is also a method of subjecting it to decaffeination treatment using a mixed solution of two components.

In this case, the degree of removal of the solvent from the extract is such that the solvent used to extract the active ingredient as a deodorant is the second component used in the subsequent decaffeination treatment, i.e.
When the solvent is at least one alcoholic organic solvent selected from lower aliphatic saturated monohydric alcohols having 1 to 4 carbon atoms, the content of the solvent in the extract to be subjected to the decaffeination treatment is as follows: It is desirable to limit the amount of the second component to the amount required in the decaffeination process, and the solvent used to extract the active ingredient as a deodorizer is not used in the subsequent decaffeination process. If the solvent is other than the second component, it is desirable to remove it completely.

However, first, the active ingredient as a deodorant is extracted from the raw material tea leaves using a solvent, and then this extract is converted into a supercritical fluid (a mixed solution of the first component and the second component).
In the method of subjecting the extract to decaffeination treatment, it is necessary to carry out the decaffeination treatment in the presence of water, which causes the extract to become lumpy due to the water, and does not allow sufficient contact with the supercritical fluid. However, there is a problem that the decaffeinization treatment cannot be carried out sufficiently, and it cannot be said to be a preferable method.

Here, when using the extract obtained above that does not substantially contain caffeine and contains an active deodorizing ingredient as a deodorant, it is necessary to use an appropriate dosage form depending on the purpose of deodorizing or deodorizing. can be adopted.

For example, (A) When using a deodorant stock solution, (a) dilute it to an appropriate concentration with lower alcohol, hydrous lower alcohol, polyhydric alcohol, hydrous polyhydric alcohol, etc., and use the obtained deodorizer liquid. Spray in areas where bad odors occur.

(b) Add directly to food-related products and mix well.

(C) Directly added to cosmetics.

(d) Used as a deodorizing ingredient in deodorizers and deodorizers.

(e) When deodorizing the malodor of pharmaceuticals, etc., form the powder into granules or tablets using a conventional method and package or seal separately in a storage container.

(B) When using a deodorant powder, (a) For refrigerators and moisture absorbents, it is molded into an appropriate shape and used alone or as part of coconut shell activated carbon.

(3) Directly added to sanitary products, shoe pads, and air conditioning products.

(C) Add directly to the factory waste liquid treatment tank.

(d) It is blended as a component of a smoker used in smoking.

Possible uses include, but use in food-related fields is particularly preferred.

The deodorant thus obtained has no difference in composition and physical properties from those obtained by conventionally known methods, except that its caffeine content is 1% by weight or less, and , the deodorizing effect is also conventionally known.
It shows the same or better effect than deodorants.

[Examples and comparative examples]

Hereinafter, the present invention will be explained in more detail with reference to Examples and Comparative Examples.

Example 1 (Manufacture of a deodorizing stock solution that does not contain caffeine) 10 g of dried green tea (sample) was charged into the inner cylinder of an extractor having an inner cylinder with a mesh-like bottom. Note that glass wool was packed above and below the sample to prevent the sample from blowing away. Furthermore, add 15% distilled water to the bottom of the extractor.
I prepared g. Therefore, liquid carbon dioxide (COz) was
The CO□ cylinder is guided to the heat exchanger at a supply rate of 36 d/h, and after being completely liquefied by the refrigerant, it is supplied to the extractor with the CO□ pump, the extractor is pressurized, and extracted using the extractor heater. Raise the temperature of the vessel to bring the inside of the extractor to a supercritical state (temperature: 50°C, 1 pressure crab, 300kg/cnlG)
And so. Note that the pressure inside the extractor was kept constant by a pressure regulating valve provided in the conduit from the extractor to the first separator on the downstream side. As a result, the supplied CO□ was moistened with water at the bottom of the extractor, and furthermore, while passing through the filled part of the dried green tea sample, the green tea was moistened and caffeine was selectively extracted.

Ethanol as the second component was premixed with liquid CO2 by a feed pump at a feed rate of 15 ml/h prior to introduction into the extractor. Supercritical COz containing caffeine, water, and ethanol is extracted from the upper part of the extractor, and is converted into gas by a pressure regulating valve installed in the conduit from the first separator to the next second separator. The pressure was reduced to the same temperature as the extractor and the pressure was 50 kg/aac. Here, gaseous CO□
and an ethanol solution containing caffeine. Then, the gaseous CO , blown into the atmosphere. The above operation was carried out for 5 hours.

Next, the green tea extraction residue in the extractor was taken out and charged into the extraction tube of a Soxhlet extractor. Furthermore, add ethanol 70 years old to the bottom flask of the Soxhlet extractor.
Extraction was carried out under heating under reflux for 10 hours. After removing the green tea residue from the obtained extract using a filter paper, the filtrate was placed under reduced pressure! ! A portion of the ethanol was distilled off to obtain 11 g of a dark green to dark brown viscous liquid concentrate (solid content: about 25% by weight).

Example 2 (Manufacture of deodorizing powder that does not contain caffeine) The procedure of Example 1 was repeated, except that the green tea residue was removed by filter paper from the heated reflux extract using a Soxhlet extractor, and the filtrate was concentrated to dryness under reduced pressure. processed in the same way. As a result, 2.7 g of a dark green solid was obtained.

Example 3 (Manufacture of a solvent diluted solution of a deodorant that does not contain caffeine) 1.0 g of the deodorant powder obtained in Example 2 was mixed with 2 parts of aqueous ethanol.
Dissolve in 3m to make deodorant solvent diluted solution (concentration 5% by weight)
20g was obtained.

Experimental Example 1 (Caffeine removal effect test of the deodorant of the present invention) The caffeine content of the deodorizing stock solution and deodorant powder obtained in Examples 1 and 2 was measured.

In measuring the caffeine content, first, the caffeine content was determined by quantitative analysis using liquid chromatography as follows.

That is, a sample solution containing a known amount of caffeine is prepared in advance, this sample solution is applied to a liquid chromatograph, a chromatogram is drawn, the peak area is determined, and this peak area and the caffeine contained in the sample solution are calculated. A calibration curve was prepared from the amounts of A chromatogram was drawn on a graph, the peak area was determined, and the amount of caffeine in each sample solution was determined from the calibration curve.

Then, the obtained amount A (g) of caffeine and the deodorizing stock solution or deodorant powder in the sample solutions prepared respectively for the deodorizing stock solution and deodorant powder obtained in Examples 1 and 2 above. From the amount B (g) of the agent, the caffeine content C (% by weight) was determined by the following formula.

C-(A/B) It was measured.

(A) Sample preparation Benzyl mercaptan (reagent) and trimethylamine (reagent; 1 gg/μ2 ethanol solution) as malodorous components
were prepared, and 5% by weight ethanol solutions of the concentrated liquid obtained in Example 1 and the solid obtained in Example 2 were prepared as deodorants, respectively.

(B) Test method (a) Analysis of benzyl mercaptan Two 15/d gas chromatography vials were prepared, and a sample (a 5% by weight ethanol solution of the concentrated liquid obtained in Example 1) and a sample were placed in each gas chromatography vial. Accurately weigh 1 g of the sample (5% by weight ethanol solution of the solid obtained in Example 2), seal it tightly, and add benzyl mercaptan (reagent) using a syringe.
Inject 50μ2 into each gas chromatography vial,
Mix well. After that, the air in the gas chromatograph vial was sampled using a syringe, and the air was collected using a gas chromatograph [■Hitachi new product 2 instrument name; ) IITAcHI 1
63 FID), a chromatogram was drawn, and the peak area was determined.

Separately, a blank test with the same operation (in case the above sample is not added)
and find the peak area of the obtained chromatogram,
It was left blank.

(b)) Analysis of Limethylamine Two gas chromatography vials prepared in 15d were prepared, and a sample (5% by weight ethanol solution of the concentrated liquid obtained in Example 1) and a sample (Example 2) were placed in each gas chromatography vial.
After accurately weighing 1 g of 5% by weight ethanol solution of the solid obtained in step 1 and sealing it tightly, add 50 μl of trimethylamine (reagent: 1 gg/μl ethanol solution) to each gas chromatography vial using a syringe. Infuse and mix well.

Thereafter, the air in each of the gas chromatography vials was sampled using a syringe and subjected to a gas chromatograph (manufactured by Hitachi, Ltd., equipment name: HITACHI 163 FID) to draw a chromatogram and determine the peak area.

Separately, a blank test with the same operation (in case the above sample is not added)
and find the peak area of the obtained chromatogram,
It was left blank.

(C) Test Results The deodorizing rates of the deodorizing stock solutions and deodorant powders obtained in Examples 1 and 2 were determined using the following formulas, and the results are shown in Table 2.

Deodorization rate (%) = [(area of blank - area of sample for measuring deodorizing effect)/(area of blank)) X100 The main measurement conditions of the gas chromatograph are as follows.

Benzyl mercaptan> Carrier: 5ILICONE DC-710UNIPOR
TB60~80 mesh Column: Glass column 3Φ×2m Column temperature: 150°C <Ethanol solution of trimethylamine> Support: Dig
lycerol (152) +TEP (15χ) +
KOH (2:) Chromosorb WAW
D M CS60~80 mesh Column: Glass column 3MΦX2m Column temperature: 50°C Comparative example 1 (conventional deodorizing/deodorizing effect test) (A) Deodorizing powder containing caffeine (conventional product) ) Dried green tea (sample) in the extraction tube of the Soxhlet extractor
10 g was charged, and 70 d of ethanol was added to the bottom flask and extracted under heating under reflux for 10 hours. The green tea residue was removed from the obtained extract using a filter paper, and the filtrate was concentrated to dryness under reduced pressure to completely remove ethanol and obtain 3.0 g of a dark green solid. The caffeine content in the obtained solid was determined by the method described in Experimental Example 1 above and was found to be 7.6% by weight.

(B) Deodorizing effect test of deodorizing powder containing caffeine (conventional product) Benzyl mercaptan (reagent) and trimethylamine (reagent; 1μg/μ2 ethanol solution) as malodor components
A 5% by weight ethanol solution of the solid material produced in (A) above was prepared, and the deodorizing effect was measured in the same manner as in Experimental Example 2 above.

The deodorization rate is 90.4 for benzyl mercaptan.
% and for trimethylamine it was 94.6%.

Comparing the results in Table 1 and Comparative Example 1, the caffeine content is 0.4% by weight in Table 1 and 7.6% by weight in Comparative Example 1. The odor concentrate or deodorant powder has approximately 95% less caffeine than conventional products.
%, indicating that the method of the present invention makes it possible to obtain a deodorant substantially free of caffeine. Furthermore, when comparing the results in Table 2 with Comparative Example 1, the deodorizing rate of the deodorizing stock solution or deodorant powder of the present invention is 92.2 to 93.8% for benzyl mercaptan;
And for trimethylamine, 95.6 to 96
．． 2%, whereas the conventional product has 90.4% benzyl mercaptan and 94.6% trimethylamine, and the deodorizing effect of the present invention is also equivalent to the conventional product. It was found that the above effects were exhibited.

[Explanation of effects]

Contains caffeine, which has a stimulant effect on the central nervous system, heart, kidneys, etc., and when added to foods, such as mouth fresheners such as chewing gum and candy, and breath odor removal sweets, etc., it may cause health problems. Compared to conventionally known deodorizers and deodorizers, which had the problem of lack of safety,
By combining the selective extraction and removal method of caffeine with a supercritical fluid and the extraction method of the active ingredient as a deodorant with a solvent, it is virtually caffeine-free and has a better deodorization rate than conventional products. This is effective in obtaining a deodorant that is safe for health.

Patent applicant: Ube Industries Co., Ltd.

Claims (2)

[Claims] (1) A tea leaf component-containing deodorizer that contains 5 to 20% by weight of tannin as the main deodorizing active ingredient, has a deodorizing rate of at least 80% or more, and has a caffeine content of 1% by weight or less. agent. (2) (A) A fluid obtained by bringing tea leaves into a supercritical state from gas in the presence of water (first component) and at least one selected from lower aliphatic saturated monohydric alcohols having 1 to 4 carbon atoms. A step of selectively extracting and removing caffeine from the tea leaves by bringing them into contact with a mixed solution with one type of alcoholic organic solvent (second component) under a supercritical state; (B) a step of selectively extracting and removing caffeine from the tea leaves obtained in step (A); extracting the extracted extraction residue using a solvent, filtering off the raw material residue from the obtained extraction solution, and concentrating or concentrating the filtrate to dryness to obtain a deodorizing stock solution or deodorant powder; A method for producing a deodorant containing tea leaf ingredients, characterized by: