JP2012147984A - Deodorant, method of manufacturing the deodorant, and deodorant product containing the deodorant - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a deodorant which is excellent in deodorizing performance against an offensive odor such as ammonia, acetic acid, etc., method of manufacturing the deodorant, and a deodorant product containing the deodorant.SOLUTION: By mixing a tea leaf hot water extract obtained by adding hot water to dried tea leaves and performing extraction with sericin solution, a tea leaf hot water extract-sericin composite with excellent deodorizing performance is obtained. In manufacturing the composite, a mixed liquid obtained by the mixing is made acidic pH to generate precipitation, and then generated precipitate is subjected to centrifugal separation. The precipitate can be washed and dried under reduced pressure, or after the mixed liquid obtained by the mixing is cooled and frozen, the freezed mixed liquid is thawed and the generated residue can be dried under reduced pressure.

Description

  The present invention provides a deodorant excellent in deodorizing performance against bad odors such as ammonia and acetic acid, and a method for producing the deodorant. The present invention also relates to a deodorizing product such as a deodorizing spray or a sweat wiping sheet that can exhibit excellent deodorizing performance by containing the deodorant.

Catechins, which are components of green tea, are derived from flavonoids and are constituents of condensed tannins. In general, isolation as catechin is carried out using various solvents and using a high-accuracy preparative column, so that the cost is very high and it is difficult to recover a large amount. Regarding catechin compounds, it has been known so far to have a deodorizing effect on compounds such as ammonia. For example, Patent Document 1 below discloses a deodorant using a catechin compound. The deodorizing effect cannot be said to be sufficient, and improvement of the deodorizing effect is demanded.
In addition, sericin on the outer side of the silk thread has extremely high hydrophilicity and water retention and anti-oxidation property because polar amino acids such as serine, aspartic acid, threonine and glutamic acid account for about 77% of the whole. Taking advantage of these characteristics, for example, Patent Documents 2 and 3 listed below disclose cosmetics containing sericin hydrolyzate and cosmetics containing sericin, respectively. However, sericin has little known about its properties other than its antioxidant and water retention effects, and the development of new applications is desired. Effective use of sericin discharged when scouring silk thread and silk fabric is effective. However, there is a demand from the viewpoint of effective use of waste resources.

JP-A-7-238079 JP 62-036308 A JP-A-11-152207

The present invention solves the above-mentioned problems in the prior art, aims to effectively utilize sericin resources, and is a novel deodorant with improved deodorizing effect of catechin compounds, tea leaf hot water extract-sericin composite The challenge is to provide a body.
Another object of the present invention is to provide a method for efficiently producing the above composite and a deodorant product containing the composite.

  The deodorant of the present invention is a tea leaf hot water extract-sericin complex obtained by mixing a tea leaf hot water extract obtained by adding hot water to a dry tea leaf and performing extraction, and a sericin solution. It is characterized by being.

In addition, the method for producing a tea leaf hot water extract-sericin complex of the present invention comprises mixing a tea leaf hot water extract obtained by adding hot water to a dry tea leaf and performing extraction, and then mixing the sericin solution. Precipitation is caused under pH, and the resulting precipitate is separated by centrifugation, washed with water, and then dried under reduced pressure.
Also, the method for producing a tea leaf hot water extract-sericin complex of the present invention comprises mixing a tea leaf hot water extract obtained by adding hot water to a dried tea leaf and performing extraction, and cooling the mixture. It is also characterized in that the residue obtained by freezing and then thawing is dried under reduced pressure.

Further, the deodorant product of the present invention is a tea leaf hot water extract obtained by mixing a tea leaf hot water extract obtained by adding hot water to a dry tea leaf and performing extraction, and a sericin solution- It is characterized by containing a sericin complex.
The present invention is also characterized in that the deodorant product has a form selected from a deodorant spray liquid, a sweat wipe sheet, a diaper and a napkin.

  The deodorizer of the present invention is excellent in deodorizing performance against bad odors such as ammonia and acetic acid, and can be used for various deodorizing products such as a deodorizing spray and a sweat wiping sheet. In addition, the deodorant of the present invention has an advantage that it can be efficiently produced from miscellaneous tea leaves discharged from a tea factory and discarded and sericin discharged during silk scouring.

It is a chromatogram about tea leaf hot-water extract-sericin complex solution. It is a chromatogram about a tea leaf hot-water extract. It is a chromatogram about a sericin solution. It is a chromatogram of a solution obtained by adding a water / acetone extract to a solution of tea leaf hot water extract-sericin complex. It is a graph which shows the result of the deodorizing performance test with respect to ammonia in Example 4. It is a graph which shows the result of the deodorizing performance test with respect to acetic acid in Example 4.

First, the tea leaf hot water extract-sericin complex which is the deodorizer of the present invention and the production method thereof will be described.
The tea leaf hot water extract-sericin complex, which is the deodorant of the present invention, is obtained by mixing a tea leaf hot water extract from which catechins are extracted by adding hot water to dry tea leaves, and a sericin solution, In such a method of mixing two liquids, catechins can be combined with sericin (protein) without using a high-precision preparative column or separation solvent that has been used for isolation of catechins until now. Utilizing the property of binding, it can be recovered in a complex state, and it is relatively easy to recover a large amount at a low cost.
The tea leaf hot water extract-sericin complex of the present invention has a characteristic that the deodorizing function of catechins is further enhanced by complexing with sericin, and in particular, a component that is a source of sweat and body odor ( Good deodorizing effect on ammonia, acetic acid, isovaleric acid, etc.)
Examples of tea leaves that can be used to produce the tea leaf hot water extract-sericin complex of the present invention include Yabukita, Okumidori, Ujimidori and the like.

Methods for producing the tea leaf hot water extract-sericin complex of the present invention include a method by centrifugation (centrifugation method) and a method by freezing (freezing method). In the following description, “%” for concentration and blending ratio means “% by weight”.
In the centrifugal separation method for producing the tea leaf hot water extract-sericin complex of the present invention, preferably, 100 parts by weight of hot water heated to 95 ° C. or more is added to 1 part by weight of dry tea leaves. Extraction is performed for -3 hours, preferably 2 hours, and this extract is suction filtered to remove tea leaves and the like to obtain a tea leaf hot water extract. When green tea is used as the dried tea leaves, the tea leaf hot water extract obtained by extraction contains about 10 to 15% catechins, and the main ones are epicatechin and epigallo. Catechin, epicatechin gallate, and epigallocatechin gallate. Among green tea catechins, the content of epigallocatechin gallate is particularly large, accounting for about 50 to 60% of catechins.
Then, a sericin solution in which sericin is dissolved is added to and mixed with the tea leaf hot water extract, and then an acid solution such as hydrochloric acid is added to make the pH acidic (preferably pH 4 to 5). -Causing precipitation of the sericin complex. In the present invention, when the tea leaf hot water extract and the sericin solution are added and mixed, it is preferable to keep the tea leaf hot water extract at a temperature of 45 ° C. ± 5 ° C. in advance. It is preferable to mix approximately the same amount with the solution, and the concentration of the sericin solution added and mixed is preferably about 1 to 2%. An example of the solvent for the sericin solution is water.
Then, the tea leaf hot water extract-sericin complex precipitated at the above acidic pH is taken out of the liquid using a centrifuge, and the precipitate separated by centrifugation is washed with water, and then a vacuum dryer. To obtain a tea leaf hot water extract-sericin complex of the present invention.

  Further, in the freezing method for producing the tea leaf hot water extract-sericin complex of the present invention, the tea leaf hot water extract and the sericin solution are mixed and mixed in the same manner as in the case of the above centrifugation method. The solution is cooled and frozen at a temperature of about −20 ° C. Then, the once frozen mixture is heated and thawed, and the resulting residue is dried under reduced pressure using a vacuum dryer to obtain the tea leaf hot water extract-sericin complex of the present invention. When the freezing method and the centrifugation method are compared, the freezing method can obtain a complex with a high yield, and is suitable for producing a large amount of the complex with a small number of work steps. ing.

Further, the deodorant product of the present invention was obtained by impregnating a base material such as paper or nonwoven fabric with an aqueous solution of tea leaf hot water extract-sericin complex obtained by the above method or an organic solution such as alcohol or glycol. Specific products that require deodorizing properties include sweat wipe sheets, paper napkins, and diapers. Moreover, it can be used also as a deodorizing spray product by accommodating said solution (deodorizing liquid) in a spray dispenser.
EXAMPLES Hereinafter, although an Example of this invention is shown and this invention is demonstrated, this invention is not limited to what was described in the Example.

Example 1: Example of production of tea leaf hot water extract-sericin complex (centrifugation method)
To 10 g of dried tea leaves, 1 L of purified water heated to 95 ° C. or higher in advance was added and extracted for 120 minutes. The resulting liquid was suction filtered to remove tea leaves and the like, and a clear tea leaf hot water extract was obtained. . An equal amount (500 mL) of 1.4% sericin solution (solvent: water) was added to the tea leaf hot water extract (500 mL) kept at 45 ° C. ± 5 ° C. and stirred for 1 hour, and then an appropriate amount of hydrochloric acid was added to adjust the pH to 4 When adjusted to .5, a tea leaf hot water extract-sericin protein complex precipitate was obtained. This precipitate is separated by a centrifuge (8000 rpm, 10 minutes, room temperature), the precipitate is washed twice with purified water, and the obtained precipitate is dried at 45 ° C. for 32 hours in a vacuum dryer, The tea leaf hot water extract-sericin complex was obtained.
The yield of the complex obtained by the above method is 3.37 g, and when the hot water extract solid content ratio in 10 g of dried tea leaves is 15%, the tea leaf hot water extract solid content 0.75 g + sericin From the solid content of 7 g, the yield of the composite was calculated to be 3.37 / (0.75 + 7) × 100 = 43.4%.

Example 2: Example of production of tea leaf hot water extract-sericin complex (freezing method)
To 10 g of dried tea leaves, 1 L of purified water heated to 95 ° C. or higher in advance was added and extracted for 120 minutes. The resulting liquid was suction filtered to remove tea leaves and the like, and a clear tea leaf hot water extract was obtained. . After adding an equal amount (500 mL) of a 1.4% sericin solution (solvent: water) to the above-mentioned tea leaf hot water extract (500 mL) kept at 45 ° C. ± 5 ° C. and stirring for 1 hour, this mixture was quickly added. Placed in a freezer (−20 ° C.) and frozen overnight. The frozen solution was thawed at 45 ° C. for 6 hours using a dryer, and the resulting residue was dried in a vacuum dryer at 45 ° C. for 32 hours to obtain a white tea leaf hot water extract-sericin. A complex was obtained.
The yield of the complex obtained by the above method is 5.33 g, and the solid content of tea leaf hot water extract 0.75 g + sericin when the ratio of solid content of hot water extract in dry tea leaves 10 g is 15% From the solid content of 7 g, the yield of the composite was calculated to be 5.33 / (0.75 + 7) × 100 = 68.8%.

Example 3: Liquid Chromatographic Analysis of the Tea Leaf Hot Water Extract-Sericin Complex of the Present Invention A solution of the tea leaf hot water extract-sericin complex obtained in Example 1 above dissolved in water, The tea leaf hot water extract and sericin solution used for the production were subjected to component analysis by liquid chromatography under the following conditions.
(Measurement condition)
Flow rate: 0.9 mL / min (A + B liquid flow rate)
Mobile phase: Liquid A: 1.5% phosphoric acid aqueous solution
Liquid B: 1.5% phosphoric acid aqueous solution, 20% acetic acid, 25% methanol aqueous solution
Linear gradient
B concentration 10% (initial) → 10% (5 minutes) → 30% (8 minutes) → 30%
(10 minutes) → 80% (15 minutes) → 80% (20 minutes) → 10% (25 minutes)
Detector used: Shimadzu SPD-M10Avp
Column used: Phenomenex Luna 5μ C18 100A 150 × 4.60mm
Column temperature: 40 ° C
Detection wavelength: 280 nm

The results are shown in FIGS. FIG. 1 is a chromatogram for a solution of tea leaf hot water extract-sericin complex, FIG. 2 is a chromatogram for tea leaf hot water extract, and FIG. 3 is a chromatogram for sericin solution. .
In FIG. 2, catechins such as epicatechin (EC), epigallocatechin (EGC), epicatechin gallate (ECg), epigallocatechin gallate (EGCg) and the like are included in the tea leaf hot water extract. In the chromatogram of FIG. 1, the peak of the complex itself obtained by mixing the tea leaf hot water extract and the sericin solution could not be confirmed, but the mixture consisting of catechins Since no peak of each compound appearing in the above case was observed, it is considered that catechins are bound to the complex.
Then, water / acetone solvent was added to the tea leaf hot water extract-sericin complex solution, and liquid chromatography analysis was performed on components eluted with water / acetone solvent. FIG. 4 is a chromatogram of a solution obtained by adding a water / acetone extract to a solution of tea leaf hot water extract-sericin complex.
From the chromatogram of FIG. 4, it was confirmed that the catechins bound to sericin constituting the complex were separated and eluted by the water / acetone extract. From the chromatograms of FIGS. It was confirmed that the product obtained by mixing the aqueous extract and the sericin solution was not a simple mixture of sericin and catechins, but a complex in which catechins were bound to sericin.

Example 4: Deodorizing performance test Using the tea leaf hot water extract-sericin complex obtained in Example 1 above, the deodorizing performance against ammonia, acetic acid and isovaleric acid was tested.
a) Deodorization performance test for ammonia The deodorization performance of the tea leaf hot water extract-sericin complex of the present invention was examined by a detector tube method using a commercially available ammonia gas detector tube. The test method is as follows.
Sample weight: 1.5g
Test container: 5 liter Tedlar bag Amount of gas in the container: 3 liter Initial gas concentration: 100 ppm
As a comparative product, a similar test was performed using catechins extracted from green tea (a mixture containing epicatechin, epigallocatechin, epicatechin gallate and epigallocatechin gallate). The same operation was performed without adding. Table 1 shows the results of measuring the ammonia concentration immediately after the start of measurement, 1 hour, 2 hours, 3 hours, and 6 hours after the start of each sample. FIG. 5 is a graph of this result.

  As shown in Table 1 and FIG. 5, in the case of a comparative product containing green tea catechins not complexed with sericin, deodorizing performance against ammonia is observed, but the tea leaf hot water extract of the present invention- In the case of the sericin complex, it was confirmed that the deodorizing performance was demonstrated in a shorter time and that the deodorizing capability was excellent (ammonia concentration was lower).

b) Deodorizing performance test for acetic acid The deodorizing performance of the tea leaf hot water extract-sericin complex of the present invention was examined by a detector tube method using a commercially available gas detector tube for acetic acid. The test method was the same as that of ammonia except that the initial gas concentration was 50 ppm. As a control, a similar test was performed using the above green tea catechins, and a blank test without a sample was also performed.
The measurement results of acetic acid concentration by the above test are shown in Table 2. FIG. 6 is a graph of this result.

  As shown in FIG. 6, deodorization performance against acetic acid is also observed in the comparative product containing green tea catechins not complexed with sericin, but the tea leaf hot water extract-sericin complex of the present invention In the case of, it was confirmed that the deodorizing performance was demonstrated in a shorter time and that the deodorizing ability was excellent (the acetic acid concentration was lower).

c) Deodorizing performance test for isovaleric acid With regard to isovaleric acid, the deodorizing performance fiber product certification standard of the Fiber Evaluation Technology Council was applied mutatis mutandis, and the deodorizing performance was tested by gas chromatography. The initial gas concentration was about 38 ppm, and the reduction rate after 2 hours was measured.
As a result, the reduction rate of isovaleric acid after 2 hours in the case of the comparative product was 81.2%, whereas the reduction rate of isovaleric acid after 2 hours in the case of the product of the present invention was 96. It was confirmed that the tea leaf hot water extract-sericin complex obtained by complexing with sericin had an excellent deodorizing performance even with respect to isovaleric acid.

Example 5: Production Example of Deodorant Spray A solution comprising 0.1% tea leaf hot water extract-sericin complex obtained in Example 1 above, 5% ethanol, 0.2% methylparaben, and the remaining water. The liquid mixture (deodorant liquid) obtained by adding and dissolving in was stored in a commercially available spray dispenser to obtain a deodorant spray product.
When the mixed liquid accommodated in the spray dispenser was sprayed and sprayed on clothing, body odor and tobacco or food odor adhering to the clothing could be eliminated.

Example 6: Production Example of Sweat Wiping Sheet The tea leaf hot water extract-sericin complex 0.1% obtained in Example 1 was mixed with 93.3% water, 3% glycerin, 2% cetearyl isononanoate, and palmitic acid. It was obtained by adding and dissolving in a solution comprising 0.5% cetyl acid, 0.5% ceteares-20, 0.2% sodium pyrrolidonecarboxylate, 0.2% methylparaben, 0.2% sodium benzoate When the mixed liquid (deodorant liquid) was impregnated into a 40 g / m ² non-woven fabric and used as a sweat wiping sheet, it was possible to deodorize the sweaty odor of sweaty bodies that were waking up and sticky skin.

  The tea leaf hot water extract-sericin complex of the present invention has excellent deodorizing performance against bad odors such as ammonia and acetic acid. Taking advantage of the deodorizing performance, a deodorizing spray, a sweat wiping sheet, etc. It can be used as a deodorant component in various deodorant products. Also, by using the production method of the present invention, a tea leaf hot water extract-sericin complex is efficiently produced using miscellaneous tea leaves discharged from a tea factory and discarded and sericin discharged during scouring of silk. The production method is also useful from the viewpoint of effective use of waste resources.

Claims (5)

  A tea leaf hot water extract-sericin complex obtained by mixing tea leaf hot water extract obtained by adding hot water to dry tea leaves and extraction and sericin solution. Odorant.   After mixing the hot tea water extract obtained by adding hot water to the dried tea leaves and the sericin solution, precipitation is caused under acidic pH, and the resulting precipitate is separated by centrifugation. A method for producing a tea leaf hot water extract-sericin complex, which is washed with water and then dried under reduced pressure.   Mix the tea leaf hot water extract obtained by adding hot water to the dried tea leaf and extract it, cool and freeze, then defrost and dry the residue obtained A method for producing a tea leaf hot water extract-sericin complex.   It contains tea leaf hot water extract obtained by adding hot water to dry tea leaves and extraction, and tea leaf hot water extract-sericin complex obtained by mixing sericin solution. Deodorant product.   The deodorant product according to claim 4, which has a form selected from a deodorant spray liquid, a sweat wipe sheet, a diaper and a napkin.

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