CN106318626A - Preparation method of perfume with green tea characteristic aroma - Google Patents
Preparation method of perfume with green tea characteristic aroma Download PDFInfo
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- CN106318626A CN106318626A CN201610696472.4A CN201610696472A CN106318626A CN 106318626 A CN106318626 A CN 106318626A CN 201610696472 A CN201610696472 A CN 201610696472A CN 106318626 A CN106318626 A CN 106318626A
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- spice
- alcohol
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
Abstract
The invention relates to a preparation method of perfume with green tea characteristic aroma. The preparation method is characterized by comprising the following steps: extracting repeatedly by using an organic solvent for green tea; merging extracting solutions and concentrating under reduced pressure to obtain concentrate; enabling the obtained concentrate to pass through macroporous resin; flushing with deionized water at first and then eluting with a polar organic solvent; concentrating eluant under reduced pressure to obtain polyamide as a concentrate; flushing with the deionized water at first and then eluting with the polar organic solvent; concentrating eluant under reduced pressure to obtain a concentrate which is the perfume with green tea characteristic aroma. The preparation method is efficient, simple and convenient, and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to the preparation method of a kind of green tea feature perfume (or spice) spice, especially a kind of employing Flavonoids by Macroporous Adsorption Resin adds
Polyamide chromatography method prepares the method for green tea spice, belongs to technical field of plant extraction.
Background technology
Green tea, also known as azymic tea.Green tea is the most fermented tea made, the most more natural goods remaining fresh leaf
Matter, the tea polyphenols contained, catechin, chlorophyll, caffeine, aminoacid, vitamins and other nutritious components are the most more.This in green tea
A little natural nutrition compositions, have special-effect to anti-aging, anti-cancer, anticancer, sterilization, antiinflammatory etc., are less than other teas.
Simultaneously as green tea contains the material compositions such as substantial amounts of alcohols, aldehydes, ketone, carboxylic acids, esters, natural to impart green tea rich
Rich special aroma.
The cross linked polymer that macroporous adsorbent resin is a class without ion-exchange group, stable in physicochemical property, insoluble in acid,
Alkali and organic solvent, have concentration, centrifugation, and do not done by inorganic salts, strong ion and low molecular compound Organic substance
Disturb.Macroporous adsorbent resin can selectively adsorb organic substance by physical absorption such that it is able to reaches isolated and purified purpose.
According to resin surface character, macroporous adsorbent resin can be divided into polarity nonpolar, middle and polarity three class.
Polyamide is the high molecular polymer in a class formation containing recurring unit's amido link (-CO-NH-), amide group
On O, atom N in acid medium, combine proton and positively charged, form the anion in adsorbent solution with electrostatic attraction, therefore
Hydrogen bond can be formed with the compound of the phenolic hydroxy group such as phenols, acids, quinones, flavonoid and be adsorbed, and hydrogen bond can not be formed
Compound separates.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that the preparation side of a kind of green tea feature perfume (or spice) spice
Method, this preparation method is efficient, easy, it is adaptable to large-scale industrial production.
The technical scheme provided according to the present invention, the preparation method of described green tea feature perfume (or spice) spice, comprise the following steps: take
Green tea organic solvent extraction, united extraction liquid concentrating under reduced pressure, the concentrate obtained crosses macroporous adsorptive resins, first spend from
Sub-water rinses and uses polar organic solvent eluting again, and eluent carries out concentrating under reduced pressure, and polyamide chromatography post crossed by the concentrate obtained, first
Use polar organic solvent eluting again with deionized water rinsing, eluent carries out concentrating under reduced pressure, and it is special that the concentrate obtained is green tea
Levy fragrant spice.
In particular it relates to the preparation method of a kind of green tea feature perfume (or spice) spice, comprise the following steps:
A, organic solvent extraction: green tea is extracted 2.0 with alcohol or ketone aqueous solutions of organic solvent under conditions of 40 ~ 60 DEG C with stirring
~ 4.0 hours, repeat to extract 2 ~ 3 times, united extraction liquid, till extracting solution is evaporated to no liquid outflow, obtain concentrate
I；Described green tea is 1:6 ~ 12 with the weight ratio of alcohol or ketone aqueous solutions of organic solvent, the volume hundred of alcohol or ketone aqueous solutions of organic solvent
Mark is 60 ~ 95%；
In the present invention, alcohol or ketone organic solvent are it should be understood that a kind of can extract the organic molten of feature perfume (or spice) spice from green tea
Agent, these organic solvents are a kind of volatile, and its residue also will not produce the organic solvent of adverse consequences to product；
In the present invention, the concentration of described organic solvent is by volume 60 ~ 95%, if this concentration is less than 60%, then can produce
A large amount of water-solubility impurities such as polysaccharide, protein, subsequent purification processes and brings difficulty；If this concentration is more than 95%, then can be lost
Many organic solvents, increase production cost；Therefore, the concentration of described organic solvent is 60 ~ 95% to be appropriate, preferably 65 ~
90%, more preferably 75 ~ 80%；
Described organic solvent is 1:6 ~ 12 with the weight ratio of alcohol or ketone aqueous solutions of organic solvent, if it exceeds this weight ratio model
Enclose, then can dissolve too much impurity, and solvent loss can be increased；
B, absorption with macroporous adsorbent resin: by concentrate I at room temperature by macroporous adsorptive resins, flow velocity is 0.5 ~ 1.5 times of post
Volume/h；Then colourless to eluate with deionized water drip washing；With alcohol eluant, macroporous adsorptive resins is carried out eluting again, receive
Collection eluent, till carrying out eluent being evaporated to no liquid outflow, obtains concentrate II；Described alcohol eluant and macropore
The volume ratio of adsorption resin column is 2 ~ 5, and flow velocity when alcohol eluant carries out eluting is 1 ~ 2 times of column volume/h；
In the present invention, macroporous adsorbent resin is that a class does not contains cation exchange groups and has the preparation of macroporous structure, tool
There are good macroreticular structure and bigger specific surface area, can organic optionally through in physical absorption aqueous solution
Thing.It is widely used in separation and the purification process of Chinese herbal medicine effective ingredients.It is with styrene and acrylate as monomer, with
Divinylbenzene is cross-linking agent, and with toluene, dimethylbenzene as porogen, they polymerizations that are cross-linked with each other define porous skeleton structure.This
Plant resin and by the Van der Waals force between itself and adsorbed molecule and hydrogen bond action, there is adsorptivity, because of its netted knot
Structure and high-specific surface area and there is the ability of selectively adsorbing organic substance, therefore use this resin to be capable of separating with pure
The purpose changed；
C, polyamide are enriched with: by concentrate II at room temperature by polyamide chromatography post, flow velocity is 0.5 ~ 1.5 times of column volume/h；
Then colourless to eluate with deionized water drip washing；Carry out eluting with alcohol eluant again, collect eluent, alcohol eluant and polyamides
The volume ratio of amine chromatographic column is 2 ~ 5, and flow velocity during eluting is 1 ~ 2 times of column volume/h；Then eluent is evaporated to
Till no liquid flows out, obtain green tea spice；
In the present invention, polyamide is the high molecular polymer in a class formation containing recurring unit's amido link (-CO-NH-), acyl
O in amine groups, atom N combine proton and positively charged in acid medium, form the moon in adsorbent solution with electrostatic attraction
Ion, therefore can form hydrogen bond with the compound of the phenolic hydroxy group such as phenols, acids, quinones, flavonoid and be adsorbed, and can not be formed
The compound of hydrogen bond separates.
Further, in described step A, while being concentrated under reduced pressure to give concentrate I, reclaim alcohol or ketone organic solvent；Institute
Stating in step B, eluent reclaims alcohol while carrying out concentrating under reduced pressure；In described step C, while eluent carries out concentrating under reduced pressure
Reclaim alcohol.Described organic solvent needs to reclaim after extraction step completes, and generally uses the technology people of the art
The way of distillation known to Yuan reclaims.
Further, described alcohol or ketone organic solvent are methanol, ethanol or acetone.
Further, described macroporous adsorptive resins use resin be D101, HPD20 or AB-8 macroporous adsorbent resin,
Or other macroporous adsorbent resin that its polarity is suitable with described D101, HPD20, AB-8 macroporous adsorbent resin.They are all current
Extensive product sold on market, the D101 type macroporous adsorbent resin such as produced by Tianjin great poly resin Science and Technology Ltd.,
By the HP20 type macroporous adsorbent resin of Mitsubishi chemical production, by the AB-8 type of Anhui Samsung resin Science and Technology Ltd. production
Macroporous adsorbent resin, other macroporous adsorbent resin of LX-11, D101C type produced by Xi'an Lanxiao Sci-Tech Co., Ltd..
Further, in described step C, the specification of the polyamide that polyamide chromatography post uses is 30-60 mesh, 60-100 mesh
Or 100-120 mesh.They are all extensive product solds in the market, such as raw by the Shanghai speed science equipment company limited that rubs
Produce.
Further, in described step B, ethanol or methanol that alcohol eluant uses percentage by volume to be 15 ~ 90% are water-soluble
Liquid.If the concentration of described alcohol eluant is less than 15%, then eluant polarity is relatively big, and object is difficult to eluting, if described alcohol
When the concentration of eluant is more than 90%, then solvent loss is relatively big, increases production cost, and therefore, the concentration of described alcohol eluant is 15
~ 90 % are rational, preferably 25 ~ 75%, more preferably 50 ~ 65%.
Further, in described step C, ethanol or methanol that alcohol eluant uses percentage by volume to be 15 ~ 90% are water-soluble
Liquid.If the concentration of described alcohol eluant is less than 15%, then eluant polarity is relatively big, and object is difficult to eluting, if described alcohol
When the concentration of eluant is more than 90%, then solvent loss is relatively big, increases production cost, and therefore, the concentration of described alcohol eluant is 15
~ 90 % are rational, preferably 55 ~ 85%, more preferably 65 ~ 80%.
Further, in described step A, B, C, the pressure condition of concentrating under reduced pressure is 0.01 ~ 0.08MPa.During concentrating under reduced pressure
The equipment used is normally used equipment in current processing technique of Chinese herbs field, such as rotary evaporator, vacuum-concentrcted
Device.
Green tea feature perfume (or spice) spice tea Flavor prepared by the present invention is strong, and without obvious bitter taste.
Owing to selecting macroporous adsorbent resin and polyamide, it is good to the adsorptive selectivity of fragrance matter, and absorption is fast, desorbing
Also fast, adsorption capacity is bigger；Physical and chemical stability is high, and mechanical strength is good, and regeneration is easily；Operating the easiest, step is few, becomes
This is cheap, and solvent all recoverables are also applied for large-scale industrial production.
Detailed description of the invention
The macroporous adsorbent resin that the present invention uses needs to carry out following pretreatment before use:
95% soak with ethanol 24h, is washed till effluent with 95% ethanol the most muddy with water 1:5, washes with water to without alcohol taste；Use 5%HCl again
By resin column, soak 2 ~ 4h, be washed to neutrality；Again with 2%NaOH by resin column, soak 2 ~ 4h, be washed to neutrality, standby.
Then, the concentrated solution allowing step A obtain passes through macropore under conditions of 0.5 ~ 1.5 times of column volume/h of flow velocity with room temperature
Adsorption resin column, reaches to adsorb completely.
Described macroporous adsorptive resins is first colourless to eluate with deionized water drip washing after absorption, so can be more
Clean fully, up hill and dale by big polar impurities of water solublity such as the saccharide of macroporous adsorptive resins absorption, mucus juice and remove, then,
Use alcohol eluent again.
The macroporous adsorbent resin that the present invention uses needs to carry out following pretreatment before use:
95% soak with ethanol 24h, with 95% ethanol be washed till effluent transparent and after being evaporated without residue (or few residue), wash with water
To without alcohol taste；Again with 2-2.5 times of volume 5%NaOH aqueous solution, the distilled water of 1 times of volume, 2-2.5 times of volume 10% aqueous acetic acid
Eluting, is finally eluted to neutrality with distilled water, standby.
Then, the concentrated solution allowing step B obtain passes through polyamides under conditions of 0.5 ~ 1.5 times of column volume/h of flow velocity with room temperature
Amine chromatographic column, reaches to adsorb completely.
Described polyamide chromatography post is first colourless to eluate with deionized water drip washing after absorption, so can more fill
Divide, up hill and dale impurity big for the very small amount polarity of polyamide chromatography post absorption cleaned removing, then, then wash with alcohol eluant
De-.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1: the preparation method of green tea feature perfume (or spice) spice, implements step as follows:
A, organic solvent extraction:
By green tea and alcohol or weight ratio 1:10 of ketone aqueous solution, described green tea uses concentration temperature 53 DEG C under conditions of stirring
65% ethanol water extracts 3 hours by volume, then repeats in the same fashion to extract 2 times, and extracting solution merges, be then used by by
The rotary evaporator that Shanghai Yarong Biochemical Instrument Plant produces carries out concentrating under reduced pressure, to no liquid under conditions of pressure 0.08MPa
Till outflow, obtain concentrate I, reclaim organic solvent simultaneously；
B, absorption with macroporous adsorbent resin:
The concentrate I allowing step A obtain passes through by Tianjin great poly resin section under conditions of 1.0 times of column volume/h of flow velocity with room temperature
The D101 type macroporous adsorptive resins that skill company limited produces, then colourless to eluate, according still further to alcohol with deionized water drip washing
Eluant is 4 with the volume ratio of macroporous adsorptive resins, is that 1.5 times of column volumes/h concentration is for 85% second by volume with flow
Alcohol-water solution eluant row eluting, collects eluent, is then used by the rotary evaporator produced by Shanghai Yarong Biochemical Instrument Plant
Concentrating under reduced pressure under conditions of pressure 0.08MPa, flowing out to no liquid, obtains concentrate II, reclaims alcohol simultaneously；
C, polyamide are enriched with:
Allow concentrate II that step B obtains by being rubbed fast science by Shanghai under conditions of 1.2 times of column volume/h of flow velocity with room temperature
Polyamide (model the is 30-60) chromatographic column that equipment company limited produces, then colourless to eluate with deionized water drip washing, then
It is 3 according to the volume ratio of alcohol eluant Yu polyamide chromatography post, is that 1.2 times of column volumes/h concentration is for by volume with flow
75% ethanol water eluting agent row eluting, collects eluent, and the rotation being then used by being produced by Shanghai Yarong Biochemical Instrument Plant is steamed
Send out device concentrating under reduced pressure under conditions of pressure 0.08MPa, flowing out to no liquid, obtain green tea spice, reclaim alcohol simultaneously；
Being detected by the green tea spice obtained, the refractive power of tea flavour is 1.4690, and density is 1.2000, and acid number is 10.2.
Embodiment 2: the preparation method of green tea feature perfume (or spice) spice, implements step as follows:
A, organic solvent extraction:
By green tea and alcohol or weight ratio 1:8 of ketone aqueous solution, described green tea uses concentration temperature 48 DEG C under conditions of stirring
78% ethanol water extracts 2.5 hours by volume, then repeats in the same fashion to extract 2 times, and extracting solution merges, and is then used by
The rotary evaporator produced by Shanghai Yarong Biochemical Instrument Plant carries out concentrating under reduced pressure under conditions of pressure 0.08MPa, to aneroid
Till body flows out, obtain concentrate I, reclaim organic solvent simultaneously；
B, absorption with macroporous adsorbent resin:
The concentrate I allowing step A obtain passes through by Anhui Samsung terebinthaceae under conditions of 1.5 times of column volume/h of flow velocity with room temperature
The AB-8 type macroporous adsorptive resins that skill company limited produces, then colourless to eluate, according still further to alcohol with deionized water drip washing
Eluant is 3 with the volume ratio of macroporous adsorptive resins, is that 2 times of column volumes/h concentration is for 75% ethanol by volume with flow
Aqueous solution eluant row eluting, collects eluent, and the rotary evaporator being then used by being produced by Shanghai Yarong Biochemical Instrument Plant exists
Concentrating under reduced pressure under conditions of pressure 0.08MPa, flowing out to no liquid, obtains concentrate II, reclaims alcohol simultaneously；
C, polyamide are enriched with:
Allow concentrate II that step B obtains by being rubbed fast science by Shanghai under conditions of 0.8 times of column volume/h of flow velocity with room temperature
Polyamide (model the is 60-100) chromatographic column that equipment company limited produces, then colourless to eluate with deionized water drip washing,
Volume ratio according still further to alcohol eluant Yu polyamide chromatography post is 3.5, is that 2.0 times of column volumes/h concentration is for volume with flow
Count 85% ethanol water eluting agent row eluting, collect eluent, be then used by the rotation produced by Shanghai Yarong Biochemical Instrument Plant
Vaporizer is concentrating under reduced pressure under conditions of pressure 0.08MPa, flowing out to no liquid, obtains green tea spice, reclaims alcohol simultaneously；
Being detected by the green tea spice obtained, the refractive power of tea flavour is 1.4580, and density is 1.1800, and acid number is 10.6.
Embodiment 3: the preparation method of green tea feature perfume (or spice) spice, implements step as follows:
A, organic solvent extraction:
By green tea and alcohol or weight ratio 1:12 of ketone aqueous solution, described green tea uses concentration temperature 58 DEG C under conditions of stirring
83% ethanol water extracts 3.5 hours by volume, then repeats in the same fashion to extract 2 times, and extracting solution merges, and is then used by
The rotary evaporator produced by Shanghai Yarong Biochemical Instrument Plant carries out concentrating under reduced pressure under conditions of pressure 0.08MPa, to aneroid
Till body flows out, obtain concentrate I, reclaim organic solvent simultaneously；
B, absorption with macroporous adsorbent resin:
Allow concentrate I that step A obtains by being given birth to by Mitsubishi chemistry under conditions of 1.2 times of column volume/h of flow velocity with room temperature
The HP20 type macroporous adsorptive resins produced, then colourless to eluate, according still further to alcohol eluant and macropore with deionized water drip washing
The volume ratio of adsorption resin column is 3.5, is that 1.2 times of column volumes/h concentration is for 68% ethanol aqueous wash by volume with flow
De-agent row eluting, collects eluent, and the rotary evaporator being then used by being produced by Shanghai Yarong Biochemical Instrument Plant is at pressure
Concentrating under reduced pressure under conditions of 0.08MPa, flowing out to no liquid, obtains concentrate II, reclaims alcohol simultaneously；
C, polyamide are enriched with:
Allow concentrate II that step B obtains by being rubbed fast science by Shanghai under conditions of 1.5 times of column volume/h of flow velocity with room temperature
Polyamide (model the is 100-120) chromatographic column that equipment company limited produces, then colourless to eluate with deionized water drip washing,
Volume ratio according still further to alcohol eluant Yu polyamide chromatography post is 2.0, is that 1.8 times of column volumes/h concentration is for volume with flow
Count 60% ethanol water eluting agent row eluting, collect eluent, be then used by the rotation produced by Shanghai Yarong Biochemical Instrument Plant
Vaporizer is concentrating under reduced pressure under conditions of pressure 0.08MPa, flowing out to no liquid, obtains green tea spice, reclaims alcohol simultaneously；
Being detected by the green tea spice obtained, the refractive power of tea flavour is 1.4490, and density is 1.1600, and acid number is 9.5.
Claims (9)
1. a preparation method for green tea feature perfume (or spice) spice, is characterized in that, comprise the following steps:
A, organic solvent extraction: green tea is extracted 2.0 with alcohol or ketone aqueous solutions of organic solvent under conditions of 40 ~ 60 DEG C with stirring
~ 4.0 hours, repeat to extract 2 ~ 3 times, united extraction liquid, till extracting solution is evaporated to no liquid outflow, obtain concentrate
I；Described green tea is 1:6 ~ 12 with the weight ratio of alcohol or ketone aqueous solutions of organic solvent, the volume hundred of alcohol or ketone aqueous solutions of organic solvent
Mark is 60 ~ 95%；
B, absorption with macroporous adsorbent resin: by concentrate I at room temperature by macroporous adsorptive resins, flow velocity is 0.5 ~ 1.5 times of post
Volume/h；Then colourless to eluate with deionized water drip washing；With alcohol eluant, macroporous adsorptive resins is carried out eluting again, receive
Collection eluent, till carrying out eluent being evaporated to no liquid outflow, obtains concentrate II；Described alcohol eluant and macropore
The volume ratio of adsorption resin column is 2 ~ 5, and flow velocity when alcohol eluant carries out eluting is 1 ~ 2 times of column volume/h；
C, polyamide are enriched with: by concentrate II at room temperature by polyamide chromatography post, flow velocity is 0.5 ~ 1.5 times of column volume/h；
Then colourless to eluate with deionized water drip washing；Carry out eluting with alcohol eluant again, collect eluent, alcohol eluant and polyamides
The volume ratio of amine chromatographic column is 2 ~ 5, and flow velocity during eluting is 1 ~ 2 times of column volume/h；Then eluent is evaporated to
Till no liquid flows out, obtain green tea spice.
2. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: in described step A, dense in decompression
Contracting reclaims alcohol or ketone organic solvent while obtaining concentrate I；In described step B, eluent returns while carrying out concentrating under reduced pressure
Receive alcohol；In described step C, eluent reclaims alcohol while carrying out concentrating under reduced pressure.
3. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: in described step A, alcohol or ketone have
The percentage by volume of machine solvent aqueous solution is 65 ~ 90%.
4. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: in described step A, alcohol or ketone have
The percentage by volume of machine solvent aqueous solution is 75 ~ 80%.
5. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: described alcohol or ketone organic solvent
For methanol, ethanol or acetone.
6. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: described macroporous adsorptive resins is adopted
Resin be D101, HPD20 or AB-8 macroporous adsorbent resin.
7. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: aramid layer in described step C
The specification of the polyamide that analysis post uses is 30-60 mesh, 60-100 mesh or 100-120 mesh.
8. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: in described step B and step C,
Ethanol or the methanol aqueous solution that alcohol eluant uses percentage by volume to be 15 ~ 90%.
9. the preparation method of green tea feature perfume (or spice) spice as claimed in claim 1, is characterized in that: in described step A, B, C, decompression
The pressure condition concentrated is 0.01 ~ 0.08MPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178357A (en) * | 2014-09-10 | 2014-12-03 | 嘉兴市得百科新材料科技有限公司 | Preparation method of green tea flavor for cigarettes |
| CN104171157A (en) * | 2014-09-10 | 2014-12-03 | 嘉兴市得百科新材料科技有限公司 | Green tea extract as well as preparation method and application thereof |
| CN105559136A (en) * | 2015-12-30 | 2016-05-11 | 立场电子科技发展（上海）有限公司 | Method for preparing electronic cigarette juice fragrance from green tea enzyme |
-
2016
- 2016-08-22 CN CN201610696472.4A patent/CN106318626A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178357A (en) * | 2014-09-10 | 2014-12-03 | 嘉兴市得百科新材料科技有限公司 | Preparation method of green tea flavor for cigarettes |
| CN104171157A (en) * | 2014-09-10 | 2014-12-03 | 嘉兴市得百科新材料科技有限公司 | Green tea extract as well as preparation method and application thereof |
| CN105559136A (en) * | 2015-12-30 | 2016-05-11 | 立场电子科技发展（上海）有限公司 | Method for preparing electronic cigarette juice fragrance from green tea enzyme |
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