CN1520811A - External use composition containing oil-soluble licorice extract and its stabilization method - Google Patents
External use composition containing oil-soluble licorice extract and its stabilization method Download PDFInfo
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Abstract
The composition containing liposoluble licorice extractive for external use can suppress discoloration and stinking-up of the liposoluble licorice extractive, prevent the effective component in the liposoluble licorice extractive from decomposing and suppress gas generation accompanying the decomposing of pyrosulfite and/or sulfite, and has greatly raised stability. It contains liposoluble licorice extractive, at least one of pyrosulfite and sulfite and at least one selected from glycyrrhizic acid, glycyrrhizinate, glycyrrhitic acid and its derivative, and has pH value regulated to 4.5-7.5.
Description
Technical field
The invention relates to and to change painted and smelly in time by inhibited oil dissolubility Radix Glycyrrhizae extract, and can prevent the decomposition such as effective ingredient glabric acid (グ ラ Block リ ジ Application), liquorice chalcone (リ コ カ Le コ Application) A of oil-soluble Radix Glycyrrhizae extract, simultaneously can suppress to follow pyrosulfite and/or sulphite to decompose and produce gas, increase substantially the preparation composition for external use that contains the oil-soluble Radix Glycyrrhizae extract of stability, and contain the stabilization method of the preparation composition for external use of this oil-soluble Radix Glycyrrhizae extract.
Background technology
The oil-soluble Radix Glycyrrhizae extract is to use pure and mild ethyl acetate equal solvent, extracts from the licorice of pulse family, stem to obtain, and contains the extract of a large amount of flavonoid.Known this oil-soluble Radix Glycyrrhizae extract has a lot of useful effects in the purposes of antioxidation (opening clear 58-217583 communique with reference to the spy), anti-oxidation effect (opening clear 59-46210 communique with reference to the spy), whitening function (open flat 1-149706 communique with reference to the spy, He Te opens flat 1-311011 communique), ultra-violet absorption effect skin preparations for extenal use such as (opening flat 1-157509 communique with reference to the spy).Yet the problem of existence is above-mentioned oil-soluble Radix Glycyrrhizae extract, even the former state extract is easy to the fixed preparation of making, long preservation also can be painted, produces stink.
Therefore, in food, cosmetics, pharmaceuticals etc.,, propose to cooperate (opening flat 2-204417 communique) such as vitamin E, Galla Turcica (Galla Helepensis) acids, ascorbic acid class, Pyrusussuriensis acids, flavonoid class with reference to the spy as stabilizing agent for stabilize oil dissolubility Radix Glycyrrhizae extract.Yet the effect of these stabilizing agents is very weak, and the oil-soluble Radix Glycyrrhizae extract is difficult to reach long-time stable in preparation.
In order to solve such problem, proposed to contain the external agent (opening flat 6-263624 communique) of oil-soluble Radix Glycyrrhizae extract and pyrosulfite and/or sulphite with reference to the spy.According to this motion, though one of the effective ingredient glabric acid of oil-soluble Radix Glycyrrhizae extract is stablized, mixed the oil-soluble Radix Glycyrrhizae extract of a lot of compositions, still can not suppress to change and color development, smelly in time.And have following shortcoming, or be accompanied by the decomposition generation gas of pyrosulfite and/or sulphite, or, damage emulsifying because of the use level of pyrosulfite and/or sulphite influences stability of formulation, thus the precipitation of generation.
Therefore, present present situation is also not obtain a kind of preparation composition for external use that contains the oil-soluble Radix Glycyrrhizae extract, can inhibited oil dissolubility Radix Glycyrrhizae extract change in time and painted and smelly, can prevent the decomposition such as effective ingredient glabric acid, licochalcone A of oil-soluble Radix Glycyrrhizae extract, can suppress to follow simultaneously the decomposition of pyrosulfite and/or sulphite and generation gas.
Summary of the invention
The present invention proposes in view of above-mentioned present situation, the above-mentioned all problems before solving, and will reach following purpose as problem.Promptly, the purpose of this invention is to provide a kind of effective ingredient such as glabric acid, licochalcone A that can prevent in the oil-soluble Radix Glycyrrhizae extract decomposes, be not accompanied by decomposition of pyrosulfite and/or sulphite and generation gas and can prevent oil-soluble Radix Glycyrrhizae extract color development, smelly, can prevent that effective ingredient from changing in time and precipitate, what increased substantially stability contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use, and contains the stabilization method of this oil-soluble Radix Glycyrrhizae extract preparation composition for external use.
Present inventors are in order to solve above-mentioned problem, and through further investigation, the result obtains following opinion.Promptly, contain (A) oil-soluble Radix Glycyrrhizae extract, (B) are selected at least one and (C) selected from pyrosulfite and sulphite at least one from glycyrrhizic acid and salt and enoxolone and derivant thereof, by PH being adjusted into 4.5～7.5 scope, can prevent the decomposition such as effective ingredient glabric acid, licochalcone A of oil-soluble Radix Glycyrrhizae extract in the preparation, simultaneously can prevent to change in time and painted, smelly, and, can also suppress to follow pyrosulfite and/or sulphite to decompose and generation gas.
The oil-soluble Radix Glycyrrhizae extract preparation composition for external use that contains of the present invention, it is characterized in that containing at least one that (A) oil-soluble Radix Glycyrrhizae extract, (B) select, at least one that (C) selects from glycyrrhizic acid and its esters and enoxolone and derivant thereof from pyrosulfite and sulphite, and, with respect to the preparation composition for external use total amount, in the drying solid composition, contain above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract of 0.005～0.1 weight %.
Also have, the stabilization method that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use of the present invention is that the PH scope that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use with the invention described above is adjusted into 4.5～7.5.
According to the present invention, can obtain can inhibited oil dissolubility Radix Glycyrrhizae extract to change in time and painted, smelly, can prevent the decomposition such as effective ingredient glabric acid, licochalcone A of oil-soluble Radix Glycyrrhizae extract, and can suppress to follow pyrosulfite and/or sulfurous acid to decompose and produce gas, what increase substantially stability contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use.
Concrete example
(containing oil-soluble Radix Glycyrrhizae extract preparation composition for external use)
The oil-soluble Radix Glycyrrhizae extract preparation composition for external use that contains of the present invention, contain that (A) oil-soluble Radix Glycyrrhizae extract, (B) are selected at least one from pyrosulfite and sulphite, (C) selects at least one from glycyrrhizic acid and its esters and enoxolone and derivant thereof, and then also can contain other compositions as required.
-oil-soluble Radix Glycyrrhizae extract-
Above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract does not have particular determination, can do suitably to select according to purpose, but preferably with the glycyrrhiza genus of pulse family and extract residue and obtain as extracting raw material.
Glycyrrhiza genus as above-mentioned pulse family does not have particular restriction, can suitably select according to desired effective ingredient.For example, G1ycyrrhiza glabra (Glycyrrhiza glabra), Glycyrrhiza inflata Bat. (Glycyrrhizainflata), Radix Glycyrrhizae (Glycyrrhiza araleasis), Radix Glycyrrhizae (Glycyrrhiza uralensis), Radix Glycyrrhizae (Glycyrrhiza echinata) etc. are arranged.Can use their root, rhizome, leaf, any position of stem to make raw material, preferably with its root and/or rhizome as raw material.
Most Radix Glycyrrhizaes all are referred to as titled with place of production name, for example, northwest, Northeast China Radix Glycyrrhizae (Glycyrrhizauralensis), Xinjiang Radix Glycyrrhizae (Glycyrrhiza echinata), Russia product Radix Glycyrrhizae (Glycyrrhizaglabura), Spain produce Radix Glycyrrhizae (Glycyrrhiza echinata), Mongolia produces Radix Glycyrrhizae, Afghanistan product Radix Glycyrrhizae, or the like.
As the said extracted raw material, can use growth-gen, also can use dry thing, also can be with the water extraction residue as raw material.
The water extraction residue of so-called above-mentioned Radix Glycyrrhizae, be meant to obtaining glycyrrhizic acid, make water, warm water or hot water, the solid residue behind perhaps use neutrality or subalkaline cold water, warm water and the hot water extraction from above-mentioned Radix Glycyrrhizae, perhaps their combination, or the solid residue after extracting repeatedly.Residue after the said extracted can be aqueous or exsiccant any state.
As contained effective ingredient in the above-mentioned oil-soluble Radix Glycyrrhizae extract, different with the Radix Glycyrrhizae kind of conduct extraction raw material, can not stipulate without exception, glabric acid, glabrene. (グ ラ Block レ Application), licochalcone A, liquorice chalcone B, グ リ シ Network マ リ Application, グ リ ソ Off ラ ボ Application etc. are for example arranged, in these, the preferably glabric acid of representing with following structural formula, glabrene., licochalcone A, liquorice chalcone B.
Glabric acid (グ ラ Block リ ジ Application)
Glabrene. (グ ラ Block Application)
Licochalcone A (リ コ カ Le コ Application A)
Liquorice chalcone B (リ コ カ Le コ Application B)
About above-mentioned glabric acid and glabrene., through confirming to have pharmacological actions such as antibacterial action, antioxidation, effect against corrosion, antifibrinolysin effect.Also know to have and suppress to generate melanic effect (spy opens flat 1-311011 communique).
About above-mentioned licochalcone A and liquorice chalcone B, known have antibacterial action (spy opens clear 62-181202 communique), inhibition platelet aggregation effect (spy opens flat 4-297418 communique), antitumor action (spy opens flat 6-122623 communique), androgen receptor to encumber effect (spy opens the 2001-163718 communique) in conjunction with encumbering effect and testosterone-5, or the like.
At least one effective ingredient of selecting in glabric acid from above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract, glabrene., licochalcone A, liquorice chalcone B, グ リ シ Network マ リ Application and the グ リ ソ Off ラ ボ Application adds up to amount, in the drying solid composition, to oil-soluble Radix Glycyrrhizae extract total amount, preferred 1～80 weight %, more preferably 5～60 weight %.
Specifically, as the said extracted raw material, when using Glycyrrhiza glabura, the total amount of glabric acid and glabrene. in the drying solid composition, is 1 weight % for oil-soluble Radix Glycyrrhizae extract total amount, more than the preferred 10 weight %, more preferably 20～50 weight %.
As the said extracted raw material, when using Glycyrrhiza echinata, Glycyrrhiza inflata, (A) the total amount of licochalcone A and liquorice chalcone B in the composition oil-soluble Radix Glycyrrhizae extract, in the drying solid composition, for oil-soluble Radix Glycyrrhizae extract total amount is more than the 1 weight %, more than the preferred 5 weight %, more preferably 10～40 weight %.
In order to extract residue from above-mentioned Radix Glycyrrhizae and/or liquorice beverage, obtain above-mentioned oil-soluble Radix Glycyrrhizae extract, with various organic solvents alone or in combination, extract with known method.
As above-mentioned organic solvent, there is not particular restriction, can do suitably to select according to purpose.For example, benzene,toluene,xylene, ether, methyl ethyl ketone, methyl iso-butyl ketone (MIBK), dichloromethane, dichloroethanes, chloroform, ethyl acetate, propyl acetate, butyl acetate, acetone, methanol, ethanol, propanol, aqueous methanol, aquiferous ethanol, moisture propanol etc. are arranged.As supercritical fluid, also can act on carbon dioxide.In these, ethanol, aquiferous ethanol, safety is best.
In order to extract residue from above-mentioned Radix Glycyrrhizae or liquorice beverage, obtain the condition of Radix Glycyrrhizae oiliness extract with above-mentioned organic solvent, there is not particular restriction, can suitably select according to purpose, for example have with respect to extracting the above-mentioned organic solvent that raw material adds 2～15 times of amounts, the method of extracting at normal temperatures while stirring, the method for heating and refluxing extraction.These methods can be distinguished use separately, and use also capable of being combined is if repeatable operation can improve extraction efficiency better.
The gained extracting solution after utilizing centrifugalize or removing by filter insoluble matter, but uses as oil-soluble Radix Glycyrrhizae extract former state.Also can utilize conventional method, concentrate the back and use.These extracting solution, in not reducing the physiologic effect scope of desired effective ingredient, it is refining suitably to carry out deodorize, decolouring etc.For above-mentioned subtractive process, generally use active carbon, synthetic adsorbent resin and ion exchange resin etc.If with the extracting solution drying,, can obtain filemot extract powder as the oil-soluble Radix Glycyrrhizae extract with suitable method.
With the concentrate of aqueous extract former state of gained or liquid extract and then the powder or the solid drying thing of aqueous extract, as the oil-soluble Radix Glycyrrhizae extract.
Making with extra care of above-mentioned oil-soluble Radix Glycyrrhizae extract for example utilized along after phase silica gel chromatographic column and the processing of anti-phase chromatographic column, utilizes the method for acetone recrystallize to carry out.According to the method, can obtain the pure product of effective ingredient with comparalive ease.In addition, the chromatographic column that also can adopt synthetic adsorbate to form, or liquid-liquid convection current extraction etc. arbitrarily the organic compound process for purification make with extra care.
As above-mentioned oil-soluble Radix Glycyrrhizae extract, there is not particular restriction, also can use commercially available product.
The amount of above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract for containing oil-soluble Radix Glycyrrhizae extract preparation composition for external use total amount, in the drying solid composition, is 0.005～0.1 weight %, preferred 0.01～0.1 weight %.When the amount of above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract is lower than 0.005 weight %, active effect from the oil-soluble Radix Glycyrrhizae extract is very little, and when surpassing 0.1 weight %, also can not improve, and cause expense to increase from the active effect of oil-soluble Radix Glycyrrhizae extract.
-pyrosulfite and/or sulphite-
Pyrosulfite as above-mentioned (B) composition does not have particular restriction, can suitably select according to purpose, for example, potassium metabisulfite, sodium pyrosulfite etc. is arranged, preferred sodium pyrosulfite in these.
Sulphite as above-mentioned (B) composition does not have particular restriction, can do suitably to select according to purpose, for example, have ammonium sulfite, potassium sulfite, ammonium bisulfite, Potassium acid sulfite, sodium sulfite, sodium sulfite, etc., preferred sodium sulfite in these.
These pyrosulfites and sulphite can use a kind separately, also can mix the back more than 2 kinds and use.
The amount of above-mentioned (B) composition pyrosulfite and/or sulphite, for containing oil-soluble Radix Glycyrrhizae extract preparation composition for external use total amount, preferred 0.001～0.5 weight %, more preferably 0.01～0.05 weight %, when the amount of above-mentioned (B) composition pyrosulfite and/or sulphite was lower than 0.001 weight %, pyrosulfite and/or sulphite can not be given full play to effect sometimes.And when surpassing 0.5 weight %, sometimes skin is had intense stimulus, and with strong odor.
-glycyrrhizic acid and its esters, and enoxolone and derivant thereof-
As above-mentioned (C) composition glycyrrhizic acid and its esters and enoxolone and derivant thereof, there is not particular restriction, can suitably select according to purpose.For example, glycyrrhizic acid, ammonium glycyrrhizinate, glycyrrhizic acid first salt, sodium glycyrrhetate, enoxolone, the hard ester of enoxolone, 3-succinum acyl-oxygen disodium glycyrrhizinate, or the like.In these, glycyrrhizic acid dipotassium, the hard ester of enoxolone are best.
These can use a kind separately, also can mix use more than 2 kinds.
Above-mentioned (C) composition glycyrrhizic acid and its esters and enoxolone and derivant thereof, available aqueous solvent extraction Radix Glycyrrhizae obtains.Also can use commercially available product.
From above-mentioned (C) composition glycyrrhizic acid and its esters, and the amount of choosing at least one in enoxolone and the derivant thereof, in the drying solid composition, for containing oil-soluble Radix Glycyrrhizae extract preparation composition for external use total amount, preferred 0.01～0.5 weight %, more preferably 0.1～0.3 weight %.When the amount of above-mentioned (C) composition glycyrrhizic acid and its esters and enoxolone and derivant thereof was lower than 0.01 weight %, the effect of glycyrrhizic acid and its esters and enoxolone and derivant thereof can not be given full play to sometimes.And when surpassing 0.5 weight %, stability of formulation can reduce sometimes.
Among the present invention, for 1 weight portion above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract (drying solid thing), the at least one that at least one that preferred cooperation 0.1～5 weight portion is selected from (B) composition pyrosulfite and sulphite and 0.5～10 weight portion are selected from (C) composition glycyrrhizic acid and its esters and enoxolone and derivant thereof.For 1 weight portion above-mentioned (A) composition oil-soluble Radix Glycyrrhizae extract (drying solid thing), preferred at least one and 0.5～5 weight portion that cooperates 0.1～0.5 quality to select from (B) composition pyrosulfite and sulphite selected at least one from (C) composition glycyrrhizic acid and its esters and enoxolone and derivant thereof.
When above-mentioned (B) composition with (C) when the use level of composition is lower than above-mentioned scope, compositions does not have pharmacological effect sometimes, and when being higher than above-mentioned scope, smelly sometimes, stability reduces.
-other compositions-
Of the present invention containing in the oil-soluble Radix Glycyrrhizae extract preparation composition for external use, except above-mentioned (A)～(C) composition, other known compositions that also can cooperate suitable selection as required, for example, PH regulator, surfactant, oils, alcohols, wetting agent, antiseptic, chelating agen, spice, pigment, UV absorbent, at random dose of ultraviolet, or the like.And then, also can cooperate whitening agent, anti-inflammatory agent, antioxidant, vitamins, vegeto-animal extract of suitable selection etc. according to purposes.
As above-mentioned pH regulator agent, be the just passable of 4.5～7.5 (best 6.0～7.0) scope as long as can will contain the pH regulator of oil-soluble Radix Glycyrrhizae extract preparation composition for external use, there is not particular restriction, can suitably select according to purpose, can use acid or alkali.As above-mentioned acid, for example have hydrochloric acid, phosphoric acid, sulphuric acid, citric acid, acetic acid, tartaric acid, malic acid, etc.As above-mentioned alkali.Potassium hydroxide, ammonium hydroxide, sodium hydroxide, sodium citrate etc. are for example arranged.
The present invention contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use, does not have particular restriction, can suitably select according to purpose, for example, can be used for pharmaceuticals, medical exterior-applied article, cosmetics.In these, skin cosmetic raw materials such as optimum astringent, cream, emulsion, beauty treatment application as its agent shape, have cream, emulsion, lotion, stick agent, ointment etc.
(stabilization method that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use)
The present invention contains the stabilization method of oil-soluble Radix Glycyrrhizae extract preparation composition for external use, is the method that the invention described above is contained pH regulator to 4.5～7.5 scopes of oil-soluble Radix Glycyrrhizae extract preparation composition for external use.Just improving the stable aspect of compositions and consider, preferably is 6.0～7.0 scope with the above-mentioned pH regulator that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use.
If when the pH of above-mentioned composition did not satisfy above-mentioned pH scope, available pH regulator agent was adjusted to desired pH scope.
When utilizing the present invention to contain the stabilization method of oil-soluble Radix Glycyrrhizae extract preparation composition for external use, preserve reduction rate (being taken as 100% o'clock reduction ratio after will modulating) before and after 3 months, that contain glabric acid amount in the oil-soluble Radix Glycyrrhizae extract preparation composition for external use or licochalcone A amount in room temperature～40 ℃ down preferably below 10%, more preferably below 5%.
At this moment, glabric acid amount or licochalcone A amount, available high-speed liquid chromatography (HPLC) is measured.
When utilizing stabilization method of the present invention, ℃ preserve down in room temperature～40 and to contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use before and after 3 months, do not have variable color, smelly and produce gas, increase substantially stability.
Below with embodiment the present invention is described, but the present invention is not limited by these embodiment.
(Production Example 1)
Root mince 500g with Radix Glycyrrhizae (Glycyrrhiza glabra) floods in 5 liters dehydrated alcohol, and reflux 2 hours extracts the solvable composition of dehydrated alcohol.Extracting solution is separated, repeat same operation, obtain adding up to 9.2 liters extracting solution for extracting residue.The solvent decompression of extracting solution is heated up in a steamer, concentrated, dry, obtain 12.4g oil-soluble Radix Glycyrrhizae extract.
Representational flavonoid containing ratio in the oil-soluble Radix Glycyrrhizae extract with gained Production Example 1 is that glabric acid is about 40% with the quantitative result of HPLC, and glabrene. is about 3%.
(Production Example 2)
In 1kg Radix Glycyrrhizae (Glycyrrhiza inflata) root, add 10 liters of dehydrated alcohol, extraction in 5 hours refluxes.With the extracting solution concentrating under reduced pressure that obtains, in exsiccant residue, add 10 liters of ethyl acetates, extracted 5 hours.With ethyl acetate extraction liquid concentrating under reduced pressure, drying obtains the oil-soluble Radix Glycyrrhizae extract 30g of Production Example 2.
Representational flavonoid containing ratio is used the HPLC quantitative result in the oil-soluble Radix Glycyrrhizae extract with gained Production Example 2, and licochalcone A is about 25%.
(embodiment 1)
According to a conventional method, modulation contains the emulsion of oil-soluble Radix Glycyrrhizae extract shown in the following table 1 (trade name: " oil-soluble Radix Glycyrrhizae extract P-T (40) ", Maruzen Pharmaceuticals Co., Ltd.'s system, contain the glabric acid of 40 weight %, the glabrene. of 3 weight %), sodium pyrosulfite (0.005 weight %, 0.01 weight %, 0.05 weight %, 0.1 weight %, and 0.2 weight %) and glycyrrhizic acid dipotassium.
[table 1]
| Composition | Use level (weight %) |
| The lipophilic glyceryl monostearate | ????1.0 |
| Monostearate polyoxyethylene sorbitan (20E.O.) | ????1.0 |
| Four oleic acid polyoxyethylene sorbitan alcohol | ????0.5 |
| Stearic acid | ????0.2 |
| Tadenan | ????0.4 |
| Cetyl palmitate | ????0.4 |
| Three decanes | ????4.0 |
| Three 2 ethyl hexanoic acid glyceride | ????2.0 |
| Propyl p-hydroxybenzoate | ????0.1 |
| Carboxy vinyl polymer | ????0.2 |
| 1,3 butylene glycol | ????5.0 |
| Oil-soluble Radix Glycyrrhizae extract P-T (40) | ????0.05 |
| Methyl parahydroxybenzoate | ????0.1 |
| Glycyrrhizic acid dipotassium | ????0.15 |
| Sodium pyrosulfite | ????0.005 |
| ????0.01 | |
| ????0.05 | |
| ????0.1 | |
| ????0.2 | |
| Purified Water | Surplus |
| Add up to | ????100 |
Emulsion, with the potassium hydroxide aqueous solution of 4 weight %, regulating pH is 6.8.
For the emulsion that obtains, as follows, estimate stability, complexion changedization, stink variation and have or not gas to produce.The results are shown in table 2 and table 3.
＜stability test 〉
With each Emulsion that obtains, in shading condition, 40 ℃ of preservations down.Utilize high-speed liquid chromatography, when measuring through 0 month, 1 month, 2 months, 3 months, the glabric acid amount in the Emulsion.Quantitative values after the modulation is taken as 100, represents the quantitative values of process stipulated time with ratio.
The evaluation that＜complexion changedization and stink change 〉
With each Emulsion of gained, at 40 ℃, under the shading condition, preserve after 0,1,2,3 month, utilize naked eyes and sense test by 10 participants, estimate by following standard with advancing.
[evaluation criterion of complexion changedization]
Zero: colourless
△: faint yellow
*: yellow
[stink variation evaluation criterion]
Zero: no stink
△: offending stink is arranged slightly
*: offending stink
The evaluation of＜generation gas 〉
Each emulsion 20ml is injected in the synthetic resin bag of the airtight body of 100ml, detect by an unaided eye under 40 ℃, sealing, shading condition, through the inflation status of synthetic resin bag after 0,1,2,3 month, by following standard evaluation.
[producing the evaluation criterion of gas]
Zero: do not have the gas of generation
△: have gas to take place slightly
*: produce a large amount of gases
[table 2]
| After 0 month | After 1 month | After 2 months | After 3 months | |
| Reference substance (do not have and add) | ????100％ | ??89.60％ | ??72.30％ | ??51.10％ |
| Sodium pyrosulfite: 0.005 weight % | ????100％ | ??94.70％ | ??87.20％ | ??78.80％ |
| Sodium pyrosulfite: 0.01 weight % | ????100％ | ??98.90％ | ??95.60％ | ??90.50％ |
| Sodium pyrosulfite: 0.05 weight % | ????100％ | ??99.40％ | ??98.10％ | ??96.30％ |
| Sodium pyrosulfite: 0.1 weight % | ????100％ | ??99.50％ | ??97.80％ | ??97.70％ |
| Sodium pyrosulfite: 0.2 weight % | ????100％ | ??100.30％ | ??99.50％ | ??98.90％ |
From the result of table 2, can confirm under 40 ℃ condition, to preserve 0,1,2,3 middle of the month, cooperated in the emulsion of 0.01～0.2 weight % sodium pyrosulfite, it is roughly stable that glabric acid is.
[table 3]
| Estimate | After 0 month | After 1 month | After 2 months | After 3 months | |
| Reference substance (do not have and add) | Tone | ????○ | ????× | ????× | ????× |
| Stink | ????○ | ????○ | ????○ | ????○ | |
| Produce gas | ????○ | ????○ | ????○ | ????○ | |
| Sodium pyrosulfite: 0.001 weight % | Tone | ????○ | ????○ | ????○ | ????△ |
| Stink | ????○ | ????○ | ????○ | ????○ | |
| Produce gas | ????○ | ????○ | ????○ | ????○ | |
| Sodium pyrosulfite: 0.01 weight % | Tone | ????○ | ????○ | ????○ | ????○ |
| Stink | ????○ | ????○ | ????○ | ????○ | |
| Produce gas | ????○ | ????○ | ????○ | ????○ | |
| Sodium pyrosulfite: 0.05 weight % | Tone | ????○ | ????○ | ????○ | ????○ |
| Stink | ????○ | ????○ | ????○ | ????○ | |
| Produce gas | ????○ | ????○ | ????○ | ????○ | |
| Sodium pyrosulfite: 0.1 weight % | Tone | ????○ | ????△ | ????× | ????× |
| Stink | ????○ | ????○ | ????△ | ????× | |
| Produce gas | ????○ | ????△ | ????× | ????× | |
| Sodium pyrosulfite: 0.2 weight % | Tone | ????○ | ????△ | ????× | ????× |
| Stink | ????○ | ????△ | ????× | ????× | |
| Produce gas | ????○ | ????△ | ????× | ????× |
From the result of table 3, cooperated the emulsion of 0.001～0.05 weight % sodium pyrosulfite as can be known, even under 40 ℃ the condition through 3 months after, very stable, do not have variable color, smelly and produce gas.
Under room temperature (25 ℃), stability, variable color, smelly, and produce the situation of gas, the same or better with result under above-mentioned 40 ℃.
(embodiment 2)
In the emulsion with prescription shown in embodiment 1 invading the exterior 1, each the emulsion pH that has cooperated 0.05 weight % sodium pyrosulfite, when using the change of citric acid or potassium hydroxide, change for complexion changedization and stink, under 40 ℃, shading condition, preserved 0,1,2,3 month, to estimate with the foregoing description 1 identical method.The results are shown in table 4.
In the test, for the prescription emulsion of each pH, use to cooperate 0.15 weight % glycyrrhizic acid dipotassium with ill-matched 2 kinds.
[table 4]
| The use level of glycyrrhizic acid dipotassium | Estimate | After 0 month | After 1 month | After 2 months | After 3 months | |
| ??pH4 | ????- | Tone | ????○ | ????△ | ????× | ????× |
| 0.15 weight % | ????○ | ????○ | ????△ | ????× | ||
| ????- | Stink | ????○ | ????○ | ????△ | ????× | |
| 0.15 weight % | ????○ | ????○ | ????△ | ????△ | ||
| ??pH4.5 | ????- | Tone | ????○ | ????○ | ????△ | ????× |
| 0.15 weight % | ????○ | ????○ | ????○ | ????○ | ||
| ????- | Stink | ????○ | ????○ | ????○ | ????△ | |
| 0.15 weight % | ????○ | ????○ | ????○ | ????○ | ||
| ??pH6 | ????- | Tone | ????○ | ????○ | ????○ | ????△ |
| 0.15 weight % | ????○ | ????○ | ????○ | ????○ | ||
| ????- | Stink | ????○ | ????○ | ????○ | ????△ | |
| 0.15 weight % | ????○ | ????○ | ????○ | ????○ | ||
| ??pH7.5 | ????- | Tone | ????○ | ????○ | ????○ | ????× |
| 0.15 weight % | ????○ | ????○ | ????○ | ????○ | ||
| ????- | Stink | ????○ | ????○ | ????△ | ????× | |
| 0.15 weight % | ????○ | ????○ | ????○ | ????○ | ||
| ??pH8 | ????- | Tone | ????○ | ????× | ????× | ????× |
| 0.15 weight % | ????○ | ????○ | ????△ | ????× | ||
| ????- | Stink | ????○ | ????× | ????× | ????× | |
| 0.15 weight % | ????○ | ????○ | ????× | ????× |
From the result of table 4, the pH that can confirm emulsion is in 4.5～7.5 the scope, because the existence of glycyrrhizic acid dipotassium with regard to tone, stink no change, has obtained long stability.
Use the oil-soluble Radix Glycyrrhizae extract of Production Example 2, with the embodiment 1 the same emulsion of modulating, estimate the same with 2 with embodiment 1.The result is 40 ℃ and preserves 3 middle of the month down that cooperated in the emulsion of 0.01～0.2 weight % sodium pyrosulfite, licochalcone A is roughly stable.The emulsion that has cooperated 0.001～0.05 weight % sodium pyrosulfite, though under 40 ℃ through 3 months after, also very stable, no variable color, smelly and do not produce gas.And then the pH of emulsion is in 4.5～7.5 scope, and is also very stable even 40 ℃ were preserved down after 3 months, do not have complexion changedization and stink to change.
(cooperating embodiment 1)-astringent-
Make the astringent of following composition according to conventional method.The pH of astringent is 6.8.
Oil-soluble Radix Glycyrrhizae extract P-T (40) (Maruzen Pharmaceuticals Co., Ltd.'s system) 0.05g
Sodium pyrosulfite 0.01g
Glycerol 3g
1,3 butylene glycol 3g
Citric acid 0.1g
Sodium citrate 0.1g
Oleic acid polyoxyethylene sorbitan (20E.O) 0.5g
To oxygen benzoic acid methyl ester 0.15g
Citric acid 0.1g
Sodium citrate 0.1g
Glycyrrhizic acid dipotassium 0.05g
Sargassum extract 0.1g
Xylopyranose mixture 0.5g
Radix Sophorae Flavescentis extract 0.1g
Spice 0.05g
The Purified Water surplus
Add up to 100g
(cooperating embodiment 2)-cream-
Make the cream of following composition according to a conventional method.The pH of cream is 6.8.
Oil-soluble Radix Glycyrrhizae extract P-T (40) (Maruzen Pharmaceuticals Co., Ltd.'s system) 0.01g
Sodium pyrosulfite 0.005g
Enoxolone 0.01g
Liquid Paraffin 5g
White beeswax 4g
Spermol 3g
Three decane 10g
Agnolin 2g
Stearic acid 1g
Oleic acid polyoxyethylene sorbitan (20E.O) 1.5g
Glyceryl monostearate 3g
1,3 butylene glycol 6g
Citric acid 0.1g
Sodium citrate 0.1g
Yeast extract 0.1g
Folium Perillae extracting solution 0.1g
Gravy extracting solution 0.1g
Tilia extracting solution 0.1g
To oxygen benzoic acid methyl ester 1.5g
Spice 0.1g
The Purified Water surplus
Add up to 100g
(cooperating embodiment 3)-astringent-
Utilize conventional method to make the astringent of following composition.The pH of astringent is 6.8.
The oil-soluble Radix Glycyrrhizae extract 0.05g of Production Example 2
Sodium pyrosulfite 0.01g
Glycerol 3g
1,3 butylene glycol 3g
Oleic acid polyoxyethylene sorbitan (20E.O) 0.5g
To oxygen benzoic acid methyl ester 0.15g
Citric acid 0.1g
Sodium citrate 0.1g
Glycyrrhizic acid dipotassium 0.05g
Sargassum extract 0.1g
Xylopyranose mixture 0.5g
Radix Sophorae Flavescentis extract 0.1g
Spice 0.05g
Add up to 100g
(cooperating embodiment 4)-cream-
Utilize conventional method to make the cream of following composition.The pH of cream is 6.8.
The oil-soluble Radix Glycyrrhizae extract 0.01g of Production Example 2
Sodium pyrosulfite 0.005g
Enoxolone 0.01g
Liquid Paraffin 5g
White beeswax 4g
Spermol 3g
Zamene 10g
Agnolin 2g
Stearic acid 1g
Oleic acid polyoxyethylene sorbitan (20E.O) 1.5g
Glyceryl monostearate 3g
1,3 butylene glycol 6g
Citric acid 0.1g
Sodium citrate 0.1g
Yeast extract 0.1g
Folium Perillae extracting solution 0.1g
Gravy extracting solution 0.1g
Tilia extracting solution 0.1g
To oxygen benzoic acid methyl ester 1.5g
Spice 0.1g
The Purified Water surplus
Add up to 100g
(cooperating embodiment 5)-astringent-
Utilize conventional method to make the astringent of following composition.The pH of astringent is 6.8.
The oil-soluble Radix Glycyrrhizae extract 0.01g of Production Example 1
The oil-soluble Radix Glycyrrhizae extract 0.05g of Production Example 2
Sodium pyrosulfite 0.01g
Glycerol 3g
1,3 butylene glycol 3g
Oleic acid polyoxyethylene sorbitan (20E.O) 0.5g
To oxygen benzoic acid methyl ester 0.15g
Citric acid 0.1g
Sodium citrate 0.1g
Glycyrrhizic acid dipotassium 0.05g
Sargassum extract 0.1g
Xylopyranose mixture 0.5g
Radix Sophorae Flavescentis extract 0.1g
Spice 0.05g
The Purified Water surplus
Add up to 100g
(cooperating embodiment 6)-cream-
Utilize conventional method to make the cream of following composition.The pH of cream is 6.8.
The oil-soluble Radix Glycyrrhizae extract 0.01g of Production Example 1
The oil-soluble Radix Glycyrrhizae extract 0.01g of Production Example 2
Sodium pyrosulfite 0.005g
Enoxolone 0.01g
Liquid Paraffin 5g
White beeswax 4g
Spermol 3g
Three decane 10g
Agnolin 2g
Stearic acid 1g
Oleic acid polyoxyethylene sorbitan (20E.O) 1.5g
Glyceryl monostearate 3g
1,3 butylene glycol 6g
Citric acid 0.1g
Sodium citrate 0.1g
Yeast extract 0.1g
Folium Perillae extracting solution 0.1g
Gravy extracting solution 0.1g
Tilia extracting solution 0.1g
To oxygen benzoic acid methyl ester 1.5g
Spice 0.1g
The Purified Water surplus
Add up to 100g
The cosmetic material of above-mentioned cooperation embodiment 1～6, after keeping 3 months under 40 ℃ the condition, invariant color, not smelly, no gas produces, excellent in stability.
Claims (19)
1, contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use, it is characterized in that containing at least one that (A) oil-soluble Radix Glycyrrhizae extract, (B) are selected from pyrosulfite and sulphite, (C) at least one of from glycyrrhizic acid and its esters and enoxolone and derivant thereof, selecting, and, the oil-soluble Radix Glycyrrhizae extract of above-mentioned (A) composition, with respect to the preparation composition for external use total amount,, contain 0.005 weight %～0.1 weight % in the drying solid composition.
2, according to claim 1 record contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use, wherein the oil-soluble Radix Glycyrrhizae extract of (A) composition is with the glycyrrhiza genus of pulse family and extracts residue and obtain as extracting raw material.
3, according to each record in the claim 1～2 contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use, wherein the oil-soluble Radix Glycyrrhizae extract of (A) composition is that at least one of selecting from G1ycyrrhiza glabra (Glycyrrhiza glabra), Glycyrrhiza inflata Bat. (Glycyrrhiza inflata) and Radix Glycyrrhizae (Glycyrrhiza uralensis) obtains as extracting raw material.
4, according to each record in the claim 1～3 contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use, wherein the oil-soluble Radix Glycyrrhizae extract of (A) composition contains at least one of selecting from glabric acid, glabrene., licochalcone A, liquorice chalcone B, グ リ シ Network マ リ Application and グ リ ソ Off ラ ボ Application.
5, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to claim 4 record, the total amount of at least one effective ingredient of selecting in the glabric acid from the oil-soluble Radix Glycyrrhizae extract of (A) composition, glabrene., licochalcone A, liquorice chalcone B, グ リ シ Network マ リ Application and the グ リ ソ Off ラ ボ Application wherein, with respect to oil-soluble Radix Glycyrrhizae extract total amount, in the drying solid composition, be 1～80 weight %.
6, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to each record in the claim 1～5, the oil-soluble Radix Glycyrrhizae extract of (A) composition wherein, as extracting raw material, use Glycyrrhizaglabura, and the total amount of glabric acid and glabrene. is with respect to oil-soluble Radix Glycyrrhizae extract total amount, in the drying solid composition, more than 1 weight %.
7, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to each record in the claim 1～5, the oil-soluble Radix Glycyrrhizae extract of (A) composition wherein, as extracting raw material, use at least a among Glycyrrhizaechinata and the Glycyrrhiza inflata, and the total amount of licochalcone A and liquorice chalcone B is with respect to oil-soluble Radix Glycyrrhizae extract total amount, in the drying solid composition, more than 1 weight %.
8, according to each record in the claim 1～7 contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use, wherein the pyrosulfite of (B) composition is select from sodium pyrosulfite and potassium metabisulfite any.
9, according to any one record in the claim 1～8 contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use, wherein the sulphite of (B) composition is at least one of selecting from ammonium sulfite, potassium sulfite, ammonium bisulfite, calcium bisulfite, sodium sulfite and sodium sulfite.
10, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to each record in the claim 1～9, the wherein pyrosulfite of (B) composition and/or the amount of sulphite, with respect to containing oil-soluble Radix Glycyrrhizae extract preparation composition for external use total amount, be 0.001～0.5 weight %.
11, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to each record in the claim 1～10, wherein glycyrrhizic acid of (C) composition and its esters and enoxolone and derivant thereof are in the hard ester of glycyrrhizic acid, glycyrrhizic acid dipotassium, enoxolone and enoxolone any.
12, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to each record in the claim 1～11, the at least one amount of from the glycyrrhizic acid of (C) composition and its esters and enoxolone and derivant thereof, selecting wherein, with respect to containing oil-soluble Radix Glycyrrhizae extract preparation composition for external use total amount, in the drying solid composition, be 0.01～0.5 weight %.
13, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to each record in the claim 1～12, wherein with respect to oil-soluble Radix Glycyrrhizae extract (drying solid thing) 1 weight portion of (A) composition, the at least one that cooperates at least one that 0.1～5 weight portion selects from the pyrosulfite of (B) composition and sulphite and 0.5～10 weight portion from the glycyrrhizic acid of (C) composition and its esters and enoxolone and derivant thereof, to select.
14, contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use according to claim 13 record, wherein with respect to the oil-soluble Radix Glycyrrhizae extract (drying solid thing) of 1 weight portion (A) composition, the at least one that cooperates at least one that 0.1～0.5 weight portion selects from the pyrosulfite of (B) composition and sulphite and 0.5～5 weight portion from the glycyrrhizic acid of (C) composition and its esters and enoxolone and derivant thereof, to select.
15, according to each record in the claim 1～14 contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use, wherein pH regulator is 4.5～7.5 scope.
16, the stabilization method that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use is characterized in that the pH that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use of each record in the claim 1～15 is adjusted to 4.5～7.5 scope.
17,, wherein be 6.0～7.0 scope with pH regulator according to the stabilization method that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use of claim 16 record.
18, according to the stabilization method that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use of each record in the claim 16～17, wherein add the pH regulator agent, with the scope of pH regulator to regulation.
19, according to the stabilization method that contains oil-soluble Radix Glycyrrhizae extract preparation composition for external use of each record in the claim 16～18, wherein after room temperature～40 ℃ are preserved 3 months, the reduction rate that contains the glabric acid amount that has in the oil-soluble Radix Glycyrrhizae extract preparation composition for external use or licochalcone A amount is below 10%, and, preserve down in room temperature～40 ℃ and to contain oil-soluble Radix Glycyrrhizae extract preparation composition for external use before and after 3 months, invariant color, not smelly, do not produce gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA03107572XA CN1520811A (en) | 2003-02-14 | 2003-02-14 | External use composition containing oil-soluble licorice extract and its stabilization method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA03107572XA CN1520811A (en) | 2003-02-14 | 2003-02-14 | External use composition containing oil-soluble licorice extract and its stabilization method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010031522A1 (en) | 2008-09-16 | 2010-03-25 | Beiersdorf Ag | Oil/water active ingredient emulsion containing uv filter |
-
2003
- 2003-02-14 CN CNA03107572XA patent/CN1520811A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010031522A1 (en) | 2008-09-16 | 2010-03-25 | Beiersdorf Ag | Oil/water active ingredient emulsion containing uv filter |
| EP2471501A1 (en) * | 2008-09-16 | 2012-07-04 | Beiersdorf AG | Oil/water active ingredient emulsion containing UV filter |
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