CN103269676B - Liquid oral composition - Google Patents
Liquid oral composition Download PDFInfo
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- CN103269676B CN103269676B CN201180062456.5A CN201180062456A CN103269676B CN 103269676 B CN103269676 B CN 103269676B CN 201180062456 A CN201180062456 A CN 201180062456A CN 103269676 B CN103269676 B CN 103269676B
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- liquid oral
- salt
- ascorbic acid
- oral composition
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/362—Polycarboxylic acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
Abstract
Provided are: a liquid oral composition in which an ascorbic acid phosphate ester compound is mixed, wherein the stability of the ascorbic acid phosphate ester compound has been improved, the reduced persistence and generation of sediment thereof over time have been simultaneously inhibited, and the composition feels good instead of feeling odd when used; and a method for stabilizing ascorbic acid phosphate esters or salts thereof in liquid oral compositions. A liquid oral composition containing (A) an ascorbic acid phosphate ester or salt thereof and not containing an abrasive, wherein (B) an organic acid or salt thereof and (C) an ortho-phosphate have been mixed, pH has been set to be 6.5-8.0, and the water content has been set to be 60 mass% or more. A method for stabilizing ascorbic acid phosphate esters or salts thereof in liquid oral compositions, wherein component (B) and component (C) are mixed into a liquid oral composition containing component (A) and not containing an abrasive, the pH is set to be 6.5-8.0, and the water content is set to be 60 mass% or more.
Description
Technical field
The present invention relates to a kind of liquid oral composition, it contains ascorbic acid phosphoric acid esters or its salt and does not comprise grinding agent, the words be described in further detail, the present invention relates to the ageing stability excellence of a kind of ascorbic acid phosphoric acid esters or its salt and precipitation can be produced by inhibitory preparation, there is no sense of discomfort and the good liquid oral composition of use sense, and the stabilization method of ascorbic acid phosphoric acid esters in liquid oral composition or its salt.
Background technology
It is reported, play important role in the manifesting of the enzymatic activity of ascorbic acid in biology, there is various physiologically active.Particularly, the coenzyme as prolyl and lysyl-hydroxylase plays a role, and is necessary in collagen synthesis.Therefore, in prevention, treat the gingivitis that the destruction due to collagen is caused, very useful on periodontitis, always develop various ascorbic acid derivates, particularly ascorbic acid phosphoric acid esters and salt thereof and enjoyed and gaze at.
But, when ascorbic acid phosphoric acid esters is mixed in composition for oral cavity, have ascorbic acid phosphoric acid esters through time the remaining rate problem that declines.Particularly because the water quantities in the liquid oral composition of collutory and liquid dentifrice etc. is many, the decline of remaining rate is remarkable, and the decline suppressing the remaining rate after its at high temperature long-time preservation is very difficult.
In addition, ascorbic acid phosphoric acid esters class is stablized in alkaline side, maintain the pH of compositions in alkaline range, restrained effectively the decline of remaining rate, but, on the other hand, if the pH of liquid oral composition is more than 8, just there is such problem: can feel when being contained in mouth and the sense of discomfort of stick-slip and abnormal flavour etc. easily produce precipitation etc., in formulation middle generation problem.
In the past, as the technology stably mixing ascorbic acid phosphoric acid esters class, Japanese documentation 1(JP 2000-256153 publication) in disclose following composition for oral cavity: there is the chelating agen of carboxyl by mixing, there is the chelating agen of the phosphate of condensed phosphoric acid or phytic acid etc., prevent ascorbic acid or its derivant through time remaining rate decline.But have such problem: the chelating agen with the phosphate of condensed phosphoric acid or phytic acid etc. is not identical with orthophosphate, in addition, have through time and produce the situation of precipitation, and damage the homogeneous outward appearance of liquid oral composition.Japanese documentation 2(Unexamined Patent 4-173727 publication) in disclose following composition for oral cavity: while ascorbic acid phosphoric acid esters apoplexy due to endogenous wind mixed-abrasive, suppress painted by mixing citric acid, phosphate, carbonate, bicarbonate etc., but this painted power is not necessarily consistent with the decline degree of the remaining rate of ascorbic acid phosphoric acid esters class.The water-insoluble compound that grinding agent is such, is difficult to be mixed in liquid oral composition, in addition, the suppression of this technology through time the effect of decomposing insufficient.
The method producing precipitation is suppressed as mixing ascorbic acid phosphoric acid esters based composition, Japanese documentation 3(JP 62-63597 publication) in disclose mixing organic carboxyl acid (salt), organic phosphoric acid (salt), organic sulfate method, patent documentation 4(JP 2002-255981 publication) in disclose the Asc 2-P and manufacture method thereof that reduce calcium compounds content, infer that calcium compounds is the factor producing precipitation.But the effect that the suppression ascorbic acid phosphoric acid esters class of these technology is decomposed is low, is difficult to solve the problem producing precipitation, suppress decomposition simultaneously.
Prior art document
Patent documentation
Patent documentation 1: Japanese Patent Laid-Open 2000-256153 publication
Patent documentation 2: Japanese Patent Laid-Open 4-173727 publication
Patent documentation 3: Japanese Patent Laid-Open No. Sho 62-63597 publication
Patent documentation 4: Japanese Patent Laid-Open 2002-255981 publication
The problem that invention will solve
From this point, expect the new technique that following preparation can be provided: in liquid oral composition, maintain the stable of ascorbic acid phosphoric acid esters class, solve its remaining rate simultaneously and decline and produce the problem of precipitation, the preparation that use sense is good.
In view of above-mentioned thing, the object of the present invention is to provide in the liquid oral composition being mixed with ascorbic acid phosphoric acid esters class, improve the stability of ascorbic acid phosphoric acid esters class, and suppress simultaneously ascorbic acid phosphoric acid esters class through time the remaining decline of rate and the generation of precipitation, and the stabilization method of ascorbic acid phosphoric acid esters in the liquid oral composition not having sense of discomfort, use sense good and liquid oral composition or its salt.
Solve the means of problem
The present inventor is in order to achieve the above object through attentively studying discovery: by making containing (A) ascorbic acid phosphoric acid esters or its salt, and not containing mixing (B) organic acid or its salt and (C) orthophosphate in the liquid oral composition of grinding agent, pH when 25 DEG C is made to be 6.5 ~ 8.0, water quantities in compositions is more than 60 quality %, thus can maintain the stability of ascorbic acid phosphoric acid esters or its salt and the inhibition of precipitation well.
Find to provide following liquid oral composition according to the present invention, thus complete the present invention: containing ascorbic acid phosphoric acid esters or its salt and not containing the liquid oral composition of grinding agent, even if at pH be less than 8 scope near, preserve at 60 DEG C and within 1 month, also can make ascorbic acid phosphoric acid esters or it is salt-stabilized, thus, outside the ageing stability excellence of ascorbic acid phosphoric acid esters or its salt, effectively can suppress the generation precipitated, and there is no sense of discomfort when being contained in mouth and there is the liquid oral composition of good use sense.
Namely in technology in the past not containing in the liquid oral composition of grinding agent, be difficult to make ascorbic acid phosphoric acid esters class stabilisation fully in the scope of below pH8, in addition, suppress the sedimentation effect of the organic carboxylate of citrate etc. also insufficient.The effect that the phosphatic suppression such as known ascorbic acid phosphoric acid esters apoplexy due to endogenous wind mixing citrate, phosphoric acid 2 sodium are painted, by preventing remaining rate from declining at ascorbic acid phosphoric acid esters apoplexy due to endogenous wind with citrate and pyrophosphate or tripolyphosphate.But the neodoxy of the present inventor is, by and with (B) organic acid or its salt and (C) orthophosphate, and make the pH of compositions be 6.5 ~ 8.0, water quantities in compositions is more than 60 quality %, even the liquid oral composition of below pH8 also effectively can make ascorbic acid phosphoric acid esters or it is salt-stabilized, thus suppress the generation that the remaining rate of ascorbic acid phosphoric acid esters or its salt declines and precipitates, and good use sense can be provided simultaneously.
In addition, the mechanism of action in the present invention is also indefinite, but infer by (A) ascorbic acid phosphoric acid esters or its salt and with (B) organic acid or its salt and (C) orthophosphate, these composition synergism, can suppress the generation that the remaining rate of ascorbic acid phosphoric acid esters or its salt declines and precipitates simultaneously.
Thus, the invention provides the stabilization method of ascorbic acid phosphoric acid esters in following liquid oral composition and liquid oral composition or its salt.
(1) a kind of liquid oral composition, it is characterized in that, containing (A) ascorbic acid phosphoric acid esters or its salt and not containing in the liquid oral composition of grinding agent, mixing (B) organic acid or its salt and (C) orthophosphate, and pH when making 25 DEG C is 6.5 ~ 8.0, makes the water quantities in compositions be more than 60 quality %.
(2) liquid oral composition as described in (1), wherein, mixed proportion (B)/(C) of (B) composition and (C) composition is 0.1 ~ 5 by quality ratio.
(3) liquid oral composition as described in (1) or (2), wherein, containing (B) composition 0.01 ~ 1 quality %, (C) composition 0.01 ~ 1 quality %.
(4) liquid oral composition as described in (1), (2) or (3), wherein, (B) composition is more than a kind of being selected from citric acid, malic acid, tartaric acid, succinic acid and salt thereof.
(5) ascorbic acid phosphoric acid esters in a kind of described liquid oral composition or the stabilization method of its salt, it is characterized in that, containing (A) ascorbic acid phosphoric acid esters or its salt and not containing in the liquid oral composition of grinding agent, mixing (B) organic acid or its salt and (C) orthophosphate, pH when making 25 DEG C is 6.5 ~ 8.0, makes the water quantities in compositions be more than 60 quality %.
(6) stabilization method as described in (5), wherein, the mass ratio of mixed proportion (B)/(C) of (B) composition and (C) composition is 0.1 ~ 5.
Invention effect
Find to provide following liquid oral composition according to the present invention: containing ascorbic acid phosphoric acid esters or its salt and not containing the liquid oral composition of grinding agent, even if be the scope of less than 8 at pH, also ascorbic acid phosphoric acid esters can be made or it is salt-stabilized, and suppress simultaneously ascorbic acid phosphoric acid esters or its salt through time the remaining decline of rate and the generation of precipitation, and the liquid oral composition not having sense of discomfort use sense good.
Detailed description of the invention
Below, the present invention is illustrated in greater detail.
Liquid oral composition of the present invention is the liquid oral composition not containing grinding agent, it is characterized in that, containing (A) ascorbic acid phosphoric acid esters or its salt, (B) organic acid or its salt and (C) orthophosphate, water quantities in compositions is more than 60 quality %, and pH when 25 DEG C is 6.5 ~ 8.0.
As (A) ascorbic acid phosphoric acid esters or its salt, it is the ester that more than 1 or 2 of the arbitrary hydroxyl of 2,3,5,6 of ascorbic acid becomes the compound of phosphoric acid, polyphosphoric acid etc., include, for example, ascorbic acid-2-phosphate, ascorbic acid-3-phosphate ester, ascorbic acid-6-phosphate ester, ascorbic acid-2-poly phosphate etc., can enumerate as its esters, the alkaline metal salt of sodium salt, potassium salt, calcium salt, magnesium salt etc., alkali earth metal salt.Particularly from the angle of the stability of compositions, the hydroxyl of 2 of preferred ascorbic acid or 3 by the derivant of Phosphation, more preferably magnesium salt, the sodium salt of ascorbic acid-2-phosphate.
(A) combined amount of ascorbic acid phosphoric acid esters or its salt is 0.1 ~ 5%(quality % of composition in its entirety, identical below.), particularly preferably 0.2 ~ 2%.The words of combined amount less than 0.1%, the situation of the effect of prevention parodontopathy can not be given full play to, more than 5%, the further improvement of the preventive effect of parodontopathy can not be expected again, in addition, having when being contained in mouth has the sense of discomfort producing abnormal flavour etc. to become the situation of large use sense difference.
(B) organic acid of composition or its salt are stabilizing agents as (A) composition and mixed, by with (C) composition and use, play the effect suppressing (A) ingredient breakdown, play the generation of the precipitation of inhibitory preparation simultaneously and manifest the effect of sense of discomfort.
As (B) composition, if the organic acid mixed in common composition for oral cavity is with regard to there is no particular limitation, but the binary of preferred tartaric acid, malic acid, succinic acid, glutamic acid, adipic acid, aspartic acid, citric acid etc. or tricarboxylic acid.In addition, as these salts, particular certain cancers, potassium salt etc.Wherein, from the discomposing effect suppressing (A) composition, suppress the effect of precipitation, the angle of sense of discomfort when not being contained in mouth is considered, particularly preferably tartaric acid, malic acid, succinic acid, citric acid or its salt, more preferably citric acid or its sodium salt.
Organic acid or its salt can independent a kind also can combine two or more mixing, its combined amount is 0.01 ~ 1% of composition in its entirety, particularly preferably 0.03 ~ 0.5%.Combined amount, less than 0.01%, suppresses the effect of (A) ingredient breakdown and suppresses the weak effect of precipitation, more than 1%, suppresses the effect of (A) ingredient breakdown to decline, has the sense of discomfort producing abnormal flavour etc. when being contained in become large situation further.
(C) orthophosphate of composition is mixed as the stabilizing agent of (A) composition, by with (B) composition and use, while playing the discomposing effect suppressing (A) composition, plays the generation of precipitation and the effect manifested of sense of discomfort of inhibitory preparation.
Can enumerate as orthophosphate, the normal salt of sodium phosphate, potassium phosphate, ammonium phosphate etc., sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium dihydrogen phosphate, the hydrogen salt of dipotassium hydrogen phosphate etc.Wherein, from the discomposing effect suppressing (A) composition, the angle of the effect of precipitation is suppressed to be set out, preferred hydrogen salt, more preferably sodium hydrogen phosphate.In addition, even use the chelating agen with the phosphate of such as pyrophosphate, Quadrafos etc. to replace orthophosphate, object of the present invention can not be reached.
The combined amount of orthophosphate is 0.01 ~ 1% of composition in its entirety, particularly preferably 0.03 ~ 0.5%.The words of combined amount less than 0.01%, there is the situation of the discomposing effect difference of suppression (A) composition, more than 1%, the decomposition inhibition of (A) composition and precipitation inhibiting effect decline, and have the sense of discomfort producing abnormal flavour etc. when being contained in mouth to become large situation further.
(B) mass ratio of mixed proportion (B) composition/(C) composition of composition and (C) composition is 0.1 ~ 5, particularly from the angle of the decomposition inhibition of (A) composition, precipitation inhibiting effect preferably 0.2 ~ 3.When mixed proportion is less than 0.1, or when more than 5, has and can not give full play to the decomposition inhibition of (A) composition and the situation of precipitation inhibiting effect.Particularly above-mentioned mixing ratio is effective for playing precipitation inhibiting effect fully.
Further, the ratio of ((B) composition+(C) composition)/(A) composition is 0.05 ~ 5 by quality ratio, particularly preferably 0.1 ~ 1, and from the angle improving the effect suppressing (A) ingredient breakdown, such ratio is suitable.When ratio is less than 0.05, or when more than 5, there is the situation of the effect that can not give full play to suppression (A) ingredient breakdown.
Solvent as the present composition generally mixes purified water.Water quantities more than 60% of composition in its entirety, preferably 75%, gratifying is less than 99.8%.Water quantities, less than 60%, feels stick-slip, sticky paste in oral cavity, in addition, because other solvents of alcohol etc. become large etc. for intraoral stimulation, have the probability that sense of discomfort when being contained in mouth becomes large.
The pH of compositions is 6.5 ~ 8.0(25 DEG C), more preferably 7.0 ~ 7.8.PH, less than 6.5, suppresses the effect of (A) ingredient breakdown to decline, more than 8.0, can not suppress precipitation fully, have the sense of discomfort of stick-slip, abnormal flavour etc. when being contained in mouth to become large probability further.
In addition, though the pH of compositions can develop into 6.5 ~ 8.0 voluntarily, pH adjusting agent also can be used as required to be adjusted to above-mentioned scope.As pH adjusting agent, the pH adjusting agent of sodium hydroxide, hydrochloric acid, sodium carbonate, sodium bicarbonate, boric acid or its salt etc. can be used, be wherein suitable for using sodium hydroxide, potassium hydroxide, hydrochloric acid.As long as the combined amount of these pH adjusting agents can by pH regulator in above-mentioned scope.
In liquid oral composition of the present invention, further, can mixed solvent, wetting agent etc. as required.The lower alcohol of the polyhydric alcohol, ethanol etc. of propylene glycol etc. can be mixed as solvent.The combined amount of these solvents is generally 0 ~ 30% of composition in its entirety, and particularly preferably 2 ~ 20%.
In addition, even if liquid oral composition of the present invention is in fact not containing ethanol (that is, the ethanol amount in compositions, below 0.01%, is in particular 0 ~ 0.0001%) composition, also effect of the present invention can be obtained.
Can enumerate as wetting agent, polyhydric alcohol, the sugar alcohol of Sorbitol, glycerol, ethylene glycol, Polyethylene Glycol, xylitol, erythritol etc.Combined amount is generally 0 ~ 20% of composition in its entirety.
Liquid oral composition of the present invention is not containing the liquid oral composition of grinding agent, can prepare and be applicable to the dosage form, particularly collutory of freshener, concentrated type collutory etc. in collutory, liquid dentifrice, the gel that cleans the teeth, mouth.As collutory, can be transparent or opaque, but the homogeneous liquid preferably not containing precipitate, float.In addition, according to its dosage form, the suitable known composition beyond mentioned component can be mixed as required.Such as, thickening agent, surfactant, antiseptic, sweeting agent, coloring agent, spice, effective ingredient etc. can also be mixed except above-mentioned solvent and wetting agent.
Can enumerate as thickening agent, sodium carboxymethyl cellulose, hydroxyethyl-cellulose etc.The combined amount of thickening agent is generally 0 ~ 5%, is in particular 0.1 ~ 3%.
Surfactant can use surfactant general in composition for oral cavity, and the combined amount of surfactant is usually in the scope of 0.1 ~ 10%.
Parabens etc. can be enumerated as antiseptic.Can enumerate as sweeting agent, saccharin sodium etc.Water colo(u)r can be enumerated as coloring agent.
The natural perfume material of Oleum Menthae Rotundifoliae, Herba Menthae wet goods can be used as spice, and the single synthetic perfume of carvone, anethole etc., also can use the well-known spice used in the dental care product of the compounding fragrances containing single synthetic perfume and/or person's natural perfume material etc. further, and not limit the spice recorded with embodiment.Usually its combined amount is in the scope of 0.00001 ~ 1%.
As effective ingredient, except the ascorbic acid phosphoric acid esters of (A) composition or its salt, in the scope not hindering effect of the present invention, the such as antiinflammatory, enzyme, fluorine compounds, antibacterial etc. of effective amount can be mixed with.
Embodiment
Below, illustrate the present invention with embodiment and comparative example, but the present invention is not limited to following embodiment.In following example, % understood, unless stated otherwise otherwise represent quality %.In addition, the pH in table uses the pH meter (model HM-30S) of East Asia electric wave industry system to measure immediately after preparation compositions, the value after representing 25 DEG C, 3 minutes.
(embodiment, comparative example)
With the liquid oral composition of composition shown in following method preparation table 1 ~ 3, obtain homogeneous liquid oral composition.The liquid oral composition obtained is transparent.With these liquid oral compositions of following method evaluation.Result is together shown in table 1 ~ 3.
(1) preparation method of liquid oral composition
In purified water 850g, mix ascorbic acid phosphoric acid esters class and other composition under room temperature, stir 1 hour until ascorbic acid phosphoric acid esters class is dissolved completely.When pH is not suitable for developing into voluntarily in the scope of 6.5 ~ 8.0, after using sodium hydroxide, hydrochloric acid etc. to regulate pH, regulate by purified water and make the total amount of compositions be 1,000g.In addition, add after sodium hydroxide and hydrochloric acid are prepared into 10% aqueous solution, make pH in above-mentioned scope.
(2) evaluation of the decomposition inhibition of (A) composition
250mL compositions is filled in the pet container of capacity 250mL, preserve at 60 DEG C and-5 DEG C after 1 month, with phosphate buffer (1.5mmol/L potassium dihydrogen phosphate, the 23.5mmol/L dipotassium hydrogen phosphate of 10mmol/L, pH8) dilute, filter, with high performance liquid chromatograph (pump: Japanese light splitting society PU1580, automatic sampler: (strain) Shimadzu Seisakusho Ltd. SIL-10A, UV detector: (strain) Shimadzu Seisakusho Ltd. SPD-6A, recording equipment: (strain) Shimadzu Seisakusho Ltd. C-R4A), carry out quantitatively with absolute calibration curve method.Movement is 25mmol/L potassium dihydrogen phosphate+5mmol/L tetrabutylammonium sulfate/acetonitrile=91/9 mixed solution (Capacity Ratio) mutually, chromatographic column is that diameter is about 4.6mm, be about the chromatographic column (example: TSK-gel ODS-80Ts(east Cao Zhushihui Co., Ltd. (East ソ ー (strain)) system) with the phase chromatography-use octadecylsilyl silicone filler of 5 μm in the stainless steel tube of 150mm), chromatogram column temperature about 50 DEG C, determined wavelength 240nm, flow velocity is 0.8mL/min.Calculate the concentration of the ascorbic acid phosphoric acid esters class in 60 DEG C of preservation product, remaining rate when to try to achieve with the amount in-5 DEG C of preservation product be 100%.
The decomposition of ascorbic acid phosphoric acid esters class suppresses metewand
◎: the remaining rate in compositions is more than 90%
Zero: the remaining rate in compositions is more than 80%, less than 90%
△: the remaining rate in compositions is more than 70%, less than 80%
×: the remaining rate in compositions is less than 70%
(3) evaluation of precipitation inhibiting effect
250mL compositions is filled in the pet container of capacity 250mL, preserves after 1 month at 60 DEG C, by precipitation when being slowly inverted pet container, compared with the pet container (reference substance) being filled with purified water, defer to the visual judgement of following benchmark.
Suppress the metewand of the effect of precipitation
◎: do not precipitate completely
Zero: the precipitation that can be seen a little, but no problem
△: obviously see precipitation
×: even if be not inverted pet container can see precipitation yet
(4) evaluation of sense of discomfort when not being contained in mouth
By 10 experimenters of oral mucosa allergy, in mouth, rinsing the mouth compositions is about 10mL, (congruent with embodiment 1 with reference substance, pH is regulated to be the composition of 9 by sodium hydroxide pH adjusting agent) compare the sense of discomfort that rinsing the mouth 20 seconds internal orifice intracavity feel, defer to following benchmark and carry out sense evaluation, try to achieve the following benchmark of meansigma methods and judge.
The metewand of sense of discomfort when not being contained in mouth
4: sense of discomfort is low significantly
3: sense of discomfort is low, be no problem degree
2: have equal sense of discomfort
1: feel significant sense of discomfort
Determinating reference
More than ◎: 3.5 points
More than zero: 3.0 point 3.5 points of deficiencies
More than △: 2.0 points 3.0 points of deficiencies
×: 2.0 points of deficiencies
Use raw material is specific as follows.
Phosphoric acid-L-AA magnesium: Wako Pure Chemical Industries, Ltd.'s biochemistry is used
Phosphoric acid-L-AA sodium: DSM Nutrition Japan(DSM ニ ュ ー ト リ シ ョ Application ジ ャ パ Application) Co., Ltd. trade name ス テ イ C50
Citric acid monohydrate compound: Fukawa Chemical Industries Co., Ltd.'s system, citric acid, exogenesis rule level (medicine part outer article raw material standard standard substance)
Citrate trisodium dihydrate: Fukawa Chemical Industries Co., Ltd.'s system, sodium citrate, exogenesis rule level
Malic acid disodium 0.5 hydrate: Kanto Kagaku K. K.'s system, superfine
Disodium succinate: Kanto Kagaku K. K.'s system, superfine
L-TARTARIC ACID: Kanto Kagaku K. K.'s system, superfine
Sodium hydrogen phosphate: peaceful Chemical Industries Co., Ltd. system, dibastic sodium phosphate, exogenesis rule level
Boric acid: Kanto Kagaku K. K.'s system, superfine (comparing product)
Carbonic acid: Kanto Kagaku K. K.'s system, superfine (comparing product)
Tetrasodium pyrophosphate: peaceful Chemical Industries Co., Ltd. system, exogenesis rule level (comparing product)
Polyphosphoric acid: peaceful Chemical Industries Co., Ltd. system, polyphosphate sodium, exogenesis rule level (comparing product)
Glycerol: Shi Wang KCC (ラ イ オ Application ケ ミ カ Le society) makes
Propylene glycol: Asahi Glass Co., Ltd's system
Sodium hydroxide: Kanto Kagaku K. K.'s system, sodium hydroxide, is diluted to 10% mixing by superfine
Hydrochloric acid: Kanto Kagaku K. K.'s system, hydrochloric acid, is diluted to 10% mixing by superfine
[table 1-1]
[table 1-2]
[table 2-1]
[table 2-2]
[table 3]
Claims (5)
1. a liquid oral composition, it is characterized in that, containing (A) ascorbic acid phosphoric acid esters or its salt 0.1 ~ 5 quality %, and not containing in the liquid oral composition of grinding agent, be mixed with (B) organic acid or its salt 0.01 ~ 1 quality % and (C) orthophosphate 0.01 ~ 1 quality %, and pH when 25 DEG C is 6.5 ~ 8.0, the water quantities in compositions is more than 60 quality %.
2. liquid oral composition as claimed in claim 1, wherein, mixed proportion (B)/(C) of (B) composition and (C) composition by quality ratio, is 0.1 ~ 5.
3. liquid oral composition as claimed in claim 1 or 2, wherein, (B) composition is more than a kind of being selected from citric acid, malic acid, tartaric acid, succinic acid and salt thereof.
4. the ascorbic acid phosphoric acid esters in a liquid oral composition or the stabilization method of its salt, it is characterized in that, containing (A) ascorbic acid phosphoric acid esters or its salt 0.1 ~ 5 quality %, and not containing in the described liquid oral composition of grinding agent, mixing (B) organic acid or its salt 0.01 ~ 1 quality % and (C) orthophosphate 0.01 ~ 1 quality %, pH when making 25 DEG C is 6.5 ~ 8.0, makes the water quantities in compositions be more than 60 quality %.
5. stabilization method as claimed in claim 4, wherein, mixed proportion (B)/(C) of (B) composition and (C) composition by quality ratio, is 0.1 ~ 5.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010-287028 | 2010-12-24 | ||
| JP2010287028A JP5691494B2 (en) | 2010-12-24 | 2010-12-24 | Liquid oral composition and method for stabilizing ascorbic acid phosphate or salt thereof in liquid oral composition |
| PCT/JP2011/076349 WO2012086341A1 (en) | 2010-12-24 | 2011-11-16 | Liquid oral composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103269676A CN103269676A (en) | 2013-08-28 |
| CN103269676B true CN103269676B (en) | 2015-07-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201180062456.5A Active CN103269676B (en) | 2010-12-24 | 2011-11-16 | Liquid oral composition |
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| Country | Link |
|---|---|
| JP (1) | JP5691494B2 (en) |
| KR (1) | KR101807905B1 (en) |
| CN (1) | CN103269676B (en) |
| MY (1) | MY162993A (en) |
| WO (1) | WO2012086341A1 (en) |
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|---|---|---|---|---|
| WO2013133096A1 (en) * | 2012-03-07 | 2013-09-12 | ライオン株式会社 | Oral composition |
| JP5880298B2 (en) * | 2012-06-13 | 2016-03-08 | ライオン株式会社 | Liquid oral composition |
| JP6118547B2 (en) * | 2012-12-10 | 2017-04-19 | 花王株式会社 | Oral composition |
| DE102013208865A1 (en) * | 2013-05-14 | 2014-11-20 | Beiersdorf Ag | Stabilized preparations containing ascorbic acid and phosphate ions |
| DE102014223570A1 (en) * | 2014-11-19 | 2016-05-19 | Beiersdorf Ag | Preparations containing ascorbic acid, ubidecarenone and phosphate ions for improved skin contouring or against cellulite |
| DE102014223568A1 (en) * | 2014-11-19 | 2016-05-19 | Beiersdorf Ag | Preparations containing ascorbic acid, ubidecarenone and mixtures of sodium stearoylglutamate and / or cetylstearylsulfate in combination with glycerylstearate |
| JP6435852B2 (en) * | 2014-12-24 | 2018-12-12 | ライオン株式会社 | Oral composition and method for preventing discoloration of oral composition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004026658A (en) * | 2002-06-21 | 2004-01-29 | Lion Corp | Composition for oral cavity |
| JP2005075825A (en) * | 2003-08-29 | 2005-03-24 | Lion Corp | Tooth-whitening oral composition |
| JP2006206581A (en) * | 2004-12-27 | 2006-08-10 | Lion Corp | Liquid composition for oral cavity |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6263597A (en) * | 1985-09-13 | 1987-03-20 | Nippon Saafuakutanto Kogyo Kk | Prevention of sediment of aqueous ascorbic acid phosphate magnesium solution |
| JP2000198723A (en) * | 1999-01-07 | 2000-07-18 | Lion Corp | Preparation compounded with ascorbic acid compound |
| JP3978605B2 (en) | 2003-04-30 | 2007-09-19 | ライオン株式会社 | Oral product and method for stably blending vitamin E or its derivative in oral product |
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2010
- 2010-12-24 JP JP2010287028A patent/JP5691494B2/en active Active
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- 2011-11-16 MY MYPI2013002191A patent/MY162993A/en unknown
- 2011-11-16 CN CN201180062456.5A patent/CN103269676B/en active Active
- 2011-11-16 WO PCT/JP2011/076349 patent/WO2012086341A1/en active Application Filing
- 2011-11-16 KR KR1020137015362A patent/KR101807905B1/en active IP Right Grant
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004026658A (en) * | 2002-06-21 | 2004-01-29 | Lion Corp | Composition for oral cavity |
| JP2005075825A (en) * | 2003-08-29 | 2005-03-24 | Lion Corp | Tooth-whitening oral composition |
| JP2006206581A (en) * | 2004-12-27 | 2006-08-10 | Lion Corp | Liquid composition for oral cavity |
Also Published As
| Publication number | Publication date |
|---|---|
| MY162993A (en) | 2017-07-31 |
| KR20130132858A (en) | 2013-12-05 |
| KR101807905B1 (en) | 2017-12-11 |
| CN103269676A (en) | 2013-08-28 |
| JP2012131755A (en) | 2012-07-12 |
| JP5691494B2 (en) | 2015-04-01 |
| WO2012086341A1 (en) | 2012-06-28 |
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