CN103998017B

CN103998017B - Dentrifice composition

Info

Publication number: CN103998017B
Application number: CN201280063091.2A
Authority: CN
Inventors: 阿部真里; 近泽贵士; 天野步
Original assignee: Lion Corp
Current assignee: Lion Corp
Priority date: 2011-12-20
Filing date: 2012-10-29
Publication date: 2017-04-12
Anticipated expiration: 2032-10-29
Also published as: KR20140113901A; PH12014501245A1; JPWO2013094312A1; CN103998017A; WO2013094312A1; JP6052185B2

Abstract

Provided is a dentrifice composition that stably contains an ascorbic acid phosphate ester or a salt thereof and provides a good sensation of cleaning. A dentrifice composition characterized by containing (B) a calcium-carbonate abrasive and (C) at least one compound selected from among hydrogen carbonate, orthophosphate, and condensed phosphate in (A) a dentrifice composition containing an ascorbic acid phosphate ester or a salt thereof. This dentrifice composition is further characterized in that the quotient of the mass of component (C) and the mass of component (B) is between 0.020 and 1.0, inclusive.

Description

Dentrifice composition

Technical field

The present invention relates to it is a kind of stably can allocate into ascorbic acid phosphoric acid esters or its salt with good cleaning the teeth using true feeling Agent compositionss.

Background technology

In recent years, ascorbic acid phosphoric acid esters or its salt, used as eliminating the biological excess activated oxygen for producing in vivo, protection is biological Organize from the antioxidant vitaminses of oxygen injury and attracted attention.Ascorbic acid phosphoric acid esters or its salt, with various physiologically actives, At (patent documentation 1) effective for the preventing/treating of gingivitiss, periodontitis known to the field of oral cavity, it is attempted and is mixed in toothpaste Or in the composition for oral cavity such as tablet.

However, when allocating ascorbic acid phosphoric acid esters or its salt in various compositionss into, can produce because of the metals such as calcium, micro- life Thing, impact of pH etc. and cause the survival rate of ascorbic acid phosphoric acid esters or its salt to decline, what its effectiveness cannot be fully demonstrated asks Topic, therefore stabilisation is the problem for needing to solve.

With regard to stabilized problem, for the composition for oral cavity for having allocated ascorbic acid phosphoric acid esters or its salt into discoloration or The problem that survival rate declines, it is proposed that by allocating the specific coloration inhibitor such as grinding agent and water-soluble phosphate into suppress long The technology (patent documentation 2) changed colour in phase preservation.Further it is proposed that the pH of the compositionss after preserving 1 month at 25 DEG C is located at 8.0, with first-class, keep the technology (patent documentation 3) of stability by the pH of compositionss is maintained alkaline side.Additionally, proposing By allocating appropriate abrasive silica into, stably allocating the technology (patent documentation of ascorbic acid phosphoric acid esters or its salt into 4)。

On the other hand, Dentrifice composition requires to pay its cleaning true feeling.The cleaning true feeling of Dentrifice composition, significantly Grinding agent species is depended on, wherein, if especially using Calcium Carbonate based abrasive, the cleaning true feeling of Dentrifice composition to carry Height, can obtain using the good compositionss of true feeling.

However, allocated the Dentrifice composition of ascorbic acid phosphoric acid esters or its salt into, particularly when allocating Calcium Carbonate system into Grinding agent then has the problem that the stability of ascorbic acid phosphoric acid esters or its salt is remarkably decreased, therefore does not almost grind Calcium Carbonate system Grinding agent is allocated into as main grinding agent.

Prior art literature

Patent documentation

Patent documentation 1：Japanese Patent Laid-Open 3-294227 publication

Patent documentation 2：Japanese Patent Laid-Open 4-173727 publication

Patent documentation 3：Japanese Patent Laid-Open 2002-20292 publication

Patent documentation 4：Japanese Patent Laid-Open 2003-212741 publication

The content of the invention

Invent problem to be solved

Therefore, the Calcium Carbonate based abrasive in Dentrifice composition to having allocated ascorbic acid phosphoric acid esters or its salt into is matched somebody with somebody In entering, the stablizing to allocate into of ascorbic acid phosphoric acid esters or its salt becomes problem.

The invention that the present invention is in view of the foregoing and makees, its objective is to provide and is allocating the clean of ascorbic acid or its salt into Calcium Carbonate based abrasive is allocated in tooth agent compositionss, stably can allocate into ascorbic acid phosphoric acid esters or its salt with good use The Dentrifice composition of true feeling.

The means to solve the problem

The present inventor is furtherd investigate repeatedly to reach above-mentioned purpose, is as a result found：By containing (A) Vitamin C In the Dentrifice composition of acid phosphoric acid ester or its salt, while (B) Calcium Carbonate based abrasive is allocated into, (C) is allocated into selected from carbonic acid The mass ratio of (C) composition/(B) composition is located at 0.020～1.0 by more than a kind in hydrogen salt, orthophosphate and condensed phosphate, It is able to ensure that the stability of ascorbic acid phosphoric acid esters or its salt and can pays and well uses true feeling.It moreover has been found that height can be obtained Convergence sense, is improved using true feeling.

I.e., it was found that if in the Dentrifice composition containing ascorbic acid phosphoric acid esters or its salt (below, being slightly designated as APE) In allocate Calcium Carbonate based abrasive into, then the calcium ion of APE and Calcium Carbonate, particularly divalent metal ion interacts, and produces APE The problem that declines of stability, and if relative to Calcium Carbonate based abrasive, allocated into selected from bicarbonate, positive phosphorus with special ratios The salt of more than a kind in hydrochlorate, condensed phosphate, then unexpectedly solve the problem being related to, comprising Calcium Carbonate based abrasive System in the time passage can stably allocate APE into, pay above-mentioned special action effect.

In addition, having recorded in patent documentation 2 comprising magnesium ascorbyl phosphate, Calcium Carbonate has been allocated into as grinding agent, And allocated phosphate, citrate into as the composition of coloration inhibitor, but its be suppress because allocating ascorbic acid derivates into and The constituent of the coloring of generation, it is unpredictable due to using bicarbonate of the invention, orthophosphate or contracting from the patent documentation 2 The APE stabilisations in Calcium Carbonate based abrasive proportioning composition closed phosphate and obtain and special action effect.

Therefore, the present invention provides following Dentrifice compositions.

(I) a kind of Dentrifice composition, it is characterised in that in the dentifrice containing (A) ascorbic acid phosphoric acid esters or its salt In compositionss, while (B) Calcium Carbonate based abrasive is allocated into, (C) is allocated into selected from bicarbonate, orthophosphate and condensed phosphoric acid More than a kind in salt, (C) mass ratio of composition/(B) composition is 0.020～1.0.

(II) a kind of Dentrifice composition, it is characterised in that in the dentifrice containing (A) ascorbic acid phosphoric acid esters or its salt In compositionss, while (B) Calcium Carbonate based abrasive is allocated into, (C) sodium bicarbonate is allocated into, (C) quality of composition/(B) composition Than for 0.020～1.0.

The effect of invention

According to the present invention it is possible to provide allocate Calcium Carbonate system in the Dentrifice composition of ascorbic acid or its salt has been allocated into Grinding agent, can stably allocate ascorbic acid phosphoric acid esters or its salt into and with the Dentrifice composition for using true feeling well.This Outward, the Dentrifice composition pays high convergence sense, excellent using the cleaning true feeling after neutralization use.

Specific embodiment

Below, the present invention is further described in detail.The Dentrifice composition of the present invention, containing (A) Vitamin C Acid phosphoric acid ester or its salt, (B) Calcium Carbonate based abrasive and a kind in bicarbonate, orthophosphate and condensed phosphate of (C) More than.

As (A) ascorbic acid phosphoric acid esters or its salt, it is 1 of the hydroxyl of any one in 2,3,5,6 of ascorbic acid Individual or more than 2 esters for becoming the compounds such as phosphoric acid, polyphosphoric acids, for example, can enumerate ascorbic acid-2-phosphate, Vitamin C Acid -3- phosphate esters, ascorbic acid -6- phosphate esters, ascorbic acid -2- condensed phosphates etc., as its esters, can enumerate sodium salt, The alkali metal salts such as potassium salt, calcium salt, magnesium salt, alkali salt.Especially as the oral cavity material for using, from the pre- preventive effect of gingivitiss From the point of view of in terms of fruit, suitably from the magnesium salt or sodium salt of ascorbic acid phosphoric acid esters.

(A) proportional quantity of ascorbic acid phosphoric acid esters or its salt preferably constitutes 0.1～2% overall (quality %, similarly hereinafter), More preferably 0.2～1%.Although proportional quantity is more, the proportioning effect of the ascorbic acid phosphoric acid esters such as gingivitiss preventive effect or its salt Fruit is more improved, but if more than 2%, then can not only expect higher effect, and have the feelings for producing that abnormal flavour use feeling declines Condition.

As (B) Calcium Carbonate based abrasive, although as long as the material with abrasiveness then precipitated calcium carbonate, heavy carbonic acid Any one of calcium can, but particularly preferably ground calcium carbonate.

As Calcium Carbonate based abrasive, it is, for example possible to use Co., Ltd. C alfine (Co., Ltd. カ Le Off ァイ Application) The commercially available products such as the trade name Calfine KS-1000RS of manufacture.

In the present composition, Calcium Carbonate based abrasive is allocated into as main grinding agent.

(B) proportional quantity of Calcium Carbonate based abrasive, preferably constitutes overall 5～40%, and more preferably 10～25%.Though So the more cleaning true feelings of proportional quantity are more improved, but if more than 40%, then have cannot stablize proportioning ascorbic acid phosphoric acid esters or its The situation of salt.Additionally, if it exceeds 40%, then have that abrasive power is too strong, the situation that use feeling is poor.

(C) composition is the salt of more than a kind in bicarbonate, orthophosphate and condensed phosphate, used as Vitamin C The stabilized preparations of acid phosphoric acid ester or its salt are allocated into.

As the salt of (C) composition, bicarbonate, phosphate, hydrophosphate, pyrophosphate, polyphosphate etc. can be enumerated, The alkali metal salt such as salt, preferably sodium salt, potassium salt.Specifically, sodium bicarbonate can be enumerated as bicarbonate, can as orthophosphate Sodium phosphate, dibastic sodium phosphate are enumerated, sodium polyphosphate, sodium pyrophosphate, potassium pyrophosphate etc. can be enumerated as condensed phosphate.These can To be used alone a kind, or from from the aspect of embodying effect, it is also possible to which two or more is applied in combination.

Sodium bicarbonate is sodium bicarbonate, also referred to as bicarb of soda.Sodium bicarbonate, for example, can use and be sold by Asahi Glass Co., Ltd The trade name sold is the commercially available products such as sodium bicarbonate.

Orthophosphate, condensed phosphate can also use commercially available product.Specifically, it is possible to use by peaceful Chemical Industries strain formula Disodium hydrogen phosphate or tertiary sodium phosphate, sodium polyphosphate, tetrasodium pyrophosphate, four potassium of polyphosphoric acids of commercial firm's sale etc..

Used as (C) composition, especially sodium bicarbonate effect is more excellent, and cleaning true feeling is excellent, therefore suitably.

(C) proportional quantity of composition, preferably constitutes overall 0.5～10%, and more preferably 1～5%.Proportional quantity is not enough When 0.5%, there is the situation of the stabilization effect variation of ascorbic acid phosphoric acid esters or its salt, if it exceeds 10%, then there is saline taste pair Use feeling produces dysgenic situation.

In the present invention, (C) composition is allocated in appropriate proportions into relative to (B) Calcium Carbonate, for stably allocating ascorbic acid phosphorus into Acid esters or its salt are important.

(B), the ratio of (C) composition be (C) composition/(B) composition mass ratio be 0.020～1.0, preferably 0.03 ～0.5, more preferably 0.05～0.3.If ratio is less than 0.020, ascorbic acid phosphoric acid esters or its salt cannot be made steady Fixedization.If it exceeds 1.0, then do not simply fail to make ascorbic acid phosphoric acid esters or which is salt-stabilized, and use feeling is deteriorated.

The Dentrifice composition of the present invention, can be prepared into toothpaste, liquid dentifrice, wet-milling dentifrice etc., particularly suitably For toothpaste.Additionally, the present composition, in the range of the effect for not damaging the present invention, according to dosage form can allocate into it is above-mentioned into Known additive beyond point.For example, the usual grinding agent allocated in Dentrifice composition, binding agent, thickening can be allocated into Agent, surfactant, further can allocate into as needed sweeting agent, preservative, spice, dye, preserving stabilizer, drug effect into Grade.

As grinding agent, in addition to above-mentioned Calcium Carbonate based abrasive, can be not damaging in the range of effect of the present invention Allocate other grinding agents being usually used into.For example, (mean diameter is 1～30 μ with calcium hydrogen phosphate can to enumerate cleaning the teeth of generally using M or so), abrasive silica, calcium pyrophosphate, aluminium hydroxide, aluminium oxide, magnesium carbonate, tricresyl phosphate magnesium, insoluble Metaphosphoric acid Sodium, insoluble potassium metaphosphate, titanium oxide, synthetic resin based abrasive etc..

When allocating above-mentioned other grinding agents into, it is desirable to not reduce the model of the stability of ascorbic acid phosphoric acid esters or its salt Enclose, its proportional quantity is to constitute overall less than 5%, particularly preferred 0～3%.

As binding agent, xanthan gum, sodium polyacrylate, carrageenan, sodium alginate, propylene glycol alginate, carboxyl can be enumerated Polyvinyl, Tragacanth, guar gum, hydroxypropyl guar gum, tara gum, locust bean gum, karaya, Fructus cydoniae oblongae seeds Glue, tamarind gum, sodium carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, methyl are fine Dimension element, cellulose, gellan gum, gelatin, curdlan, arabic gum, agar, pectin, sodium caseinate, polyvinyl alcohol, grow sturdily it is mould Polysaccharide, tackifying silicon dioxide, VEEGUM (aluminium-magnesium silicate), montmorillonite, hectorite, montmorillonite, bentonite etc..Proportional quantity is usual For the 0.01～8% of composition entirety.

As thickening agent, it is possible to use glycerol, Sorbitol, Propylene Glycol, the Polyethylene Glycol of molecular weight 200～6000,1, 1 kind of the polyhydric alcohol such as 3- butanediols, xylitol, maltose alcohol, lactose, erythritol, palatinose, trehalose and sugar alcohol etc. with On.Proportional quantity usually constitutes overall 5～50%.

As surfactant, anionic surfactant, cationic surface active agent, nonionic can be allocated into Surfactant, amphoteric surfactant, it is particularly suitable using selected from anionic surfactant, non-ionic surface work More than a kind in property agent, amphoteric surfactant.For example, as anionic surfactant, sodium lauryl sulfate can be enumerated Deng the acyl sarcosinates such as alkyl sulfate or its salt, sodium N-lauroyl sarcosinate, alpha-alkene sulfonate etc., as cationic Surfactant, can enumerate alkylammonium, benzyl o ammonium salt etc., as nonionic surfactant, can enumerate polyoxy second Alkene castor oil hydrogenated, polyoxyethylene alkyl ether, poloxalkol, alkyl androstanediol, sucrose fatty acid ester, mountain Pears sugar alcohol acid anhydride fatty acid ester etc., as amphoteric surfactant, can enumerate imidazolinium betaine etc..The proportional quantity of surfactant Overall 0.2～15% constituted preferably generally, particularly preferably 0.5～10%.

As sweetening material, saccharin sodium, stevioside, Flos Chrysanthemi extract, glycyrrhizin, perillartine, Talin, new can be allocated into Hesperidin hydrogenation chalcone, p-met hoxycinnamic aldehyde, aspartyl-phenylalanine methyl ester, acesulfame potassium, sucralose, sugarcane Sugar, glucose, dextrin, Nulomoline, Fructose, xylitol, erythritol, Sorbitol, mannitol, maltose alcohol, lactose, Palatinose, isomalt (Palatinit), trehalose, oligosaccharide, reductive water maltosemalt sugar, aspartame etc..

As preservative, methyl parahydroxybenzoate, butyl p-hydroxybenzoate, ethylparaben etc. can be enumerated Parabenses, benzoic acid or its salt, salicylic acid or its ester or salt, cetylpyridinium chloride, isopropyl methyl phenol, sorbic acid Salt etc..

Spice can use Oleum menthae, Oleum Menthae Rotundifoliae, Oleum Anisi Stellati, eucalyptus oil, wintergreen oil, Oleum Cinnamomi, Oleum Caryophylli, hundred inner grass Oil, sage oil, Fructus Citri Limoniae oil, orange oil, Oleum menthae (Ha ッカ are oily), cardamom oil, Fructus Coriandri oil, mandarin oil, lime oil, Essential lavender oil, Oil of rosemary, laurel fat, Flos Matricariae chamomillae oil, caraway oil, Majorana hortensis oil, cassia oil, Indian oil of verbena, Herba Origani oil, pinke needle oil, orange blossom The natural perfume materials such as oil, Oleum Rosae Rugosae, Jasmin oil, Rhizoma Iridis Tectori flower essential oil, Herba Menthae absolute oil, moss rose, orange blossom；These natural perfume materials are added The spice that work process (except head fraction, except tails, fractional distillation, liquid-liquid extraction, refine, spice powdered etc.) is obtained；Menthol, perfume (or spice) Celery ketone, anethole, cineole, methyl salicylate, cinnamic aldehyde, eugenol, 3-L- menthoxypropane -1,2- glycol, thymol, Linalool, linalyl acetate, limonenes, menthone, menthyl acetate, N- replace-to terpane -3- Methanamides, pinene, octanal, Citral, pulegone, carvacryl acetate, anisaldehyde, ethyl acetate, ethyl n-butyrate., allyl cyclohexyl propionate, adjacent aminobenzene Methyl formate, ethyl methylphenylglycidate, vanillin, 11 carbon lactones, hexanal, propanol, butanol, isoamyl alcohol, hexenol, Dimethyl sulfide, methyl cyclopentenyl ketone, furfural, trimethylpyrazine, ethyl lactate, methyl lactate, ethyl thioacetate etc. are single Product spice；Further, strawberry flavor, apple aroma, banana flavor, Fructus Ananadis comosi taste, grape flavor, Fructus Mangifera Indicae taste, butter taste, milk taste, fruit are mixed Close the known spice raw material that taste, tropical fruit (tree) taste etc. reconcile used in the Dentrifice compositions such as spice.

In addition, although there is no particular limitation for proportional quantity, but preferably above-mentioned spice raw material is using in preparation composition 0.000001～1%.Additionally, as the tax perfume (or spice) spice for having used above-mentioned spice raw material, preferably making in preparation composition With 0.1～2.0%.

As coloring agent, Amaranth, red No. 3, yellow 4, Sunset Yellow FCF, blue No. 1, blue No. 2, green can be enumerated The legal pigments such as No. 3, carthamin, gardenin, cochineal red pigment, annatto pigment, mica titanium, titanium oxide, iron oxide red Deng.

As preserving stabilizer, can enumerate vitamin C, Vitamin E, sodium sulfite, sodium pyrosulfite, sodium sulfite, Butylated hydroxytoluene, propylgallate, butylhydroxy aryl ester etc..

As effective ingredient, in addition to (A) ascorbic acid phosphoric acid esters or its salt, can be in the effect of the without prejudice to present invention In the range of, allocate other effective ingredient into, such as isopropyl methyl phenol, triclosan, cetylpyridinium chloride, benzethonium chloride, benzene are pricked The antibacterial such as oronain, dequalinium chloride, chlorhexidine hydrochloride, chlorhexidine gluconate, dodecyl diamino ethyl glycine, fluorination The antifibrin solvents such as the fluorine compounds such as sodium, single sodium monofluorophosphate, stannic fluoride, tranexamic acid, episilon amino caproic acid, Vitamin C Ascorbic acid derivates, tocopherol and its derivant, riboflavin, pyridoxine hydrochloride, cobalamin, β-Hu beyond acid, (A) composition Vitamin such as Radix Raphani element, ergocalciferol, menadione, ubiquinone etc., glycyrrhetate, enoxolone, allantoin class, Cortex Phellodendri, Rhizoma Coptidis, Herba Rosmarini Officinalis, Flos Caryophylli, Salvia japonica Thunb., Herba thymi vulgariss, Radix Scutellariae, Radix Angelicae Sinensis, Radix Hamamelidis Molliss, Folium Eriobotryae, green tea, Semen Ginkgo, Mespilus germinica Linn, Flos lupuli (Flos Humuli Lupuli), Elm, Herba Hyperici Erecti, oolong tea, tilia, catechu, Flos rosae multiflorae, Herba Houttuyniae, Herba Equiseti Arvinsiss, black tea, Radix Paeoniae, Betula platyphylla Suk., Fructus Crataegi, Aesculus hippocastanum L., The plant extracts such as Radix Malvae sylvestriss, glucanase, change dextranase, lysozyme, proteolytic enzyme, lyase, superoxide dismutase etc. Enzyme, potassium nitrate, gamma oryzanol, dihydro cholesterol, α-bisabolol, azulene, methoxy-ethylene, copolymer-maleic anhydride, trichlorine carbon Anilid, alanine, glycine, proline, L-Arginine, L-Aspartic acid sodium, trimethyl glycine, copper chlorophyllin Sodium, copper gluconate, zinc chloride, zinc citrate, zeolite, aluctyl. etc..

Although the pH of the present composition is not particularly limited, in terms of the stability of ascorbic acid phosphoric acid esters or its salt Consider, the pH in preferably 25 DEG C is more than 8, particularly preferably 8.0～9.3 scope.

The container of the Dentrifice composition of the filling present invention is not particularly limited, it is possible to use be generally used for dentifrice composition The container of thing.Specifically, can be using plastic containers such as polyethylene, polypropylene, polyethylene terephthalate, nylon etc..

Embodiment

Hereinafter, as shown in embodiment and comparative example, Formulation Example, specifically the present invention will be described, but the present invention is not It is limited to following embodiments.In addition, in following examples, % is quality % when being not particularly limited.

[embodiment, comparative example]

Shown in table 1～3, the Dentrifice composition of component is prepared according to following manufacture methods, and with following method evaluations. As a result as shown in table 1～3.

The manufacture method of 1 ＞ Dentrifice compositions of ＜

(1) water soluble ingredient (in addition to binding agent, Propylene Glycol) mixed dissolution, in purified water, is prepared into into A under room temperature Phase.

(2) binding agent is distributed in Propylene Glycol under room temperature, is prepared into B phases.

(3) B phases are added in the A phases being mixed in stirring, is prepared into C phases.

(4) under room temperature, using 1.5L kneader (tor work manufactured) will except the water soluble ingredients such as spice, grinding agent with Outer composition is mixed in C phases, and by reducing pressure, (5.3kPa) carries out deaeration, obtains Dentrifice composition 1.2kg.

Dentrifice composition 60g fabricated as described above is filled in and is formed for straight-chain Low Density Polyethylene by innermost layer Diameter 26mm, laminated tube (the white LDPE60/EMAA20/AL10/EMAA30/ of LDPE55/PET12/LDPE20/ of bore 8mm LDPE20/LLDPE30,257 μm of thickness (Janpanese Printing Co., Ltd's manufacture)) in, at 25 DEG C, determine dispensing and hold in 20ml PH (analyzers in the plastic containers of amount after 3 minutes：Prunus mume (sieb.) sieb.et zucc. Teller-support benefit Co., Ltd. manufacture, MP220, electrode：Prunus mume (sieb.) sieb.et zucc. Teller- The manufacture of support benefit Co., Ltd., InLab410).

Dummy suffix notation and title in the Rotating fields of the laminated tube for using is as follows, the digital table closelyed follow after dummy suffix notation Show the thickness (μm) of each layer.

LDPE：Low Density Polyethylene

White LDPE：White low density polyethylene

LLDPE：Straight-chain Low Density Polyethylene

AL：Aluminum

PET：Polyethylene terephthalate

EMAA：The copolymer resin of ethylene methacrylic acid

The stability of 2 ＞ ascorbic acid phosphoric acid esters salt of ＜

The preservation of the ascorbic acid phosphoric acid esters salt after Dentrifice composition is preserved 3 months at 40 DEG C is evaluated with following methods Stability.- 5 DEG C of preservation product are used as Undec reference substance.

Ascorbic acid phosphoric acid esters salt it is quantitative：

The each Dentrifice compositions of 0.1g are weighed, phosphate buffer solution (the 1.5mmol/L biphosphates of 10mmol/L are added Potassium, 23.5mmol/L dipotassium hydrogen phosphates, pH8.0), with shaker high degree of agitation 20 minutes afterwards, it is settled to 10ml.Take the liquid 1ml, after being filtered with pre-treatment filter, using high performance liquid chromatograph (pump：Japan Spectroscopy Corporation's manufacture PU1580, automatic sampler：The SIL-10A of Shimadzu Scisakusho Ltd's manufacture, UV detectors：Shimadzu Scisakusho Ltd The SPD-6A of manufacture, recording equipment：The C-R4A of Shimadzu Scisakusho Ltd's manufacture), it is fixed to be carried out with absolute standard curve method Amount.Mixed solution (capacity of the mobile phase for 25mmol/L potassium dihydrogen phosphates+5mmol/L TBuAs/acetonitrile=91/9 is set Than), chromatographic column is diameter about 4.6mm, fills 5 μm of chromatograph of liquid with 18 in the stainless steel tube of length about 150mm The chromatographic column of alkyl silane bonded silica gel is (for example：TSK-gel ODS-80Ts (TOSOH Co., Ltd's manufacture)), chromatogram column temperature About 40 DEG C, Detection wavelength is 240nm, and flow velocity is 0.8ml/ point, about 7 points of the retention time of ascorbic acid phosphoric acid esters salt Clock.The content of ascorbic acid phosphoric acid esters salt in the preservation product for preserve at 40 DEG C 3 months is calculated, and obtains 3 to be preserved at -5 DEG C The survival rate when content of ascorbic acid phosphoric acid esters salt is 100% in the preservation product of the moon.

Scoring：

◎：Survival rate is more than 95%

○：Survival rate is more than 90% and less than 95%

△：Survival rate is more than 80% and less than 90%

×：Survival rate is less than 80%

3 ＞ of ＜ restrain the evaluation of effect

With regard to Dentrifice composition, the sensory test that member implements convergence sense is tested with 10 people panels of expert.By preparation 1g Being placed on commercially available product toothbrush carries out 3 minutes brushing teeth, and is evaluated according to following scoring using the convergence sense after neutralization use.Obtain The meansigma methodss of 10 people's evaluation results, will be confirmed as the preparation of the evaluation of zero, ◎ by following standard, be judged as restraining high clean of effect Tooth agent compositionss.

Scoring

3 points：Feel convergence effect

2 points：Feel slightly convergence effect

1 point：Complete imperceptible convergence effect

Evaluation criterion

◎：More than 2.5 points

○：More than 2.0 points and less than 2.5 points

△：More than 1.3 points and less than 2.0 points

×：Less than 1.3 points

[table 1]

[table 2]

[table 3]

The details of raw material used is as described below.

(1) APM：

Wako Pure Chemical Industries, Ltd. manufactures, biochemical to use

(2) Calcium Carbonate：Co., Ltd. C's alfine metric systems are made,

Calcium Carbonate based abrasive, trade name Calfine KS-1000RS

(3) sodium bicarbonate：Asahi Glass Co., Ltd manufactures, trade name sodium bicarbonate

Tertiary sodium phosphate：Peaceful Chemical Industries Co., Ltd. manufacture, trade name tertiary sodium phosphate

Disodium hydrogen phosphate：Peaceful Chemical Industries Co., Ltd. manufacture, trade name disodium hydrogen phosphate

Sodium polyphosphate：Peaceful Chemical Industries Co., Ltd. manufacture, trade name sodium tripolyphosphate

Tetrasodium pyrophosphate：Peaceful Chemical Industries Co., Ltd. manufacture, trade name sodium pyrophosphate

Four potassium of polyphosphoric acids：Peaceful Chemical Industries Co., Ltd. manufacture, trade name potassium polyphosphate

Can be seen from the result of table 1～3, when lacking (C) composition, (comparative example 2) and (B), the ratio of (C) composition are inappropriate When, the stability of ascorbic acid phosphoric acid esters salt is poor, on the other hand, (B), the present invention that allocates in appropriate proportions of (C) composition it is clean Tooth agent compositionss (embodiment 1～16), ascorbic acid phosphoric acid esters salt stably can be allocated into, additionally, convergence excellent effect.

With the Dentrifice composition that following Formulation Example is prepared as with above-mentioned identical raw material, and evaluated.Respectively The Dentrifice composition of example, is the excellent in stability of ascorbic acid phosphoric acid esters salt, high using the convergence sense after neutralization use, pays With the good Dentrifice composition using true feeling.

[Formulation Example 1] toothpaste (pH8.18)

(C) mass ratio ((C)/(B))=0.10 of composition and (B) composition

[Formulation Example 2] toothpaste (pH8.11)

(C) mass ratio ((C)/(B))=0.13 of composition and (B) composition

[Formulation Example 3] toothpaste (pH8.03)

(C) mass ratio ((C)/(B))=0.15 of composition and (B) composition

[Formulation Example 4] toothpaste (pH8.10)

(C) mass ratio ((C)/(B))=0.10 of composition and (B) composition

[Formulation Example 5] toothpaste (pH8.06)

(C) mass ratio ((C)/(B))=0.13 of composition and (B) composition

[Formulation Example 6] toothpaste (pH8.12)

(C) mass ratio ((C)/(B))=0.53 of composition and (B) composition

[Formulation Example 7] toothpaste (pH8.19)

(C) mass ratio ((C)/(B))=0.05 of composition and (B) composition

[Formulation Example 8] toothpaste (pH8.12)

(C) mass ratio ((C)/(B))=0.2 of composition and (B) composition

[Formulation Example 9] toothpaste (pH8.11)

(C) mass ratio ((C)/(B))=0.10 of composition and (B) composition

[Formulation Example 10] toothpaste (pH8.19)

(C) mass ratio ((C)/(B))=0.06 of composition and (B) composition

Claims

1. a kind of Dentrifice composition, it is characterised in that in the Dentrifice composition containing (A) ascorbic acid phosphoric acid esters or its salt In, while allocating (B) Calcium Carbonate based abrasive into, allocate (C) a kind in bicarbonate, phosphate and hydrophosphate into On, (C) mass ratio of composition/(B) composition is 0.020～1.0, and (B) proportional quantity of composition is 5～25 mass %.

2. Dentrifice composition as claimed in claim 1, wherein, (C) composition is sodium bicarbonate.

3. Dentrifice composition as claimed in claim 1 or 2, wherein, (C) proportional quantity of composition is 0.5～10 mass %.

4. Dentrifice composition as claimed in claim 1 or 2, wherein, (A) proportional quantity of composition is 0.1～2 mass %.

5. Dentrifice composition as claimed in claim 1 or 2, wherein, further allocate into beyond (B) Calcium Carbonate based abrasive 0～3 mass % of grinding agent, 0.01～8 mass % of binding agent, 5～50 mass % of thickening agent, 0.2～15 matter of surfactant Amount %, makes toothpaste.