EP4243759A1 - Bleichende mundpflegezusammensetzungen - Google Patents

Bleichende mundpflegezusammensetzungen

Info

Publication number
EP4243759A1
EP4243759A1 EP21802236.6A EP21802236A EP4243759A1 EP 4243759 A1 EP4243759 A1 EP 4243759A1 EP 21802236 A EP21802236 A EP 21802236A EP 4243759 A1 EP4243759 A1 EP 4243759A1
Authority
EP
European Patent Office
Prior art keywords
silica
surface area
precipitated silica
oral care
peroxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP21802236.6A
Other languages
English (en)
French (fr)
Inventor
M. Cédric FERAL-MARTIN
Caroline FAYOLLE
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rhodia Operations SAS
Original Assignee
Rhodia Operations SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rhodia Operations SAS filed Critical Rhodia Operations SAS
Publication of EP4243759A1 publication Critical patent/EP4243759A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • 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
    • A61K8/25—Silicon; Compounds thereof
    • 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

Definitions

  • the present invention relates to precipitated silica suitable for the use in whitening oral care compositions having improved stability over time.
  • compositions described in the art for preventing or treating the discoloration of teeth There are a variety of compositions described in the art for preventing or treating the discoloration of teeth.
  • the materials most commonly used in teeth whitening today are peroxides. Peroxides are generally deemed safe from a physiological standpoint, and can be effective to whiten teeth.
  • Oral care compositions comprising peroxides or peroxide-releasing compounds are known.
  • One drawback of the use of peroxides is their high reactivity, which leads to decomposition of the peroxide during storage hence to lower whitening activity of the composition.
  • precipitated silica in the formulation may induce the decomposition of peroxide or peroxidereleasing compounds.
  • Precipitated silica is used extensively in oral care formulations as abrasive and/or thickening agent.
  • precipitated silica abrasives provide controlled mechanical cleaning, plaque removal and polishing of teeth.
  • Such silica abrasives are known to interact not only with peroxide or peroxide-releasing compound but also with other active ingredients of the compositions, such as certain antimicrobial agents, fluorides and zinc compounds. Such interactions have the consequence that these active ingredients are no longer available to elicit their beneficial effects.
  • compositions comprising a peroxide or peroxide-releasing compound and precipitated silica, characterised by a reduced decomposition of the peroxide or peroxide-releasing compound, hence by a longer shelf-life.
  • Object of the invention is a precipitated silica characterised by:
  • silic is used herein to refer to silicon dioxide, SiO .
  • sica is used throughout the text to refer to precipitated silica.
  • precipitated silica is used to refer to a synthetic amorphous silica obtained by a process wherein a silicate is reacted with an acid causing the precipitation of SiO .
  • the inventive silica is characterised by a number of OH groups per surface area, expressed as number of OH/nm 2 , which is equal to or lower than 2.00 OH/nm 2 , even less than 1.50 OH/nm 2 , preferably less than 1.00 OH/nm 2 .
  • the number of OH groups per surface area is typically equal to or greater than 0.05 OH/nm 2 , even equal to or greater than 0.10 OH/nm 2 , preferably equal to or greater than 0.20 OH/nm 2 .
  • the inventive silica is advantageously characterised by a number of OH groups per surface area of 0.10 to 2.00 OH/nm 2 , preferably of 0.15 to 1.00 OH/nm 2 , more preferably of 0.15 to 1.00 OH/nm 2 .
  • silanol density i.e. the number of OH groups per surface area
  • the CTAB surface area SCTAB is at least 5 m 2 /g, typically at least 10 m 2 /g.
  • the CTAB surface area SCTAB may be greater than 15 m 2 /g.
  • the CTAB surface area does not exceed 45 m 2 /g, the CTAB surface area is preferably lower than 42 m 2 /g, even lower than 40 m 2 /g.
  • CTAB surface area SCTAB are from 15 to 42 m 2 /g, preferably from 15 to 40 m 2 /g.
  • the CTAB surface area is a measure of the external specific surface area as determined by measuring the quantity of N-hexadecyl-N,N,N- trimethylammonium bromide adsorbed on the silica surface at a given pH.
  • the CTAB surface area can be determined according to the standard NF ISO 5794-1 , Appendix G (June 2010).
  • the BET surface area SBET of the inventive silica is not particularly limited but it is at least 5 m 2 /g, typically at least 10 m 2 /g.
  • BET surface area SBET may in certain instances be greater than 15 m 2 /g, even greater than 20 m 2 /g.
  • BET surface area SBET is generally at most 60 m 2 /g.
  • the BET surface area may advantageously be from 5 to 50 m 2 /g, even from 10 to 45 m 2 /g, preferably from 15 to 45 m 2 /g.
  • the BET surface area is determined according to the Brunauer - Emmett - Teller method described in The Journal of the American Chemical Society, Vol. 60, page 309, February 1938, and corresponding to the standard NF ISO 5794-1 , Appendix D (June 2010).
  • the inventive silica is characterised by a good balance of abrasive properties, that is ability to remove the pellicle deposit of the teeth without damaging the enamel.
  • the silica is characterised by an abrasion depth value Hm, as determined using the PMMA abrasion test described hereafter, between 3.5 and 25.0 pm, even between 3.5 and 20.0 pm, preferably between 4.0 and 18.0 pm, more preferably between 4.0 and 15.0 pm.
  • the silica is further characterised by a Relative Dentin Abrasion (RDA), determined according to the method detailed hereafter, between 100 and 200, typically between 120 and 190.
  • RDA Relative Dentin Abrasion
  • the second object of the invention is an oral care composition comprising a peroxide-releasing compound and the precipitated silica which is the first object of the invention, that is a precipitated silica characterised by:
  • peroxide-releasing compound is used herein to refer to hydrogen peroxide, peroxides as well as any compound capable to release hydrogen peroxide under the conditions of use in an oral care application.
  • peroxide-releasing compounds are include hydroperoxides, hydrogen peroxide, peroxides of alkali and alkaline earth metals, organic peroxy compounds, peroxy acids, pharmaceutically-acceptable salts thereof, and mixtures thereof.
  • Peroxides of alkali and alkaline earth metals include lithium peroxide, potassium peroxide, sodium peroxide, magnesium peroxide, calcium peroxide, barium peroxide, and mixtures thereof.
  • Organic peroxy compounds include urea peroxide, glyceryl hydrogen peroxide, alkyl hydrogen peroxides, dialkyl peroxides, alkyl peroxy acids, peroxy esters, diacyl peroxides, benzoyl peroxide, and monoperoxyphthalate, and mixtures thereof.
  • Peroxy acids and their salts include organic peroxy acids such as alkyl peroxy acids, and monoperoxyphthalate and mixtures thereof, as well as inorganic peroxy acid salts such as and perborate salts of alkali and alkaline earth metals such as lithium, potassium, sodium, magnesium, calcium and barium, and mixtures thereof.
  • Preferred solid peroxides are sodium perborate, urea peroxide, and mixtures thereof.
  • the peroxide-releasing compound may be bound to a polymer such as polymers of poly(vinylpyrrolidone), polyacrylates, polymethacrylates.
  • the oral care composition typically contains from 1 to 50%, typically from 3 to 40%, preferably from 3 to 20 % by weight of the peroxide-releasing compound.
  • the oral care composition contains from 3 to 60%, typically from 5 to 50%, preferably from 5 to 30 % by weight of the inventive silica.
  • composition of the invention may include other ingredients commonly used in oral care applications, in particular other water-insoluble inorganic abrasive agents, thickening agents, moisturizers, surfactants, and the like.
  • abrasive agents which may be mentioned in particular are calcium carbonate, hydrated alumina, bentonite, aluminium silicate, zirconium silicate and sodium, potassium, calcium and magnesium metaphosphates and phosphates.
  • thickening agents mention may be made in particular of xanthan gum, guar gum, carrageenans, cellulose derivatives and alginates, in a quantity that can range up to 5 % by weight of the composition.
  • moisturizers mention may be made, for example, of glycerol, sorbitol, polyethylene glycols, polypropylene glycols and xylitol, in a quantity of the order of 2 to 85 %, preferably of the order of 10 to 70 % of the weight of composition, expressed on dry basis.
  • inventive composition may additionally comprise surface-active agents, detergent agents, colorants, bactericides, fluorine derivatives, opacifiers, sweeteners, antitartar and antiplaque agents, sodium bicarbonate, antiseptics, enzymes, etc.
  • the composition further comprises antibacterial agent.
  • antibacterial agents are chlorhexidine and chlorhexidine salts, such as bigluconate or diacetate, triclosan, cetylpyridinium chloride, benzalconium chloride and cetyltrimethylammonium bromide.
  • inventive silica not only increases the stability of the inventive composition towards the loss of peroxide activity but it also increases the stability of antibacterial agents, and in particular antibacterial agents containing chlorhexidine.
  • the oral care composition comprises a peroxide-releasing compound, an antibacterial agent containing chlorhexidine and the inventive precipitated silica.
  • the inventive silica may further exhibit a good compatibility with respect to cations which are customarily present in oral care compositions.
  • cations which are customarily present in oral care compositions.
  • cations are for instance, calcium, strontium, barium, manganese, indium, nickel, zinc, titanium, zirconium, silver, palladium, ammonium or amino cations.
  • These cations may be in the form of mineral salts, for example chloride, fluoride, nitrate, phosphate, sulfate or in the form of organic salts such as acetates, citrates.
  • the oral care composition comprises a peroxide-releasing compound, an antimicrobial agent containing chlorhexidine, a Zn containing salt and the inventive precipitated silica.
  • the inventive composition has a compatibility with zinc, as determined using the Zn compatibility method described hereafter, of at least 50%.
  • the oral composition is a dentifrice.
  • dentifrices may include toothpaste (dental cream), tooth powders, or gel, or any other form known to one skilled in the art.
  • the dentifrice is characterised by a Relative Dentine Abrasion (RDA), measured on the formulation as detailed hereafter, of 90 to 200, typically of 100 to 160.
  • RDA Relative Dentine Abrasion
  • the dentifrice is characterised by a Pellicle Cleaning Ratio (PCR), measured on the formulation as detailed hereafter, between 75 and 110, typically between 80 to 100.
  • PCR Pellicle Cleaning Ratio
  • inventive oral care composition may be used for the cleaning of teeth.
  • a further object of the invention is a process for the preparation of the inventive precipitated silica, said process comprising the steps of: providing a precipitated silica, hereinafter defined as the “Starting Silica”; and submitting said precipitated silica to a thermal treatment at a temperature of 400 to 650°C for 1 to 180 minutes.
  • the Starting Silica may be in any form, such as a powder, granules, or substantially spherical beads.
  • the Starting Silica is characterised by a number of OH groups per surface area higher than 2.00 OH/nm 2 .
  • the Starting Silica is characterised by a number of OH groups per surface area higher than 10.00 OH/nm 2 , typically higher than 20 OH/nm 2 , even higher than 40 OH/nm 2 , in some instances higher than 50 OH/nm 2 .
  • the thermal treatment may be carried out using any suitable equipment.
  • suitable equipment for the thermal treatment is for instance a rotating oven.
  • the process for the preparation of the modified silica comprises the steps of:
  • the thermal treatment is preferably performed at a temperature of 500 to 650°C, more preferably at a temperature of 550 to 650 °C.
  • the precipitated silica is preferably held at the thermal treating temperature for 30 to 150 minutes, preferably for 30 to 120 minutes. The duration of the thermal treatment is adjusted so that the number of the OH groups per surface area are reduced from the initial value of the Starting Silica to a value below 2.0 OH/nm 2 .
  • the Starting Silica may be any precipitated silica which is suitable for use as an abrasive silica in oral care application.
  • the Starting Silica typically has a surface area CTAB of less than 50 m 2 /g, typically between 5 and 50 m 2 /g.
  • Suitable commercially available precipitated silicas which can be used as Starting Silica are for instance : Tixosil® 73, Tixosil® 63, Tixosil® SoftClean, all available from Solvay SA.
  • a further object of the present invention is a method for reducing the decomposition of peroxide-releasing compounds in an oral care composition comprising a peroxide-releasing compound and precipitated silica, said method characterized in that the precipitated silica is a precipitated silica characterised by:
  • inventive precipitated silica allows at the same time to maintain high over time the availability of both chlorhexidine based antibacterial agents as well as zinc based compounds.
  • CTAB surface area (SCTAB) values were determined according to an internal method derived from standard NF ISO 5794-1 , Appendix G.
  • BET surface area SBET was determined according to the Brunauer - Emmett - Teller method as detailed in standard NF ISO 5794-1 , Appendix E (June 2010) with the following adjustments: the sample was pre-dried at 200°C ⁇ 10°C; the partial pressure used for the measurement P/P° was between 0.05 and 0.3.
  • the silanol density is directly related to the loss of mass between 200°C and 800°C.
  • the loss of mass (%) between 200°C and 800°C is identified as AW% this value.
  • silanol ratio (mmol/g) is defined by:
  • the hydrogen peroxide solution used was (solution A).
  • solution A a suspension containing 10 wt% of silica, 2 wt% of hydrogen peroxide was prepared. The suspension thus obtained was stirred for 7 days at 25°C (suspension B).
  • a iodometry dosing was then performed on suspension B.
  • the unreacted iodine was dosed using a sodium thiosulfate solution at 0.1 mol/L with a Pt titrode.
  • the hydrogen peroxide compatibility was calculated as the ratio of peroxide hydrogen available in suspension B with respect to the initial value according to the following formula:
  • H2O2 in suspension B H2O2 compatibility (%) — . - - — - - — x 100
  • Abrasivity of silica was determined according to an internal method using poly(methyl methacrylate) (PMMA) plates as a substrate. Method is correlated to state of the art abrasivity test Relative Dentine Abrasion (RDA) (F. Peditto et al. “Which Alternatives to ISO11609 RDA? PMMA Abrasion Test with Silicas”, IADR GA Seattle, 2013).
  • RDA Relative Dentine Abrasion
  • the abrasion depth (Hm, expressed in pm) at the end of the brushing cycles was measured across a 20 x 10 mm area including the Testing area by optical profilometry (Altimet Altisurf 500) on rinsed plates. The area around the Testing area was used to define the baseline for the optical profilometry determination.
  • RDA Relative Dentine Abrasion
  • RDA Relative Dentin Abrasions
  • Toothpaste formulations described in Table 1 were prepared in a GUEDll reactor (4.5 L) according to the protocol detailed Table 1 below. Silicas from the invention were used in the formulation in an amount of 11 wt%. Pre-gel was prepared in a RAYNERI mixer, adding ingredients at 1000- 1500 rpm, the day before mixing on the GUEDll reactor.
  • PCR Pellicle Cleaning Ratio
  • CS1 Precipitated silica Tixosil® 73 commercially available from Solvay SA
  • Thickening silica Precipitated silica Tixosil®43 commercially available from Solvay SA
  • Tixosil®73 (commercially available form Solvay, identified as CS1 in Table 1) was used as a starting material for the preparation of a modified silica. 100 g of Tixosil®73 were placed in an oven and heated from 25°C to the final temperature of 600°C at a ramp-up speed of 2°C/ min. The silica was the held at 600°C for 60 minutes. Finally the temperature was reduced from 600°C to 30°C with a speed of 10°C/min. At the end of the cool-down cycle the precipitated silica S1 was recovered and placed in a sampling bottle.
  • Silica S1 exhibits higher cleaning performances (PCR) vs CS1 in toothpaste formulation, related to a higher abrasivity as shown by both RDA and PMMA methods.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)
EP21802236.6A 2020-11-10 2021-10-27 Bleichende mundpflegezusammensetzungen Withdrawn EP4243759A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP20306356 2020-11-10
PCT/EP2021/079827 WO2022101015A1 (en) 2020-11-10 2021-10-27 Whitening oral care compositions

Publications (1)

Publication Number Publication Date
EP4243759A1 true EP4243759A1 (de) 2023-09-20

Family

ID=73554382

Family Applications (1)

Application Number Title Priority Date Filing Date
EP21802236.6A Withdrawn EP4243759A1 (de) 2020-11-10 2021-10-27 Bleichende mundpflegezusammensetzungen

Country Status (3)

Country Link
EP (1) EP4243759A1 (de)
CN (1) CN116437893A (de)
WO (1) WO2022101015A1 (de)

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4427137B4 (de) * 1993-10-07 2007-08-23 Degussa Gmbh Fällungskieselsäure
FR2714369B1 (fr) * 1993-12-29 1996-01-26 Rhone Poulenc Chimie Silices abrasives pour compositions dentifrices.
ATE168663T1 (de) * 1996-03-27 1998-08-15 Degussa Fällungskieselsäure
DE10138490A1 (de) * 2001-08-04 2003-02-13 Degussa Hydrophobe Fällungskieselsäure mit hohem Weißgrad und extrem niedriger Feuchtigkeitsaufnahme
US20150209252A1 (en) * 2014-01-27 2015-07-30 J.M. Huber Corporation Heat Treated Silica for Improved Dentifrice
JP6797194B2 (ja) * 2015-09-28 2020-12-09 エボニック オペレーションズ ゲーエムベーハー シリカベースの抗微生物性口腔用組成物
WO2017109743A1 (en) * 2015-12-23 2017-06-29 Tata Chemicals Limited Precipitated silica
RU2726804C1 (ru) * 2016-12-19 2020-07-15 Дзе Проктер Энд Гэмбл Компани Композиции для чистки зубов, содержащие совместимые с оловом частицы оксида кремния
CN110603224B (zh) * 2017-05-05 2024-01-02 罗地亚经营管理公司 沉淀二氧化硅及其制造方法
MX2020012354A (es) * 2018-06-19 2021-04-28 Rhodia Operations Silice para composiciones de cuidado oral.

Also Published As

Publication number Publication date
WO2022101015A1 (en) 2022-05-19
CN116437893A (zh) 2023-07-14

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