PT78871B - Process for preparing stable antiplaque dentifrice with improved foaming and fluoride stability - Google Patents

Process for preparing stable antiplaque dentifrice with improved foaming and fluoride stability Download PDF

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Publication number
PT78871B
PT78871B PT78871A PT7887184A PT78871B PT 78871 B PT78871 B PT 78871B PT 78871 A PT78871 A PT 78871A PT 7887184 A PT7887184 A PT 7887184A PT 78871 B PT78871 B PT 78871B
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process according
weight
fluoride
polyethylene glycol
dentifrice
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PT78871A
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Portuguese (pt)
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PT78871A (en
Inventor
John P Curtis
Richard J Crawford
Katllen M Yuhasz
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Colgate Palmolive Co
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Priority claimed from US06/513,474 external-priority patent/US4490353A/en
Priority claimed from US06/513,473 external-priority patent/US4528182A/en
Application filed by Colgate Palmolive Co filed Critical Colgate Palmolive Co
Publication of PT78871A publication Critical patent/PT78871A/en
Publication of PT78871B publication Critical patent/PT78871B/en

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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
    • 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
    • A61K8/20—Halogens; Compounds thereof
    • A61K8/21—Fluorides; Derivatives thereof
    • 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
    • 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
    • A61K8/26—Aluminium; Compounds thereof
    • 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
    • A61K8/34—Alcohols
    • A61K8/345—Alcohols containing more than one hydroxy group
    • 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
    • A61K8/39—Derivatives containing from 2 to 10 oxyalkylene groups
    • 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
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/41—Amines
    • A61K8/416—Quaternary ammonium compounds
    • 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
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • 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
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • A61K8/442—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof substituted by amido group(s)
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/731—Cellulose; Quaternized cellulose derivatives
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86—Polyethers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/54—Polymers characterized by specific structures/properties
    • A61K2800/542—Polymers characterized by specific structures/properties characterized by the charge
    • A61K2800/5422—Polymers characterized by specific structures/properties characterized by the charge nonionic

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Emergency Medicine (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)
  • Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)

Abstract

A stable antiplaque dentifrice with improved foaming and fluoride chemical stability containing an antiplaque quaternary ammonium compound, a betaine surfactant to improve foaming without inactivating the antibacterial and antiplaque activity of the quaternary ammonium compound, a humectant selected from the group consisting of polyethylene glycol, sorbitol and mixtures thereof, a nonionic gelling agent, such as hydroxyethylcellulose, and preferably a fluorine-containing compound capable of providing a fluoride ion, in an aqueous vehicle containing a dental abrasive. The sorbitol component, which stabilises the betaine quaternary ammonium system, also improves long term fluoride chemical stability of the dentifrice. In a sole polyethylene glycol humectant, a small amount of glycerin, as low as 1%, may be utilised to improve long term fluoride stability, without adversely affecting the cosmetic stability of the dentifrice.

Description

Descrição Pormenorizada do Invento

Os exemplos que seguem, são mais ainda elucidativos da natureza do invento em consideração, mas deve entender-se que o invento não está limitado, por esse efeito. As composições são preparadas pela maneira habitual, e todas as quantidades e proporções, referidas nesta Memória Descritiva e nas reivindicações anexas, são em peso, salvo indicação em contrário.

Exemplo 1

Ingredientes Percentagem Hidroxietilcelulose 1,0 Carbowax 6001 20,0 Sacarina Sódica 0,2 MFF2 0,76 CAB5(35% A.I.) 3,5 Fosfato Dicalcico 49,0 BZC14 0,5 D.I. H20 24,04 Aromatizante 1,0

^Polietileno Glicol peso molecular 600

“Tfonof luorofosf ato de Sodio

3 f Cocoamidopropilbetaina

4

Cloreto de Benzetonio

A hidroxietilcelulose e a água são pré-misturatfe. s, durante 10 minutos, para se formar um gel. As substâncias pulverizadas MPF, BZOl e a sacarina, e o humectante Carbowax são adicionados ao gel, e são misturados durante 10 a 20 minutos. A mistura gelada é adicionada ao fosfato e dicálcico e é misturada durante 2Ó minutos, à velocidade 8, no agitador Ross. A betaina e o aromatizante são adicionados â mistura e são misturados durante 5 minutos â velocidade 6, no agitador Ross.1 0 creme dentário resultante, que é atraente cosmeticamente, é entubado.

Os testes de actuação, realizados com este produto, em tubos revestidos, à temperatura ambiente, a 40°E (4°C) e a 100°P (37°C), durante 9 semanas, e em tubos não revestidos, a 120°P (49°C), durante 9 semanas, revelaram uma estabilidade cosméticaexcelente.

Exemplo 2 Ingredientes Percenta Hidroxietilcelulose 1,1 Carbowax 600 20,0 Sacarina Sódica 0,2 MPP 0,76 CAB (35% A.I.) 5,7 Fosfato Dicálcico 46,8

BZC1

0,5

-22(Cont.)

Ingredientes Percentagem h2o 24,04 Aromatizante 1,0

Este creme dentário é preparado de acordo com o processo do exemplo 1. Este produto tem um pH de 6,7 β uma altira de espuma de 55, mas não tem um bom paladar.

Exemplo 3

Ingredientes Percentagem Essência de Hortelã-pimenta Doce Hi 1,0 MAG1 0,1 BZC1 0,5 MFF 0,76 Sacarina Sódica 0,2 h2o 23,44 PEG 6002 20,0 Natrosol 1,0

49,0

4,0

Fosfato Dicalcico OAB(3O7o A.I.)

•1

xGlicirrizinato de monoamónio

2

Polietileno Glicol de peso molecular 600

Hidroxietilcelulose

Este creme dentário e preparado de acordo com o processo do exemplo 1, excepto que o pH é ajustado a 8,5, com NaOH diluido para os fins de hidratação depois de o polietileno glicol ter sido adicionado à pre-mistura gelada.

0 creme resultante tem uma boa aparência, tem uma altura de espuma de 38 a 40, e apresenta uma estabilidade excelente empregando-se os ensaios de actuação durante um periodo superior a 12 semanas, a 100θΕ, bem como a 140°P, em tubos não revestidos, durante 3 semanas.

Exemplo 4

Repete-se o exemplo 3, excepto que a glicerina substitui o humectante polietileno glicol. Este produto dá origem a uma altura de espuma de 46, mas revela um vestígio de separação em 3 dias, a 140°P (60°c) e uma humidade e separação no gargalo do tubo, a 120°P (49°C) em 3 semanas. Este produto é instável cosmeticamente.

-24Exemplo 5

Ingredientes Percentagem h2o 21,14 Natrosol 1,3 Propiino Glicol 20,0 Sacarina Sódica 0,2 BZC1 0,5 MAG 0,1 MFF 0,76 Fosfato Dicálcico 50,0 CAB (30% A.I.) 5,0 Aromatizante 1,0

Este creme dentário e preparado de acordo com o processo do exemplo 1, excepto que o humectante de polietileno glicol e misturado com ogel da prá-mistura, durante somente 10 minutos. 0 produto resultante e bom na sua aparência e produz uma espuma com uma altura de 44.

Conta do, a sua instabilidade e nitidamente evidente pela separação, pela humidade ao longo da faixa e derrame no grampo em 3 semanas, a 8°p (-33 °c) e a 40°F (4°C) e por uma ligeira coloração amarela a 110°F (43°C) e a 120°F (49°C) dentro de 3 semanas.

Exemplo 6 Ingredientes Percentagem H2° 19,68 Natrosol 1,1 Carbowax 600 20,0 Sacarina Sódica 0,2 BZC1 0,5 MAG 0,1 MFF 0,76 Fosfato Dicálcico 50,0 CAB (30% A.I.) 6,66 Aromatizante 1,0 de acordo com o processe Este creme dentário ó preparado » do Exemplo 1. 0 produto resultante e ligeiramente espesso, mas apresenta uma boa produção de espuma e uma boa estabilidade.

Exemplo 7

Ingredientes Percentagem h2o 21,34 Natrosol 1,1 Carbowax 600 20,0 Sacarina Sódica 0,2 BZC1 0,5 MAG 0,1 MFF 0,76 Ca2P2°71 50,0 CAB (30% A.l.) 5,0 Aromatizante 1,0 ^Pirofosfato de Cálcio

Este creme dental é preparado de acordo com o processo do exemplo 1.

0 creme resultante ó espesso e granuloso, o que pode ser devido à granulometria do abrasivo dentário de pirofosfato de cálcio.

-27Exemplo 8

Ingredientes Percentagem h2o 17,68 Natrosol 1,1 Carbowax 600 20,0 Sacarina Sódica 0,2 BZC1 0,5 MAG 0,1 MFF 0,76 Di-hidrato de Fosfato Dicálcico 42,0 Fosfato Dicálcico Mdro 10,0 CAB (30% A.I.) 6,66

Aromatizante

1,0

Exemplo 9

Ingredientes Percentagem Carbowax 600 20,0 Natrosol 1,1 Sacarina Sodica 0,2 MAG 0,1 BZC1 0,5 H2° 17,68 MFP 0,76 Alumina Hidratada 42,0 Alumina Calcinada 10,0

Co coamidopropilbetaína (30% A.I.) 6,66 Aromatizante 1,0

Co coamidopropilbetaína (30% A.I.) 6,66 Aromatizante 1,0 pH 8,3

Este produto apresenta uma estabilidade completa, depois de se actuar durante 9 semanas, à tempe ratura ambiente, a 40°? (4°C) a 100°P (37°C), e a 120°P (49°C).

Exemplos 10 e 11

Ingredientes

PEG 600

Natrosol

Sacarina Sódica

Alumina Hidratada

Alumina Calcinada

CAB (30% A.I.)

MFF

AromaU zante

H20 D. I.

BZCl

Red 40 (Solução a 1%)

Exemplo 10 Exemplo 11 Per centagem Percentagem 20,0 20,0 1,1 1,3 0,3 0,3 42,0 42,0 10,0 10,0 5,0 5,0 0,76 0,76 1,0 1,0 19,27 18,64 0,5 0,5 0,07 0,07

-30·

Exemplo 12

Ingredientes

Sorbitol 70%

Natrosol

Sacarina Sódica

BZC1

MEE

Alumina

Alumina Calcinada

CAB (30% A.I.)

Aromatizante

h2o

pH Inicial 7,4

pH após 3 semanas 7,5 pH após 6 semanas 7,6

Percentagem

28,0

1,1

0,5

0,5

0,76

42,0

10,0

5,0

1,0

11,54

Este produto revela uma estabilidade completa, a 8°E (-13°C) e a 40°E (4°C), durante um periodo de 9 semanas, mas revela uma tampa ligeiramente húmida a 110°E (43°C) e a 120°E (49°C), depois de 3 a 9 semanas. Em complemento da boa estabilidade fisica deste produto, o conteúdo do ingrediente activo (fluoreto iónico e cloreto de benzetónio)permanece estável, como e testemunhado pelo

pH que permanece substancialmente estável·

Exemplo 13 Ingredientes Fercentag h20 21,14 Natrosol 1,5 Sorbitol 20,0 Sacarina Sádica 0,2 B2C1 0,5 MAG 0,1 MFF 0,76 Di-hidrato de Fosfato Dicálcico 50,0 CAB (30% A.I.) 5,0 Aromâizaate 1,0

0 creme resultante apresenta uma altura de espuma de 42 e nenhum desprendimento do aroma depois de 9 semanas a 120 F (49°C). Este produto e completamente estável e 8°F (-13°C) e a 40°F (4°C) durante um periodo de 9 semanas, mas revela vestígios de uma tampa húmida a 11O°F(43°O) e a 120°F (45°0), depois de 3 a 9 semanas.

Exemplo 14

Ingredientes Percentagem Natrosol 1,1 Sacarina Sódica 0,3 BZC1 0,5 MPB 0,76 Carbowax 600 10,0 Sorbitol (70%) 10,0 HgO Desionizada 19,34 Alumina Hidratada 10,0 Alumina Calcinada 42,0 Aromatizante 1,0 CAB (30% A.I.) 5,0

Exemplo 15 Ingredientes Percenta Natrosol 1,1 Sacarina Sódica 0,5 MFF 0,76 BZCl 0,5 Carbowax 600 15,0 Sorbitol (70%) 5,0 h2o 19,34 Alumina Hidratada 42,0 Alumina Calcinada 10,0 Aromatizante 1,0 CAB (30% A.I.) 5,0

Este produto, que contem 5% de sorbitol apresenta uma recuperação de 84% do fluoreto solúvel, em 12 semanas, a 100°F (37°C), em comparação com a recuperação de 61% de fluoreto (nivel aceitável) para o sistema do humectante de polietileno glicol isolado, sob as mesmas condições, por exemplo, exemplos 1 a 11. Isto indica que a presença do sorbitol, em quantidades tão reduzidas como 5% (70% A.I·), proporciona uma estabilidade de fluoreto maior.

Exemplos 16 a 20

Percentagem

Ingredientes Ex. 16 Ex.17 Ex.18 Ex.19 Ex.20 Polietileno glicol (Carbowax 600) 15 17 19 10 20 Glicerina 5 3 1 10 0 Hidroxietil Celulose 1,10 1,10 1,10 1,10 1,10 Monofluorofosfato de Sodio 0,76 0,76 0,76 0,76 0,76 Sacarina Sódica 0,30 0,30 0,30 0,30 0,30 Cloreto de benzetónio 0,50 0,50 0,50 0,50 0,50 Alumina Hidratada 42 42 42 42 42 Alumina Calcinada 10 10 10 10 10 CAB (30% A.I.) 5 5 5 5 5 Aromatizante 1 1 1 1 1 Água 19,34 19,34 19,34 19,34 19,34 Conteúdo de FI 0,07 0,067 0,066 0,077 Q057

x A estabilidade quimica das formulações precedentes, depois

de uma actuação durante 12 semanas, a 100°F (37°C) como verificada pela percentagem do conteúdo de Fl”.

Todas as formulações precedentes são eficientes contra as bactérias relacionadas com a pedra, enquanto possuem aperfeiçoadas caracteristicas de produção de espuma, estabilidade cosmética e estabilidade quimica. A presença de uma quantidade pequena de glicerina, tão reduzida como 1%, em peso, aumenta a estabilidade quimica do fluoreto no dentifrico contendo o humectante de polietileno glicol, para mais do que a estabilidade aceitável do fluoreto, na ausência da glicerina (Exemplo 20).

Podem fazer-se variações nas formulações precedentes. Por exemplo, outras betaínas, tais como a lauramidopropil betaina, cocobetaina e outras afins podem substituir a cocoamidopropil betaina nos exemplos. De um modo semelhante, outros abrasivos podem substituir os abrasivos específicos dos exemplos. De um modo idêntico, outros compostos contendo o fluoreto, tais como o fluoreto de sodio, o fluoreto de potássio, etc., podem substituir o monofluorofosfato de sodio, nos exemplos específicos.

Deve compreender-se que a descrição pormenorizada precedente é dada unicamente a titulo de elucidação e que podem fazer-se nela variações sem se afastar do espirito do invento. 0 ''Resumo” dado anteriormente foi unicamente para a conveniência dos investigadores técnicos, e a ele não deve atribuir-se qualquer preponderância, no que respeita ao âmbito do invento.

-36

Detailed Description of the Invention

The examples which follow are even more illustrative of the nature of the invention under consideration, but it is to be understood that the invention is not limited by that effect. The compositions are prepared in the usual manner, and all amounts and proportions, referred to in this specification and the appended claims, are by weight unless otherwise indicated.

Example 1

Ingredients Percentage Hydroxyethylcellulose 1.0 Carbowax 600 1 20.0 Saccharin Sodium 0.2 MFF 2 0.76 CAB 5 (35% AI) 3.5 Dicalcium Phosphate 49.0 BZC1 4 0.5 DI H 2 0 24.04 Flavoring 1.0

^ Polyethylene Glycol 600 molecular weight

"Sodium Phosphonofluorophosphate

3 f Cocoamidopropylbetaine

4

Benzethonium Chloride

Hydroxyethylcellulose and water are preblended. s over 10 minutes to form a gel. The MPF, BZO1 and saccharin sprayed substances, and the Carbowax humectant are added to the gel, and are mixed for 10 to 20 minutes. The chilled mixture is added to the phosphate and dicalcium and is mixed for 20 minutes at speed 8 on the Ross shaker. The betaine and the flavoring are added to the blend and are blended for 5 minutes at speed 6 on the Ross shaker. 1 0 resulting dental cream, which is cosmetically attractive, is intubated.

The actuation tests performed with this product were coated tubes at room temperature at 40øC (4øC) and 100øP (37øC) for 9 weeks in uncoated tubes at 120øC (49 ° C) for 9 weeks showed excellent cosmetic stability.

Example 2 Ingredients Percenta Hydroxyethylcellulose 1.1 Carbowax 600 20.0 Saccharin Sodium 0.2 MPP 0.76 CAB (35% AI) 5.7 Dicalcium Phosphate 46.8

BZC1

0.5

-22 (Cont.)

Ingredients Percentage h 2 o 24.04 Flavoring 1.0

This toothpaste is prepared according to the process of example 1. This product has a pH of 6.7 a foam top of 55 but does not have a good taste.

Example 3

Ingredients Percentage Sweet Peppermint Essence Hi 1.0 MAG 1 0.1 BZC1 0.5 MFF 0.76 Saccharin Sodium 0.2 h 2 o 23.44 PEG 600 2 20.0 Natrosol 1.0

49.0

4.0

Dicalcium Phosphate OAB (307 ° AI)

•1

x Monoammonium glycyrrhizinate

2

Polyethylene glycol 600 molecular weight

Hydroxyethylcellulose

This toothpaste is prepared according to the process of example 1, except that the pH is adjusted to 8.5 with dilute NaOH for the purpose of hydration after the polyethylene glycol has been added to the ice-cold premix.

The resulting cream has a good appearance, has a foam height of 38 to 40, and exhibits excellent stability by employing the actuation tests for a period of more than 12 weeks at 100θÅ as well as at 140øP in tubes uncoated, for 3 weeks.

Example 4

Example 3 is repeated except that the glycerin replaces the polyethylene glycol humectant. This product gives rise to a foam height of 46 but shows a separation trait in 3 days at 140øP (60øC) and a moisture and separation at the neck of the tube at 120øP (49øC) in 3 weeks. This product is unstable cosmetically.

Example 5

Ingredients Percentage h 2 o 21.14 Natrosol 1.3 Propiino Glycol 20.0 Saccharin Sodium 0.2 BZC1 0.5 MAG 0.1 MFF 0.76 Dicalcium Phosphate 50.0 CAB (30% AI) 5.0 Flavoring 1.0

This toothpaste is prepared according to the procedure of Example 1, except that the polyethylene glycol humectant is mixed with the pregelatinized gel for only 10 minutes. The resulting product is good in appearance and produces a foam with a height of 44.

Account, its instability and markedly evident by separation, moisture along the lane and effusion on the clamp at 3 weeks, at 8Â ° C (-33Â ° C) and at 40Â ° F (4Â ° C) and by a slight yellow color at 110 ° F (43 ° C) and 120 ° F (49 ° C) within 3 weeks.

Example 6 Ingredients Percentage H 2 ° 19.68 Natrosol 1.1 Carbowax 600 20.0 Saccharin Sodium 0.2 BZC1 0.5 MAG 0.1 MFF 0.76 Dicalcium Phosphate 50.0 CAB (30% AI) 6.66 Flavoring 1.0 according to the process This dental cream is prepared from Example 1. The resulting product is slightly thick but has good foam production and good stability.

Example 7

Ingredients Percentage h 2 o 21.34 Natrosol 1.1 Carbowax 600 20.0 Saccharin Sodium 0.2 BZC1 0.5 MAG 0.1 MFF 0.76 Ca 2 P 2 7 1 50.0 CAB (30% Al) 5.0 Flavoring 1.0 Calcium Pyrophosphate

This toothpaste is prepared according to the process of example 1.

The resulting cream is thick and granular, which may be due to the granulometry of the calcium pyrophosphate dental abrasive.

Example 8

Ingredients Percentage h 2 o 17.68 Natrosol 1.1 Carbowax 600 20.0 Saccharin Sodium 0.2 BZC1 0.5 MAG 0.1 MFF 0.76 Dicalcium Phosphate Dihydrate 42.0 Phosphate Dicalcium Mdro 10.0 CAB (30% AI) 6.66

Flavoring

1.0

Example 9

Ingredients Percentage Carbowax 600 20.0 Natrosol 1.1 Saccharin Sodica 0.2 MAG 0.1 BZC1 0.5 H 2 ° 17.68 MFP 0.76 Hydrated Alumina 42.0 Calcined Alumina 10.0

Co coamidopropyl betaine (30% AI) 6.66 Flavoring 1.0

Co coamidopropyl betaine (30% AI) 6.66 Flavoring 1.0 pH 8.3

This product exhibits complete stability, after operating for 9 weeks at room temperature, at 40 ° C. (4 ° C) at 100 ° P (37 ° C), and at 120 ° P (49 ° C).

Examples 10 and 11

Ingredients

PEG 600

Natrosol

Saccharin Sodium

Hydrated Alumina

Calcined Alumina

CAB (30% AI)

MFF

Sunflower

H 2 0 DI

BZCl

Red 40 (1% solution)

Example 10 Example 11 Per centage Percentage 20.0 20.0 1.1 1.3 0.3 0.3 42.0 42.0 10.0 10.0 5.0 5.0 0.76 0.76 1.0 1.0 19.27 18.64 0.5 0.5 0.07 0.07

-30 ·

Example 12

Ingredients

Sorbitol 70%

Natrosol

Saccharin Sodium

BZC1

MEE

Alumina

Calcined Alumina

CAB (30% AI)

Flavoring

h 2 o

Initial pH 7.4

pH after 3 weeks 7.5 pH after 6 weeks 7.6

Percentage

28.0

1.1

0.5

0.5

0.76

42.0

10.0

5.0

1.0

11.54

This product shows complete stability at 8 ° E (-13 ° C) and 40 ° E (4 ° C) over a period of 9 weeks, but reveals a slightly damp cap at 110 ° E (43 ° C) and at 120 ° E (49 ° C), after 3 to 9 weeks. In addition to the good physical stability of this product, the content of the active ingredient (ionic fluoride and benzethonium chloride) remains stable, as witnessed by

pH remaining substantially stable

Example 13 Ingredients Fercentag h 2 0 21.14 Natrosol 1.5 Sorbitol 20.0 Saccharin Sadic 0.2 B2C1 0.5 MAG 0.1 MFF 0.76 Dicalcium Phosphate Dihydrate 50.0 CAB (30% AI) 5.0 Cheer up 1.0

The resulting cream exhibits a foam height of 42 and no aroma detachment after 9 weeks at 120 F (49 ° C). This product is completely stable at 8øF (-13øC) and at 40øF (4øC) over a period of 9 weeks, but reveals traces of a wet cap at 110øF (43øC) and 120 ° F (45 ° C), after 3 to 9 weeks.

Example 14

Ingredients Percentage Natrosol 1.1 Saccharin Sodium 0.3 BZC1 0.5 MPB 0.76 Carbowax 600 10.0 Sorbitol (70%) 10.0 Deionized HgO 19.34 Hydrated Alumina 10.0 Calcined Alumina 42.0 Flavoring 1.0 CAB (30% AI) 5.0

Example 15 Ingredients Percenta Natrosol 1.1 Saccharin Sodium 0.5 MFF 0.76 BZCl 0.5 Carbowax 600 15.0 Sorbitol (70%) 5.0 h 2 o 19.34 Hydrated Alumina 42.0 Calcined Alumina 10.0 Flavoring 1.0 CAB (30% AI) 5.0

This product containing 5% sorbitol exhibits 84% recovery of soluble fluoride at 12 weeks at 100 ° F (37 ° C), compared to recovery of 61% fluoride (acceptable level) for the system of the polyethylene glycol humectant alone, under the same conditions, for example, Examples 1 to 11. This indicates that the presence of sorbitol, in amounts as low as 5% (70% Al), provides greater fluoride stability.

Examples 16 to 20

Percentage

Ingredients Ex. 16 Ex.17 Ex.18 Ex.19 Ex.20 Polyethylene glycol (Carbowax 600) 15 17 19 10 20 Glycerin 5 3 1 10 0 Hydroxyethyl Cellulose 1.10 1.10 1.10 1.10 1.10 Sodium Monofluorophosphate 0.76 0.76 0.76 0.76 0.76 Saccharin Sodium 0.30 0.30 0.30 0.30 0.30 Benzethonium chloride 0.50 0.50 0.50 0.50 0.50 Hydrated Alumina 42 42 42 42 42 Calcined Alumina 10 10 10 10 10 CAB (30% AI) 5 5 5 5 5 Flavoring 1 1 1 1 1 Water 19.34 19.34 19.34 19.34 19.34 FI content 0.07 0.067 0.066 0.077 Q057

The chemical stability of the foregoing formulations, then

of a performance for 12 weeks at 100Â ° F (37Â ° C) as ascertained by the percentage of the F1 content.

All of the foregoing formulations are effective against stone-related bacteria, while having improved foam production, cosmetic stability and chemical stability characteristics. The presence of a small amount of glycerin as low as 1% by weight increases the chemical stability of the fluoride in the dentifrice containing the polyethylene glycol humectant for more than the acceptable stability of the fluoride in the absence of glycerol (Example 20 ).

Variations can be made in the foregoing formulations. For example, other betaines, such as lauramidopropyl betaine, cocobetaine and the like may substitute the cocoamidopropyl betaine in the examples. In a similar manner, other abrasives may replace the specific abrasives of the examples. Likewise, other fluoride-containing compounds, such as sodium fluoride, potassium fluoride, etc., may replace sodium monofluorophosphate in the specific examples.

It should be understood that the foregoing detailed description is given solely by way of elucidation and that variations may be made therein without departing from the spirit of the invention. The foregoing 'Summary' was solely for the convenience of the technical investigators, and no preponderance should be attributed thereto, with regard to the scope of the invention.

-36

Claims (15)

REIVINDICAÇÕES lâ. - Processo para a preparaçao de um dentifrico antipedra estável, com formação de espuma melhorada e estabilidade melhorada do fluoreto, caracterizado por se incluir no referido dentifrico, como ingredientes essenciais, uma quantidade eficaz de um composto quaternário de amónio antipedra, pelo menos, 1,5% de um surfactante de betaina, um humectante seleccionado do grupo constituido por polietileno glicol, sorbitol e suas misturas, um agente de gelificação não iónico e, de preferência, um composto que forneça fluoreto num veiculo aquoso contendo um abrasivo dentário.over there. A process for the preparation of a stable antipyretic dentifrice with improved foaming and improved stability of fluoride, characterized in that an effective amount of a quaternary ammonium compound is added to said dentifrice by at least 1, 5% of a betaine surfactant, a humectant selected from the group consisting of polyethylene glycol, sorbitol and mixtures thereof, a nonionic gelling agent, and preferably a compound which provides fluoride in an aqueous vehicle containing a dental abrasive. 2â. - Processo de acordo com a reivindicação 1, caracterizado por o conteúdo em betaina constituir cerca de 1,5 a 2%, em peso, da formulação.2â. 5. A process according to claim 1, wherein the betaine content constitutes about 1.5 to 2% by weight of the formulation. 3>. - Processo de acordo com a reivindicação 2, caracterizado por o agente de gelificação não iónico ser a hidroxietilcelulose, em quantidade de cerca de 0,5 a 2% em peso·3>. 2. A process according to claim 2, wherein the nonionic gelling agent is hydroxyethylcellulose in an amount of about 0.5 to 2% by weight. 4-· - Processo de acordo com a reivindicação 3, caracterizado por se incluir cerca de 20 a 30% em peso, de polietileno glicol, tendo um peso molecular de 600,4. A process according to claim 3, characterized in that about 20 to 30% by weight of polyethylene glycol having a molecular weight of 600, 5a· - Processo de acordo com a reivindicação 3, caracterizado por se incluir cerca de 20 a 30%, em peso de sorbitol.5. A process according to claim 3, characterized in that about 20 to 30% by weight of sorbitol is included. 6a· - Processo de acordo com a reivindicação 1, caracterizado por se incluir cerca de 40 a 60%, em peso de um abrasivo dentário insolúvel em água.6. A process according to claim 1, characterized in that about 40 to 60% by weight of a water-insoluble dental abrasive is included. 7a. - Processo de acordo com a reivindica-7 a . 2. A method according to claim 1, ção 4» caracterizado por o abrasivo dentário ser o fosfato dicalcico.characterized in that the dental abrasive is dicalcium phosphate. 8*. - Processo de acordo com a reivindica ção 3, caracterizado por o agente antipedra ser o cloreto de benzetónio, numa quantidade de cerca de 0,01 a 5% em peso.8 *. 3. A process according to claim 3, characterized in that the antiblocking agent is benzethonium chloride in an amount of about 0.01 to 5% by weight. 9â. - Processo de acordo com a reivindicação 1, caracterizado por o composto que fornece fluoreto constituir cerca de 0,05 a 2%, em peso, do dèntifrico.9 â . 2. A process according to claim 1, wherein the fluoride-providing compound constitutes about 0.05 to 2% by weight of the diethyl ether. lQâ. - Processo de acordo com a reivindicação 9, caracterizado por o composto que fornece fluoreto ser o monofluorofosfato de sódio.lQâ. 8. A process according to claim 9, wherein the fluoride-providing compound is sodium monofluorophosphate. 11&. - Processo de acordo com a reivindicação 9, caracterizado por o humectante ser constituido_ por cerca de 20 a 30%, em peso, de uma mistura de polietileno glicol e pelo menos, 5% de sorbitol.11 &. 9. A composition according to claim 9, wherein the wetting agent comprises from 20 to 30% by weight of a mixture of polyethylene glycol and at least 5% of sorbitol. 12ê. - Processo de acordo com a reivindicação 9, caracterizado por se incluir tambem 1 a 10%, em peso, de glicerina, como estabilizador de fluoreto no humectante de polietileno glicol.12 e . A process according to claim 9, characterized in that 1 to 10% by weight of glycerin is included as the fluoride stabilizer in the polyethylene glycol humectant. 13â. - Processo de acordo com a reivindicação 2, caracterizado por a betaina ser cocoamidopropil betaina.13 â . A process according to claim 2, wherein the betaine is cocoamidopropyl betaine. 14â. - Processo de acordo com a reivindicação 1, caracterizado por o referido dèntifrico es tar isento de surfactantes não iónicos e aniónicos.14 â . 6. A process according to claim 1, wherein said diphenyl ether is free of nonionic and anionic surfactants. 15â. - Processo de acordo com a reivindicação 6, caracterizado por o abrasivo ser fosfato dicalcico.15 â . 6. A process according to claim 6, wherein the abrasive is dicalcium phosphate. -38I6â. - Processo de acordo com a reivindi cação 6, caracterizado por o abrasivo ser alumina.. 6. A process according to claim 6, characterized in that the abrasive is alumina. 17s. - Processo de acordo com a reivindicação 16, caracterizado por o abrasivo ser uma mistura de alumina hidratada e de alumina calcinada.17 sec . 6. A process according to claim 16, wherein the abrasive is a blend of hydrated alumina and calcined alumina.
PT78871A 1983-07-13 1984-07-09 Process for preparing stable antiplaque dentifrice with improved foaming and fluoride stability PT78871B (en)

Applications Claiming Priority (2)

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US06/513,474 US4490353A (en) 1983-07-13 1983-07-13 Antiplaque dentifrice with improved fluoride stability
US06/513,473 US4528182A (en) 1983-07-13 1983-07-13 Stable antiplaque dentifrice with improved foaming

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PT78871B true PT78871B (en) 1986-06-02

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ZA856445B (en) * 1984-09-10 1987-04-29 Colgate Palmolive Co Stable antiplaque dentifrice
US4574081A (en) * 1984-09-25 1986-03-04 Colgate-Palmolive Co. Antiplaque dentifrice having improved flavor
KR980000425A (en) * 1996-06-29 1998-03-30 이능희 Toothpaste foam
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US4098878A (en) * 1974-10-29 1978-07-04 Colgate-Palmolive Company Toothpaste containing milled alpha-alumina trihydrate
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US4130637A (en) * 1977-01-31 1978-12-19 Colgate-Palmolive Company Anti-plaque agents
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DK346784D0 (en) 1984-07-13
GB2143129B (en) 1987-07-01
NZ208730A (en) 1987-03-31
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FI79784B (en) 1989-11-30
IT1177897B (en) 1987-08-26
FI842808A (en) 1985-01-14
PT78871A (en) 1984-08-01
ZW10984A1 (en) 1985-02-20
KR850000965A (en) 1985-03-14
GB2143129A (en) 1985-02-06
IT8448567A0 (en) 1984-07-13
DK346784A (en) 1985-01-14
HK84890A (en) 1990-10-25
SE8403537L (en) 1985-01-14
IN161843B (en) 1988-02-13
KR910003554B1 (en) 1991-06-05
ES534252A0 (en) 1986-07-16
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NO165377B (en) 1990-10-29
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ES8608857A1 (en) 1986-07-16
GR81614B (en) 1984-12-11
IE841793L (en) 1985-01-13
AU565937B2 (en) 1987-10-01
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BR8403476A (en) 1985-06-25
IE57870B1 (en) 1993-05-05
CH660686A5 (en) 1987-06-15
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