BRPI0801811A2 - Manufacturing process of reduced fluoride toothpaste composition supplemented with calcium and / or phosphate and their dentifrice composition - Google Patents

Abstract

PROCESS OF MANUFACTURING COMPOSITION OF DENTIFICATION WITH REDUCED FLUORIDE CONCENTRATION SUPPLEMENTED WITH CALCIUM AND / OR PHOSPHATE AND RESPECTIVE COMPOSITION OF DENTIFICATION. Fluoridated dentifrices are effective in controlling tooth decay, but they increase the prevalence of dental fluorosis (decreased enamel mineralization and tooth dentin), when used in children under 6 years of age. The present invention provides a toothpaste formulation with reduced fluoride concentration (500 ppm F) in order to increase the effectiveness of the product when compared to the commercial toothpastes already tested (1000 to 1500 ppm F) and decrease the risk of occurrence of dental fluorosis. To achieve this goal, dentifrice is supplemented with a source of phosphate (sodium trimetaphosphate - TMP) at a concentration of 1%, or a source of calcium and phosphate (calcium glycerophosphate - CaGP) at a concentration of 0.25%, during the preparation of the product. The addition of these assets in the product does not insolubilize fluoride, as the compounds are insoluble in the mixture. As there is no interaction between the assets (fluoride sources with TMP, or with CaGP) the formulation is easy to manufacture without the addition of other technologies or formulas or container design to maintain the product's effectiveness. Antiplaque, bleaching and desensitizing agents can be added to the product. The product can be manufactured and marketed directly for consumption by pharmaceutical or cosmetic industries, not only being restricted to children, but also to adults, being considered a product for safe and effective family.

Description

"PROCESS FOR MANUFACTURING COMPOSITION WITH REDUCED CONCENTRATION OF CALCIUM AND / OR PHOSPHATE AND THEIR RESPECTIVEDENTIFICATIONPOSITION"

The present invention is a novel process of manufacturing low-fluoride toothpaste composition supplemented with calcium and / or phosphate and its dentifrice composition, of innovative design and endowed with important technological and functional improvements, according to the most modern concepts of dentistry and according to the required standards and specifications, having its own characteristics and fundamental requirements of novelty and inventive activity, resulting in a series of real and extraordinary technical, practical and economic advantages.

TECHNICAL STATE

1) COLGATEPALMOLIVE CO document US4343786 is extremely relevant as it deals with a composition for dentifrices containing alpha-albumin trihydrate containing within a concentration range of 500 - 1500 ppm which has a pH of 5.5 on average.

2o) HEDLEY THOMAS & CO LTD document GB845611 describes an invention which deals with the development of a toothpaste having a pH of 4 - 5.5 which contains sufficient materials so that when in contact with water it is capable of providing at least 25 parts of Fluoride at least 10 parts Tin ions per million parts toothpaste.

3) EKULF AB document US6375934 provides an educational system for identifying surface pH and makes it possible to determine an optimal pH for pasture application for each specific individual.

4o) US6143281 from SMITHKLINEBEECHAM PLC describes a toothpaste composition comprising a fluorine salt incorporated into this formulation in order to depress 100 - 3000 ppm fluorine.

5) US20060099153 to KATO; KAZUHIKO et al. refers to an oral hygiene preparation comprising an inorganic acid, a fluoride ion at a pH of 3 - 5.5.

6) MONSANTO COse US4721615 refers to a toothpaste composition based on decal phosphates.

7) SCHAEFFERHANS A US4983379 describes a method of preparing a parenteral composition consisting of fluorine, whether or not supplemented with phosphate, at a concentration of 200 - 3000 ppm.

8) AMERICANDENTAL ASS document US5993786 relates to a dentifrice composition based on the use of a phosphate supplemented fluorine source at a concentration of 200 - 2200 ppm.

9) COLGATEPALMOLIVE CO document US2006141039 relates to a camellia extract oral hygiene composition and a source of phosphate supplemented or non-phosphate which is capable of providing 25 - 2000 ppm concentration fluoride ion.

10 °) COLGATEPALMOLIVE CO document US2006286044 refers to an oral hygiene and anti-caries composition containing glycerophosphate in its composition and a source of fl uoride providing a concentration of 200 - 3000 ppm of fluoride in the medium.11 °) US2003152527 from PROCTER & GAMBLE relates to an oral hygiene composition based on a phosphate supplemented fluorine source that is capable of imparting fluoride at a concentration of 50 - 3500 ppm.

12 °) Procter & Gamble WO09621420 discloses a dentifrice composition comprising: a) from about 5% to about 50% by weight of sodium bicarbonate; b) a soluble fluoride ion source in an amount sufficient to provide from about 10ppm to about 3500ppm fluoride ion; c) at least about 1.5% by weight of tetrasodium pyrophosphate, of which some tetrasodium pyrophosphate is in the form of undissolved particles of anhydrous tetrasodium pyrophosphate; and d) from about 50% to about 94% of dentifrice carrier materials; and where further said decomposition has a soluble pyrophosphate ion content in the range 1 to about 100ppm. Further, it is said that a calcium source such as calcium carbonate, dicalcium orthophosphate, calcium pyrophosphate, tricalcium phosphate and decalcium polymetaphosphate may be added. Thus, it is possible to prepare the formulation of item b) described in the objective of this opinion - composition containing:

i. 450 ppm fluorine (amount between 10ppm and 3500ppm fluoride ion);

ii. calcium carbonate, dicalcium orthophosphate dihydrate, calcium pyrophosphate, tricalcium phosphate or calcium polymetaphosphate and

iii. phosphate - at least about 1.5% by weight of tetrasodium pyrophosphate.

In this regard, this document anticipates the composition described as an acidulated fluorine-containing dentifrice with a pH of 4.5.

13 °) Johnson & Johnson EP 0 162 574 discloses an oral hygiene composition comprising a pharmaceutical fluoride salt, zinc salt, buffering agent and a personal hygiene vehicle at a pH ranging from 3.5 to 6.0. Examples of acceptable fluoride salts are NaF, KF, LiF, AIF3, ZnF2, SnF2, sodium monofluorophosphate, acidulated phosphate fluoride, NH4F, among others. The amount of fluorine may range from 0.0025% to 4.0% by weight. It is therefore a very relevant document and should be studied in detail.

TECHNICAL STATE DEVELOPMENTS

In relation to the current state of products already on the market, this product has the same physical characteristics and main ingredients as abrasive, detergent, base, preservative, taste, etc. There are products that present calcium phosphate associated with fluoride, in a concentration above 1000 ppm F, but they are not more effective and have problems in the formulation that make their commercial production more expensive or impossible.

Also, there are dentifrices with lower concentrations of commercialized fluoride (550 ppm F) or no fluoride, but have reduced efficacy when compared to the product with 1100 ppm F. Discovery shows that the combination fluorine and calcium and phosphate sources have a sum of effects (synergism). when used at lower concentrations than those available on the market and achieving maximum efficacy with the concentrations described above. With a lower fluoride concentration there is a risky reduction in the occurrence of dental fluorosis when used in children aged 6 years. But it can also be used by adults, as the product is similar in effectiveness to the higher fluoride toothpastes (1100 ppm F). Another feature is that the products are insoluble in the formulation (they do not react with fluorine inactivating it), but show an (active) action during its use. This allows the formulation of products with different fluorine sources that can provide fluoride dentifrice in ionic form or not, making the formulation stable and with low production cost.

INNOVATIONS PURSUANT TO THIS PATENT

Fluoride dentifrices are effective in controlling tooth decay, but increase the prevalence of dental fluorosis (decreased enamel and tooth dentin mineralization) when used in children under 6 years of age. The present invention provides a low fluoride (500 ppm F) dentifrice formulation in order to increase the efficacy of the product when compared to the commercially tested dentifrices (1000 to 1500 ppm F) and to reduce the risk of dental fluorosis. dentifrice with a phosphate font (Sodium Trimetaphosphate - TMP) at a concentration of 1%, or a calcium and phosphate source (Calcium Glycerophosphate - CaGP) at a concentration of 0.25% during product preparation. The addition of these active substances in the product does not insolubilize the fluorine, because the compounds are insoluble in the mixture. As there is no interaction between the assets (fluoride sources with TMP or CaGP) the formulation is easy to manufacture without adding other technologies or formulas or container designs to maintain product effectiveness. To the product, antiplate, whitening and sensitizing agents may be added. The product can be manufactured and marketed directly for consumption by pharmaceutical or decosmetic industries, being not only restricted to children but also adults, being considered a safe and effective family product. This technology can be used in other dental products such as: mouthwash solutions, prophylactic pastes, gels, foams or varnishes for professional topical application or home use.

The present invention provides a dentifrice, cream or gel formulation with a low fluorine concentration and pH 7.3-8.0 in order to increase the effectiveness of the product in controlling dental caries and reducing the risk of dental fluorosis occurring.

In a particular embodiment the formulation comprises ingredients such as abrasives, for example calcium carbonate, calcium pyrophosphate (the use of carbonate or pyrophosphate is conditional upon the use of monofluorophosphate as fluorinated agent), but preferably abrasive and / or thickening silica, such as , sorbitol, glycerin, polyethylene glycol / or mixtures thereof, binders such as carboxymethylcellulose, gomaxanthan, thickening silica and / or mixture thereof, surfactants (betaines, preferably sodium lauryl sulfate and / or mixtures), preservatives (methylparaben, propylparaben or mixtures thereof) , fluoridating agents (sodium monofluorophosphate, titanium tetrafluoride, stannous fluoride, amine fluoride, preferably sodium fluoride), antiplaque agents (chlorhexidine, decetylpyridine chloride) and calcium and / or phosphate supplementation with organic acids, preferably sodium trimethophosphate and / or phosphates of calcium.

The concentrations of abrasive agents may vary from 4 to 50%, depending on the desired degree of abrasiveness. The humectants according to the composition of the present invention have concentrations ranging from 20 to 65%. Agglutinating ingredients comprise concentrations ranging from about 0.5 to 7%. Surfactants provide concentrations ranging from 1 to 6% of the composition. The concentrations of the preservatives used in the composition of the present invention may range from 0.01 to 0.5%. Fluorinated agents added to the present composition have concentrations that may range from 0 to 500ppm. Antiplate agents demonstrate concentrations ranging from 0.25 to 2% of the total composition. And because it is a composition supplemented with calcium and / or phosphate, the organic sources comprise a concentration which may range from 0.1 to 3% of the total composition.

The source of supplementation is preferably sodium trimetaphosphate which may range from 0.1 to 3% and / or calcium glycerophosphate which may range from 0.1 to 0.25% of the total composition. The presence of these compounds in the present invention represents a dual function in the formulation of the dentifrice. On the one hand, the compounds give rise to a highly supersaturated solution with respect to calcium, phosphate and fluoride ions in the environment (dental biofilm interface and dental enamel) and consequent process paralysis. demineralization of the enamel. In these conditions there is precipitation of fluorapatite, calcium fluoride, hydroxyapatite, amorphous calcium phosphate and other calcium phosphates, which is enamel remineralization phase and second function performed by the supplementation compounds. In the oral environment, hydroxyapatite and fluorapatite are the most stable crystalline phase containing calcium, phosphate and fluorine, precipitating a less soluble enamel. Thus ,emineralization involves the diffusion of calcium, phosphate and fluoride ions into incipient lesions, followed by precipitation of decalcium phosphate. The objective was to increase the diffusion and precipitation pattern by using high concentrations of calcium and phosphate to produce less acid-soluble apatite at low fluorine concentration. The present invention shows that even with the reduction of fluorine concentration there is no reduction in the aniogenic activity of the dentifrice, since the amount of fluoride present in the dentifrice is sufficient to catalyze the de-mineralized apatite reconstruction by saturation in the calcium and phosphate medium.

As for the fluorine-containing compound, sodium fluoride is preferably employed, and another may be used as already shown here. Other ions that may be useful for the dental structure may also be incorporated, such as iron, zinc, tin, titanium, aluminum and / or copper. The formulation disclosed herein has a fluorine concentration less than or equal to 500 ppm.

In a particular embodiment, the present application provides a process for obtaining the cream or gel dentifrice formulation from the steps: (A) separately mixing and homogenizing medium-density carboxymethylcellulose (CMC) to glycerine and / or propylene glycol, (B) solubilization, separate sodium saccharin in 20% water and add the mixture A, (C) solubilization, separately, sodium fluoride in 20% water and add the mixture A, (D) separate solubilization of methylparaben and propylparaben in 20 % water and add mixture A, (E) separate solubilization of sodium trimetaphosphate and / or calcium glycerophosphate in 20% water and add mixture A. Mix thoroughly until complete lump-free mixing.

In a second step of the process the steps are performed, (F) adding the total abrasive silica mixture and / or thickener, starting with the abrasive silica, (G) adding the total flavoring and / or flavoring mixture. Mix thoroughly until completely free of lumps in the total mixture. Then (H) is added sodium lauryl sulfate and / or sulfonated olefin under slow homogenization, preferably under vacuum.

EXAMPLES

<table> table see original document page 10 </column> </row> <table> There is no known process of manufacturing low-fluoride-concentrated toothpaste composition supplemented with calcium and / or phosphate that together, all the constructive characteristics described above, and which directly or indirectly is or was as effective as the process and dentifrice composition object of the present patent.

It is, therefore, a process and a composition of great importance to the intended purpose, which consists of an unprecedented way of obtaining a dentifrice, fully fulfilling the proposed objectives and fulfilling the intended functions in a practical and efficient manner, providing a series of inherent advantages to its purpose. applicability, having their own characteristics, innovative and endowed with fundamental requirements of novelty and inventive activity, required for patent protection to appear.

Claims (6)

1. - "PROCESS FOR MANUFACTURING DENTIFICATION COMPOSITION WITH REDUCED CALCIUM AND / OR PHOSPHATE FLUORS CONCENTRATION", characterized by the fact that it consists of the following steps: (A) mix and homogenize separately the carboxymethyl cellulose (CMC) glens to give and / or propylene glycol, (B) separate solubilization of sodium saccharin in 20% water and add mixture A, (C) separate solubilization of sodium fluoride in 20% water and add mixture A, (D ) Separate solubilization of methylparaben and propylparaben in 20% water and increasing the mixture A, (E) Solubilization separately with sodium trimethophosphate and / or calcium glycerophosphate in 20% water and adding the mixture well. total lumpiness in the total mixture; 2. - "PROCESS FOR MANUFACTURING COMPOSITION WITH REDUCED CALCIUM AND / OR PHOSPHATE FLOOR CONCENTRATION", according to claim 1, characterized in that in a second stage it consists of, (F) adding the total mixture of abrasive silica and / or thickening, starting with the abrasive silica, (G) adding to the total mix flavoring and / or flavoring, thoroughly mixing the mixture until total lump-freeness in the total mixture, so that (H) is then added sodium lauryl sulfate and / or sulfonated olefin, under slow homogenization, preferably under vacuum; 3. - "CALCIUM / PHOSPHATE SUPPLEMENTED FLUORINE REDUCED CONCENTRATION COMPOSITION", characterized in that it consists of a dentifrice formulation with reduced fluorine concentration (500 ppmF), supplemented with a phosphate dentifrice (sodium dephosphate) - TMP) at a concentration of 1%, or a calcium and phosphate source (CaGP) at a concentration of 0,25% during the preparation of the product, so that anti-plate, bleaching and sensitizing agents may be added; 4. - "CALCIUM / PHOSPHATE SUPPLEMENTED FLUORINE DENTURE COMPOSITION", characterized by the fact that it consists of a dentifrice, cream or gel formulation with a low concentration of fluorine and pH 7,3-8,0. ingredients such as abrasives, for example calcium carbonate, calcium pyrophosphate, the use of carbonate or pyrophosphate being conditional upon the use of demonofluorophosphate as a fluorinated agent, but preferably abrasive silica and / or thickener, such as sorbitol, glycerine, polyethylene glycol. and / or mixtures thereof, carboxymethylcellulose binders, xanthan gum, thickener and / or mixed silica, surfactants (betaines, preferably sodium lauryl sulfate and / or mixture thereof), preservatives (methylparaben, propylparaben or mixture thereof), fluorinated agents (monofluorophosphate) sodium chloride, titanium tetrafluoride, stannous fluoride, amine fluoride, preferably sodium), antiplaque agents (chlorhexidine, cetylpyridine chloride) and calcium and / or phosphate supplementation with organic acids, preferably sodium trimethophosphate and / or calcium glycerophosphate; 5. - "CALCIUM / PHOSPHATE SUPPLEMENTED FLUORINE DENTAL COMPOSITION COMPOSITION", characterized in that the concentrations of abrasive agents vary from 4 to 50%, depending on the desired degree of abrasion; humectants have concentrations ranging from 20 to 65%; binder ingredients comprised of concentrations ranging from about 0.5 to 7%; surfactants that provide concentrations ranging from 1 to 6% of the composition; preservative concentrations ranging from 0.01 to 0.5%; fluoridating agents added to the present composition have concentrations ranging from 0 to 500ppm; antiplaque agents at concentrations ranging from 0.25 to 2% of the total composition; a calcium and / or phosphate supplemented composition, the organic sources of which comprise a concentration that may range from 0.1 to 3% of the total composition; 6. - "CALCIUM AND / OR PHOSPHATE SUPPLEMENTED FLUORINE REDUCED CONCENTRATION", characterized by the fact that the source of supplementation preferably refers to sodium trimetaphosphate which may vary from 0.1 to 3% and / or calcium glycerophosphate. 0.1 to 0.25% of the total composition, so that the presence of these compounds represents a dual function in the formulation of the dentifrice, on the one hand, the compounds give a highly supersaturated solution with respect to calcium, phosphate and fluorine ions in the toothpaste. environment (dental biofilm interface and dental enamel) and consequent paralysis of the enamel demineralization process (dental caries and erosion), and under these conditions there is appreciation of fluorapatite, calcium fluoride, hydroxyapatite, amorphous calcium phosphate and other calcium phosphates. is the enamel deremineralization phase and the second function exerted by the supplementation whereas, in the oral environment, hydroxyapatite and fluorapatite are the most stable crystalline phase that contains calcium, phosphate and fluorine, precipitating a less soluble enamel, and remineralization involves the diffusion of calcium ions, fluorine phosphates into incipient lesions, followed by precipitation of calcium phosphate; - "CALCIUM / PHOSPHATE SUPPLEMENTED FLUORINE REDUCED CONCENTRATION COMPOSITION", characterized in that the fluorine-containing compound is preferably used as sodium fluoride and may be used as shown here, and may still be incorporated herein. other ions that may be useful for dental structure, such as iron, zinc, tin, titanium, aluminum and / or copper, the formulation disclosed herein having a fluorine concentration of 500 ppm or less.