WO2022072605A1

WO2022072605A1 - Oral care compositions with improved stability

Info

Publication number: WO2022072605A1
Application number: PCT/US2021/052831
Authority: WO
Inventors: Yuqiu ZHU; Christoph SCHLUETER; Elena DRAGANOIU; Liliana Miinea
Original assignee: Lubrizol Advanced Materials, Inc.
Priority date: 2020-09-30
Filing date: 2021-09-30
Publication date: 2022-04-07

Abstract

In one aspect, the present technology generally relates to the use of alkoxylated methyl glucosides as a humectant component replacement in oral care compositions. More specifically, the disclosed technology relates to stable dentifrice compositions having desirable rheology properties comprising i) a humectant selected from an alkoxylated methyl glucoside; ii) a dental abrasive component; iii) a thickener component; iv) a detersive surfactant; iv) a fluoride ion source; and optionally iv) water.

Description

ORAL CARE COMPOSITIONS WITH IMPROVED STABILITY

TECHNOLOGICAL FIELD

[0001] The present technology generally relates to the use of alkoxylated methyl glucosides as a humectant component in oral care compositions. More specifically, the disclosed technology relates to stable dentifrice compositions having desirable rheology properties comprising i) a humectant selected from an alkoxylated methyl glucoside; ii) a dental abrasive component; iii) a thickener component; iv) a detersive surfactant; iv) a fluoride ion source; and optionally iv) water.

BACKGROUND

[0002] For consumer satisfaction, it is necessary that dentifrice compositions possess certain physical properties to which the consumer is accustomed. These properties provide a dentifrice that has appealing taste, has good cleansing effect, is easy to rinse, has excellent mouth feel, and has physical stability. Dentifrice compositions with acceptable physical stability do not readily harden on the shelf and do not exhibit phase separation such as water or flavor separation. The appearance of the paste as it comes out of the dispenser is also considered important. The dentifrice should appear smooth and have a pleasant sheen or glossy appearance. Moreover, the dentifrice should be resistant to drying when the dispensing container (e.g., tube or pump dispenser) is left open to the environment, importantly, these properties must be provided in a dentifrice composition that is cost effective for the consumer. Accordingly, there is a continuing demand to provide dentifrice compositions at lower cost while maintaining stability, rheological properties as well as aesthetics. This is especially important in parts of the world where dentifrice is unaffordable. In general, there is a need to reduce the amount of ingredients in a dentifrice formulation with the associated cost reduction and positive environmental impact. [0003] Dentifrice compositions typically contain a humectant, a binder or thickener, a polishing agent or abrasive (abrasive silica or a calcium containing compound such as caicium carbonate), a detergent or surfactant and water, as weli as materials that provide therapeutic or cosmetic benefits, such as fluorides, flavorings, and sweeteners. Other than water, the predominant components of dentifrices are the abrasive and the humectant system. For exampie, in recent years the most common dentifrices in the market contain 10 wt.% or higher abrasive and 20 wt.% up to about 80 wt.% of humectants. Compared to the cost of the other ingredients, water is relatively inexpensive. One way to iower the cost of a dentifrice composition is to increase the water content in the formulation. However, a reiativeiy high-water content often produces problems of iow viscosity and/or phase separation. With a high moisture dentifrice, the consumer may notice “wet cap” or fiavor concentration in the tip depending on whether fiiied tubes were stored with the capped ends up or down. Phase separation may aiso adversely affect the sheen or gloss of the extruded dentifrice composition.

[0004] Another cost savings approach is to reduce the amount of components other than water in the dentifrice formuiation. As the humectant component is one of the main ingredients (in terms of usage amount) compared to the reiativeiy minor amounts of other dentifrice components, reduction of the amount of humectant in the formuiation to create a more economical dentifrice is an option. However, a iarge reduction in the humectant ievei in a dentifrice brings a concomitant drop in desirable physicai and aesthetic properties of the dentifrice formulation.

[0005] The humectant serves to keep dentifrice compositions from hardening or crystallizing upon exposure to air, to give compositions a moist feei to the mouth, and to impart desirabie sweetness. The humectants comprise one or more iiquids which aiong with water and/or other soivents make up the carrier phase in which other dentifrice ingredients particularly insoiubie abrasives are dispersed to provide a stable paste. An important function of humectants is to siow the dentifrice from drying out due to evaporation of water or other volatile materials when the dentifrice dispenser is left open during storage and/or upon use of product by the consumer. A problem that can arise with dentifrice products packaged in squeeze tubes is the cementing of the cap to the tube during use of the product by the consumer. This can occur, for exampie, when dentifrice unintentionally gets onto the threads of the tube and the tube is ieft undisturbed for a iong period of time. This problem is caiied cap iock and is due to the crystallization of solid material in the dentifrice. In order to prevent cap lock, humectants are added to dentifrices in order to preserve moisture and prevent crystaiiization. A related probiem is caused by the cap not being replaced between uses. The paste in the nozzle of the tube can dry out if appropriate humectants are not present in the dentifrice in effective amounts. Dental rinses are also formulated with humectants because of the mouth feel and taste benefits they provide. Typical humectants that have been used in dentifrice and rinse compositions include edible poiyhydric alcohols such as glycerin, sorbitol, xylitol, propylene glycol, butylene glycoi, polyethylene glycol and polypropylene glycol.

[0006] The most commonly used liquid humectants are glycerin, 70% aqueous sorbitol and mixtures thereof. One advantage of glycerin and sorbitoi is that they are essentially not fermentable by cariogenic bacteria. Other humectants that have been suggested such as maltodextrins are fermentable by cariogenic bacteria and are thus less suitable. Another advantage of glycerin and sorbitol is the ability to be formulated in clear or translucent gels by virtue of having a refractive index similar to the refractive index of the abrasive component, particularly silica. In both opaque pastes and transparent gels, the level of glycerin and/or sorbitol must remain relatively high to effectively inhibit drying out of the composition and provide the mouth feel benefits. High levels of humectant, particularly glycerin and sorbitol are undesirable because of high and rapidly increasing cost. Significant cost reduction can be achieved if part or all the humectant(s) can be eliminated.

[0007] International Patent Application Pub. No. WO 2014/170096 A1 discloses an attempt to lower the amount of humectant to provide a cost- effective dentifrice formulation. It is reported that: “...as expected, drastic reduction in humectants led to products with poorer sensory properties which may not find consumer acceptance. This posed a technical problem of how to balance the sensory properties whilst still being able to minimize costs.” By reducing the amount of thickening silica and introducing smectite clay into the dentifrice composition provides the objective of providing a cost-effective dentifrice formulation with requisite sensory properties was met.

[0008] United States Patent Application Pub. No. US 2009/0269287 A1 discloses oral care compositions, such as thickened dentifrices in liquid, paste or gel form comprising a binding/thickening system that also functions effectively as a humectant agent thereby replacing a significant portion or all of traditional humectant components such as glycerin, sorbitol and other polyols. The binding/thickening system comprises select carrageenans that are effective water-binding agents to prevent significant water loss from the composition when exposed to air to cause unacceptable drying out.

[0009] In one aspect, the present technology provides oral care products comprising alkoxylated methyl glucosides which function effectively as a humectant and replaces a significant portion or all of the polyol humectants heretofore employed in oral care formulations thereby simplifying formulation and reducing cost, while maintaining desired properties including moisture retention, texture and mouthfeel

SUMMARY OF THE DISCLOSED TECHNOLOGY

[0010] The present technology is based on the discovery that certain alkoxylated methyl glucosides have improved humectant properties at reduced use levels and thus can replace all or at least part of traditional polyol humectants, particularly glycerin and sorbitol, in dentifrice compositions.

[0011] In one aspect, the present technology relates to a dentifrice composition comprising: i) a humectant component comprising an alkoxylated methyl glucoside in an amount ranging from about 4 to about 20 wt. %; or from about 6 to about 18 wt.%, or from about 8 to about 17 wt.%, or from about 10 to about 16 wt.%, or from about 12 to about 14 wt.%; ii) a dental abrasive component selected from a calcium containing abrasive, an abrasive silica, and mixtures thereof, wherein said dental abrasive is present in an amount ranging from about 5 to about 50 wt.%, or from about 10 to about 45 wt.%, or from about 15 to about 40 wt.%, or from about 20 to about 35 wt.%; iii) a thickener component in an amount ranging from about 0.1 to about 10 wt. %, or from about 0.5 to about 8 wt.%, or about 0.75 to about 5 wt.%, or from about 1 to about 2.5 wt.%; iv) a detersive surfactant component in an amount ranging from about 0.25 to about 2.5 wt.%, or from about 0.4 to about 1 wt.%, or about 1 .25 to about 2 wt.%; v) a fluoride ion source in an amount ranging from about 0.1 to about 2 wt.%, or from about 0.25 to about 1 .75 wt.%, or about 0.5 to about 1.5 wt.%, or from about 0.75 to about 1 .25 wt.%; and optionally vi) water in an amount ranging from about 0 to 50 wt.%, or from about 1 to about 45 wt.%, or from about 5 to about 40 wt.%, or from about 10 to about 35 wt.%, or from about 15 to about 25 wt.%, wherein all weight percentages are based on the weight of the total composition.

[0012] In one aspect, the present technology relates to a dentifrice composition comprising: i) a humectant component comprising an alkoxylated methyl glucoside in an amount ranging from about 4 to about 20 wt.%; or from about 6 to about 18 wt.%, or from about 8 to about 17 wt.%, or from about 10 to about 16 wt.%, or from about 12 to about 14 wt.%; ii) a dental abrasive component in an amount ranging from about 5 to about 50 wt.%, or from about 10 to about 45 wt.%, or from about 15 to about 40 wt.%, or from about 20 to about 35 wt.%; iii) a thickener component in an amount ranging from about 0.1 to about 10 wt. %, or from about 0.5 to about 8 wt.%, or about 0.75 to about 5 wt.%, or from about 1 to about 2.5 wt.%; iv) a detersive surfactant component in an amount ranging from about 0.25 to about 2.5 wt.%, or from about 0.4 to about 1 wt.%, or about 1 .25 to about 2 wt.%; v) a fluoride ion source in an amount ranging from about 0.1 to about 2 wt.%, or from about 0.25 to about 1 .75 wt.%, or about 0.5 to about 1.5 wt.%, or from about 0.75 to about 1 .25 wt.%; and optionally vi) water in an amount ranging from about 0 to 50 wt.%, or from about 1 to about 45 wt.%, or from about 5 to about 40 wt.%, or from about 10 to about 35 wt.%, or from about 15 to about 25 wt.%, wherein all percentages are based on the weight of the total composition.

[0013] In one aspect, the present technology relates to a translucent dentifrice or gel composition comprising: i) a humectant component comprising an alkoxylated methyl glucoside polyol in an amount ranging from about 4 to about 20 wt.%, or from about 5 to about 18 wt.%, or from about 6 to about 16 wt.%, or from about 7 to about 14 wt.%, or from about 8 to about 12 wt.%; ii) an abrasive silica component in an amount ranging from about 5 to about 50 wt.%, or from about 10 to about 45 wt.%, or from about 15 to about 40 wt.%, or from about 20 to about 35 wt.%; iii) a thickener component in an amount ranging from about 0.1 to about 10 wt. %, or from about 0.5 to about 8 wt.%, or about 0.75 to about 5 wt.%, or from about 1 to about 2.5 wt.%; iv) a detersive surfactant component in an amount ranging from about 0.25 to about 2.5 wt.%, or from about 0.4 to about 1 wt.%, or about 1 .25 to about 2 wt.%; v) a fluoride ion source in an amount ranging from about 0.1 to about 2 wt.%, or from about 0.25 to about 1 .75 wt.%, or about 0.5 to about 1.5 wt.%, or from about 0.75 to about 1 .25 wt.%; and optionally vi) water in an amount ranging from about 0 to 50 wt.%, or from about 1 to about 45 wt.%, or from about 5 to about 40 wt.%, or from about 10 to about 35 wt.%, or from about 15 to about 25 wt.%, wherein all percentages are based on the weight of the total composition.

[0014] In one aspect, the present technology relates to a dentifrice composition comprising: i) a humectant component comprising an alkoxylated methyl glucoside in an amount ranging from about 4 to about 15.5 wt.%, or from about 5 to about 15 wt.%, or from about 6 to about 14 wt.%, or from about 7 to about 12 wt.%, or from about 8 to about 10 wt.%.; ii) a calcium carbonate abrasive component in an amount ranging from about 5 to about 50 wt.%, or from about 10 to about 45 wt.%, or from about 15 to about 40 wt.%, or from about 20 to about 35 wt.%; iii) a thickener component in an amount ranging from about 0.1 to about 10 wt. %, or from about 0.5 to about 8 wt.%, or about 0.75 to about 5 wt.%, or from about 1 to about 2.5 wt.%; iv) a detersive surfactant component in an amount ranging from about 0.25 to about 2.5 wt.%, or from about 0.4 to about 1 wt.%, or about 1 .25 to about 2 wt.%; v) a fluoride ion source in an amount ranging from about 0.1 to about 2 wt.%, or from about 0.25 to about 1 .75 wt.%, or about 0.5 to about 1.5 wt.%, or from about 0.75 to about 1 .25 wt.%; and optionally vi) water in an amount ranging from about 0 to 50 wt.%, or from about 1 to about 45 wt.%, or from about 5 to about 40 wt.%, or from about 10 to about 35 wt.%, or from about 15 to about 25 wt.%, wherein all percentages are based on the weight of the total composition.

Detailed Description of the Disclosed Technology

[0015] In all aspects of the disclosed technology all percentages are calculated by the weight of the total composition. All ratios are expressed as weight ratios. All numerical ranges of amounts are inclusive and combinable unless otherwise specified. [0016] While overlapping weight ranges for the various components and ingredients that can be contained in the disclosed compositions have been expressed for selected embodiments and aspects of the disclosed technology, the amount of each component in the disclosed compositions is selected from its disclosed range such that the sum of all components or ingredients in the composition will total 100 weight percent. The amounts employed will vary with the purpose and character of the desired product and can be readily determined by one skilled in the art.

[0017] All percentages, ratios, and levels of components referred to herein are based on the actual amount of the component, and do not include solvents fillers, or other materials with which the component may be combined as commercially available product, unless otherwise indicated.

[0018] The dentifrice compositions of the disclosed technology may suitably comprise, consist essentially of, or consist of, the components, elements, and process delineations described herein. The disclosed technology illustratively disclosed herein suitably may be practiced in the absence of any element which is not specifically disclosed herein.

[0019] As defined herein, “stable” and “stability” means that no visible phase separation is observed for a period of at least about one week of storage, or at least about 1 month of storage, or at least about 6 months of storage at ambient room temperature (20 to about 25 °C). In another aspect, the products of the disclosed technology show no visible phase separation after about at least four weeks, or at least about 6 weeks, or at least about 8 weeks, or at least about 12 weeks of storage at about 45 °C.

[0020] The term “dentifrice” as used herein means paste, gel, powder, tablets, or liquid formulations, unless otherwise specified, that are used to clean the surfaces of the oral cavity and may be in the form of toothpaste, tooth gel, tooth powders, tablets, foams, strips and rinses. In one aspect the dentifrice is a toothpaste or tooth gel.

[0021] The components of the compositions of the present technology are described in the following paragraphs. Alkoxylated Methyl Glucoside

In one aspect, the humectant component comprises, consists essentially of, or consists of an alkoxylated methyl glucoside polyol. In certain aspects, the alkoxylated methyl glucoside is alkoxylated with ethylene and/or propylene oxide. In certain aspects, the alkoxylated methyl glucoside polyol is a mixture of ethoxylated methyl glucoside and propoxylated methyl glucoside polyols. In one aspect, the alkoxylated methyl glucoside polyols suitable for use in the present technology have an average degree of alkoxylation of about from about 7 to about 25, or from about 8 to about 15, or from about 9 to about 12, or about 10. [0022] In one aspect, the alkoxylated methyl glucoside polyol is an ethoxylated methyl glucoside polyol represented by the formula:

wherein the sum of w + x + y + z averages from about 7 to about 25, or from about 8 to about 15, or from about 9 to about 12, or about 10.

[0023] Examples of commercially available alkoxylated methyl glucoside polyols are (INCI) Methyl Gluceth-10, Methyl Gluceth-20, PPG-10 Methyl Glucose Ether, and PPG-20 Methyl Glucose Ether, available from Lubrizol Advanced Materials, Inc., under the trade names, Glucam™ E-10, Glucam™ E- 20, Glucam™ P-10, and Glucam™ P-20, respectively. [0024] In one aspect, a suitable alkoxylated methyl glucoside is Methyl Gluceth-10. Methyl Gluceth-10 is methyl glucoside alkoxylated with an average of 10 moles of ethylene oxide.

[0025] In one aspect, the alkoxylated methyl glucoside polyol is present in an amount ranging from about 4 to about 20 wt. %; or from about 6 to about 18 wt.%, or from about 8 to about 17 wt.%, or from about 10 to about 16 wt.%, or from about 12 to about 14 wt.%, based on the total weight of the dentifrice composition.

Dental Abrasives

[0026] Dental abrasives useful in the compositions of the present technology include many different materials. The material seiected must be one which is compatibie within the other components in the composition of interest and does not excessively abrade dentin. Suitable abrasives include, for example, silicas including gels and precipitates; insoluble sodium polymetaphosphate; hydrated alumina; calcium containing compounds including calcium carbonate, sodium carbonate, sodium bicarbonate, dicalcium orthophosphate dihydrate, calcium pyrophosphate, tricalcium phosphate, calcium polymetaphosphate, caicium oxapatite; resinous abrasive materials such as particulate condensation products of urea and formaldehyde; and mixtures thereof.

[0027] Other abrasives suitable for use in the compositions of the present technology is the particulate thermo-setting polymerized resins as described in United States Patent No. 3,070,510. Suitable resins include, for example, melamines, phenolics, ureas, melamine-ureas, melamine-formaldehydes, urea- formaldehyde, melamine-urea-formaldehydes, cross-linked epoxides, and cross- linked polyesters.

[0028] In one aspect, the dental abrasive is selected from calcium carbonate. Suitable sources include finely ground natural chalk (FGNC), ground calcium carbonate, precipitated calcium carbonate, and combinations thereof. Calcium carbonate abrasives are generally used in dentifrice compositions such as toothpastes that do not require a translucent to ciear appearance, i.e., are opaque.

[0029] In one aspect the calcium carbonate is selected from FGNC obtained from limestone or marble. FGNC may also be modified chemically or physically by coating during milling or after milling by heat treatment. Typical coating materials include magnesium stearate or oleate. The morphology of FGNC may also be modified during the milling process by using different milling techniques, for example, bail milling, air-classifier miliing or spiral jet milling. One example of natural chalk is described in International Patent Appiication Pub. No. WO 03/030850 having a medium particle size of 1 to 15 microns and a BET (Brunauer, Emmett and Teller) surface area of 0.5 to 3 m²/g. The natural calcium carbonate may have a particle size of 325 to 800 mesh, alternatively a mesh size selected from 325, 400 600, 800, or combinations thereof. Alternatively, the particle is from about 0.1 to about 30 microns, or from about 0.1 to about 20 microns, or from about 5 to about 20 microns.

[0030] In one aspect, the dental abrasive is selected from an abrasive silica. Dental siiica abrasives of various types are well-known in the art and possess the unique benefits of exceptional dental cleaning and polishing performance without unduly abrading tooth enamel or dentine. Moreover, silica abrasives are generally empioyed in the formulation of clear to translucent dentifrices such as toothpastes and tooth gels because their refractive indices are similar to the refractive indices of the clear to translucent carrier components used in the formulation.

[0031] The silica dental abrasives polishing materials herein, as well as other abrasives, generally have an average particle size ranging between about 0.1 to about 30 microns, or from about 5 to about 20 microns. The abrasive can be precipitated silica or silica gels such as the silica xerogels described in United States Patent No. 3,538,230 and United States Patent No. 3,862,307. Commercially availabie examples include the silica xerogeis marketed under the trade name Syloid ™ by the W.R. Grace and Co. and precipitated silica abrasive materials marketed by Evonik Corporation under the trade name, Zeodent™, particularly the silicas carrying the designation Zeodent™ 113, Zeodent™ 115, Zeodent™ 124 and Zeodent™ 623. The types of silica dental abrasives useful in the toothpastes of the present technoiogy are described in more detail in United States Patent Nos. 4,340,583; 5,603,920; 5,589,160; 5,658,553; 5,651 ,958; and 6,740,311.

[0032] It is to be noted that there are two types of silica that can be used in toothpaste and tooth gel compositions. As discussed above silica is used as a dental abrasive. However, certain silicas may also be used as a thickener. The difference between the two types of silica is discussed in United States Patent No. 6,342,205 (see Tables B and C and the accompanying disclosure), the disclosure of which is hereby incorporated by reference in its entirety. Generally, abrasive silicas have an oil absorption value ranging from about 50 to about 125 cm³/100 g, a pore volume ranging from about 1.5 to about 3 cm³/g, a pore density ranging from about 0.2 to about 0.3 g/cm³, and a pack density ranging from about 0.35 to about 0.45 g/cm³. In contrast, thickening silicas have higher oil absorption values, higher pore volumes, lower pore densities and lower pack densities than the abrasive silicas, wherein oil absorption value, pore volume, pore density and pack density is measured as set forth in columns 3 to 5 of United States Patent No. 6,342,205 supra.

[0033] Mixtures of abrasives can be used such as, for example, mixtures of the various grades of Zeodent™ silica abrasives listed above. In one aspect, the total amount of abrasive component in the dentifrice compositions of the present technology typically range from about 5 to about 50 wt.%, or from about 10 to about 45 wt.%, or from about 15 to about 40 wt.%, or from about 20 to about 35 wt.%, based on the total weight of the composition. Toothpastes and tooth gels typically contain from about 10% to about 50% of abrasives. Dental solutions, mouth sprays, mouthwashes typically contain little or no abrasive.

Thickener

[0034] The thickener provides a desirable consistency and/or stabilizes and/or enhances the performance of the dentifrice composition. The thickener used in the compositions of the present technology is limited only to the extent that it may be added to a composition suitable for use in the oral cavity and provides desirable release of active components to the oral cavity. Suitable thickeners include cellulose derivatives (“cellulose gums”) such as carboxymethyl cellulose (CMC) and salts thereof (e.g., sodium CMC), methyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, bacterial fermentation derived cellulose (FDC), microfibrous cellulose (MFC), and mixtures thereof; polyvinyl pyrrolidone; polyethylene glycol; xanthan; carrageenans such as iota-carrageenan, kappa-carrageenan, kappa2- carrageenan, lambda-carrageenan, and mixtures thereof; guar gum; gum karaya; gum arable; gum tragacanth: and mixtures thereof: carboxyvinyl polymers such as Carbomers (crosslinked polyacrylic acid) and crosslinked copolymers of (meth)acrylic acid and C2 to Cso alkyl esters of (meth)acrylic acid; and silica.

[0035] Polyethylene glycol (PEG) is available in various ranges of average molecular weights. In one aspect, suitable PEG materials have an average molecular weight ranging from about 200 to about 1600 Daltons, or from about 300 to about 1000 Daltons, or from about 400 to about 800 Daltons, or from about 500 to about 700 Daltons. PEG is commercially available under the Carbowax™ trade name marketed by the Dow Chemical Company.

[0036] Carbomers are commercially available under the Carbopol™ trade name marketed by Lubrizol Advanced Materials, Inc. under product designations 956, 971 P NF, 974P NF and 980 NF. Commercially available carboxyvinyl copolymers are commercially available under the Carbopol tradename marketed by Lubrizol Advanced Materials, Inc. under product designation ETD 2020 (INCI: Acrylates/C 10-30 Alkyl Acrylate Crosspolymer).

[0037] FDC can be obtained from Sphingomonas ferment extract (commercially available as Kelco Care™ Diutan gum). Kelco Care™ Diutan gum is a natural high molecular weight polysaccharide with a low anionic charge density produced by fermentation of the mircrorganism, Sphingomonas sp. ATCC 53159. It is comprised of six sugar units of d-glucose, d-glucuronic acid, d-glucose (with 2 l-rhamnose in the side chain) and l-rhamnoses, forming a linear backbone with a repeating side chain. Diutan gum has high molecular weight (typically millions of kD) and thus long molecular chain length. This leads to Diutan gum polymer chain entanglement at relatively low concentrations in solution. The structured network of entangled, stiff molecules creates high viscosity at low shear rates, resulting in outstanding suspension properties. The molecules in the complex network of a Diutan gum formulation are weakly associated. This network is progressively disrupted under the influence of applied shear stress making diutan gum solutions highly pseudoplastic. This rheology behavior makes Sphingomonas ferment extract (Kelco Care™ Diutan gum) a robust candidate as a thickener and stabilizing agent in challenging dentifrice formulations such as low or high pH, high ion content or in natural formulations.

[0038] Microfibrous cellulose can be prepared by mechanically disrupting/altering cereal, wood, or cotton-based cellulose fibers, and is commercially available under the Betafib™ trade name supplied by Royal Cosun.

[0039] As discussed previously, thickening silicas are differentiated over abrasive silicas by having higher oil absorption values, higher pore volumes, lower pore densities and lower pack densities than the abrasive silicas. In one aspect, thickening silicas have an oil absorption value ranging from about 150 to about 225 cm³/100 g, a pore volume ranging from about 3.5 to about 6.5 cm³/g, a pore density ranging from about 0.1 to about 0.15 g/cm³, and a pack density ranging from about 0.1 to about 0.25 g/cm³. As mentioned previously oil absorption values, pore volumes, pore densities and pack densities are measured as set forth in columns 3 to 5 of United States Patent No. 6,342,205 supra. Silica thickener materials are marketed by Evonik Corporation under the trade name, Zeodent™, particularly the silicas carrying the designation Zeodent™ 153, Zeodent™ 163 and Zeodent™ 165.

[0040] In one aspect, the thickener can be selected from the individual thickeners listed above, or mixtures of two or more thickeners selected from the list above can be utilized in the compositions of the present technology. In one aspect, the thickener component is present in the dentifrice compositions of the present technology in an amount ranging from about 0.1 to about 10 wt. %, or from about 0.5 to about 8 wt.%, or about 0.75 to about 5 wt.%, or from about 1 to about 2.5 wt.%, based on the total weight of the composition.

Surfactant

[0041] In one aspect, the dentifrice compositions of the present technology comprise at least one orally acceptable detersive surfactant. Surfactants enhance stability of a dentifrice composition, help clean the oral cavity surfaces through detergency, and provide foam upon agitation, e.g., during brushing with an oral care product of the disclosure, e.g., toothpastes and tooth gels. Surfactants facilitate the efficacy of dentifrice active components such as anti- caries agents and Whiteners by thoroughly dispersing these materials throughout the oral cavity. The detersive surfactant component can be selected from an anionic surfactant, an amphoteric surfactant, a nonionic surfactant, and mixtures thereof.

[0042] In one aspect, the surfactant may comprise an anionic surfactant. Suitabie anionic surfactants include without limitation water-soluble salts of C₈- C₂₀ alkyl sulfates, sulfonated monoglycerides of C₈-C₂₀ fatty acids, sarcosinates, taurates, and the like. Illustrative examples include, but are not limited to sodium lauryl sulfate, sodium cocoyl monoglyceride sulfonate, sodium lauryl sarcosinate, sodium lauryl isoethionate, sodium laureth carboxylate, and sodium dodecyl benzenesulfonate.

[0043] In one aspect, the surfactant may comprise an amphoteric surfactant. Suitable amphoteric surfactants include without limitation alkyl betaines, e.g., lauryl betaine, coco betaine; alkylamido betaines, e.g., cocam idopropyl betaine and cocohexadecyl dimethylbetaine; alkylamido sultaines, e.g., cocam idopropyl hydroxysultaine; (mono- and di-) amphocarboxylates, e.g., sodium cocoamphoacetate, sodium lauroamphoacetate, sodium capryloamphoacetate, disodium cocoamphodiacetate, disodium lauroamphodiacetate, disodium caprylamphodiacetate, disodium capryloamphodiacetate, disodium cocoamphodipropionate, disodium lauroamphodipropionate, disodium caprylamphodipropionate, disodium capryloamphodipropionate, C8-C22 alkyl amine oxides, e.g., octyldimethylamine oxide, decyldimethylamine oxide, dodecyldimethylamine oxide, iso-dodecyldimethyl amine oxide, myristyldimethylamine oxide, myristyl/cetyldimethylamine oxide, myristyldimethylamine oxide, cocodimethylamine oxide; and mixtures thereof. [0044] In one aspect, the surfactant may comprise a nonionic surfactant. Suitable nonionic surfactants include without limitation poloxamers, polyoxyethylene sorbitan esters, polysorbates, fatty alcohol ethoxylates, alkylphenol ethoxylates, tertiary amine oxides, tertiary phosphine oxides, dialkyl sulfoxides and the like.

[0045] In one aspect, the surfactant may comprise a cationic surfactant. Suitable cationic surfactants include without limitation stearyldimenthylbenzyl ammonium chloride; dodecyltrimethylammonium chloride; nonylbenzylethyldimethyl ammonium nitrate; tetradecylpyridinium bromide; laurylpyridinium chloride; cetylpyridinium chloride; laurylpyridinium chloride; laurylisoquinolium bromide; ditallow (Hydrogenated) dimethyl ammonium chloride; dilauryldimethyl ammonium chloride; and stearaikonium chloride, and mixtures thereof.

[0046] In one aspect, the surfactant comprises an anionic surfactant, an amphoteric surfactant and a nonionic surfactant.

[0047] In one aspect the amount of surfactant present in the dentifrice compositions of the present technology range from about 0.1 to about 5 wt.%, or from about 0.25 to about 2.5 wt.%, or from about 0.4 to about 2.5 wt., or about from about 1 to about 2 wt.%, based on the total weight of the composition.

Fluoride Ion Source

[0048] The dentifrice composition of the present technology also may include a fluoride ion source to mitigate calcium loss. Suitable fluoride ion sources include without limitation sodium fluoride, potassium fluoride, barium fluoride, potassium monofluorophosphate, sodium monofluorophosphate, ammonium monofluorophosphate, sodium fiuorosiiicate, ammonium fiuorosiiicate, an amine fluoride such as Olaflur (N'--octadecyltrimethylendiamine“N,N,N'4ris(2-ethanol)“ dihydrofluoride), ammonium fluoride, sodium fiuorosiiicate, ammonium fiuorosiiicate, sodium fluoroziconate, sodium monofluorophosphate, aluminum monofluorophosphate, aluminum difluorophosphate, and combinations thereof. In one aspect, one or more fluoride ion sources are included in the dentifrice composition.

[0049] Stannous compounds may be used in combination with the fluoride ion source compounds disclosed above. Suitable stannous compounds include but are not limited to stannous chloride dihydrate, stannous chlorofluoride, stannous pyrophosphate, organic stannous carboxylate salts such as stannous formate, acetate, gluconate, lactate, tartrate, oxaiate, malonate and citrate, stannous ethylene glyoxide, and combinations thereof.

[0050] In one aspect, the dentifrice composition of the present technology includes a fluoride ion source in an amount ranging from about 0.01 to about 10 wt.%, or from about 0.1 to about 7 wt.%, or from about 0.2 to about 5 wt.%, or from about 0.25 to about 1.75 wt.%, or about 0.5 to about 1.5 wt.%, or from about 0.75 to about 1 .25 wt.%, based on the total weight of the composition.

[0051] In one aspect, the amount of fluoride in the dentifrice composition can be expressed in terms of the active fluoride ion present in the composition. The active fluoride ion may be present in an amount ranging from about 500 to about 20,000 ppm, or from about 850 to about 15,000 ppm, or from about 1 ,500 to about 10,000 ppm, or from about 2,500 to about 8,000 ppm, or from about 3,000 to about 5,000 ppm.

Water

[0052] Water is an optional component of the dentifrice compositions of the present technology. Water employed in the preparation of the dentifrice composition should preferably be deionized and free of organic impurities. In one aspect, the dentifrice composition comprises from about 0 to 50 wt.%, or from about 1 to about 45 wt.%, or from about 5 to about 40 wt.%, or from about 10 to about 35 wt.%, or from about 15 to about 25 wt.% water, wherein all percentages are based on the weight of the total composition. These ranges of free water are in addition to the water which is introduced with other materials in the composition.

[0053] In addition to the above described components, the compositions of the present technology can contain a variety of optional conventional ingredients typically used in dentifrice compositions such as toothpastes and tooth gel compositions. Such components include, but are not limited to, flavoring agents, sweetening agents, sensates, pH adjusting agents and buffering agents, coloring agents, anti-calculus agents, anti-bacterial agents, preservatives, whitening agents, desensitizing agents, and mixtures thereof.

[0054] In some aspects, the compositions of the present technology comprise at least one flavoring agent. Suitable flavoring agents include but are limited to essential oils, various flavoring aldehydes, esters, alcohols, and similar materials, as well as menthol, carvone, and anethole, as well as mixtures thereof. Examples of essential oils include oils of spearmint, peppermint, Wintergreen, sassafras, clove, sage, eucalyptus, marjoram, cinnamon, lemon, lime, grapefruit, and orange. In some embodiments, a mixture of peppermint oil and spearmint oil is used as the flavorant in the compositions disclosed herein.

[0055] The amount of flavorant, if employed, ranges from about 0.1 to about 5 wt.%, or from about 0.2 to 4 wt. %, or from about 0.3 to about 3 wt. %, or from about 0.4 to about 2 wt., or from about 0.5 to 2 wt. %, or from about 0.6 to about 2 wt. %, or from about 0.7 to about 2 wt., or from about 0.8 to about 2 wt.%, or from about 0.9 to about 2 wt.%, or from about 1 to about 2 wt.%, based on the total weight of the composition.

[0056] In some aspects, the compositions of the present technology comprise at least one sweetening agent. Any food grade or pharmaceutically acceptable sweetener may be used. Suitable sweetening agents include, for example, sucrose, glucose, saccharin, sucralose, dextrose, levulose, lactose, mannitol, sorbitol, fructose, maltose, xylitol, saccharin salts (e.g., sodium saccharin), thaumatin, aspartame, D-tryptophan, dihydrochalcones, acesulfame, cyclamate salts, and mixtures thereof.

[0057] The amount of sweetening agent, if employed, ranges from about 0.005 to about 10 wt.%, or from about 0.01 to 9 wt.%, or from about 0.1 to 7 wt.%, or from about 0.1 to 5 weight %, or from about 0.3 to about 3 wt.%, or from about 0.5 to 2 wt.%, or from about 0.6 to about 1 wt.%, based on the total weight of the composition.

[0058] Sensates such as cooling, warming, and tingiing agents are useful to deliver signals to the consumer. The most well-known cooling agent is menthol, particularly 1 -menthol, which is found naturally in peppermint oil. Among synthetic cooling agents, many are derivatives of or are structurally related to menthol, i.e., containing the cyclohexane moiety, and derivatized with functional groups including carboxamide, ketal, ester, ether and alcohol. Examples include the p-menthanecarboxamide compounds such as N-ethyl-p-methan-3- carboxamide or N-(4~cyanomethylphenyl)~p-menthanecarboxamide. An example of a synthetic carboxamide cooling agent that is structurally unrelated to menthol is N,2,3-trimethyl-2-isopropylbutanamide. Additional exemplary- synthetic cooling agents include alcohol derivatives such as 3-1 -menthoxy- propane-1 ,2-diol, isopulegol, p-menthane-3,8-diol; menthone glycerol acetal; menthyl esters such as menthyl acetate, menthyl acetoacetate, menthyl lactate, and monomenthyl succinate.

[0059] Additional agents that are structurally unrelated to menthol but have been reported to have a similar physiological cooling effect include alpha-keto enamine derivatives described in United State Patent No. 6,592,884, including 3- methyl-2~(1 -pyrrolidinyl)-2-cyclopenten-1 -one (3-MPC), 5-methyl-2-(1 - pyrrolidinyl)-2-cyclopenten-1 -one (5-MPC); 2,5-dimethyl-4-(1 -pyrrolidinyl)-3(2H)- furanone (DMPF); icilin (also known as AG-3-5, chemical name 142- hydroxyphenyl]-4-[2-nitrophenyl]-1 ,2,3,6-tetrahydropyrimidine-2-one). [0060] Examples of warming agents include ethanol; nicotinate esters, such as benzyl nicotinate; polyhydric alcohols; nonanoyl vanillyl amide; nonanoic acid vanillyl ether; vanillyl alcohol alkyl ether derivatives such as vanillyl ethyl ether, vanillyl butyl ether, vanillyl pentyl ether, and vanillyl hexyl ether; isovanillyl alcohol alkyl ethers; ethylvanillyl alcohol alkyl ethers; veratryl alcohol derivatives; substituted benzyl alcohol derivatives; substituted benzyl alcohol alkyl ethers; vanillin propylene glycol acetal; ethylvanillin propylene glycol acetal; ginger extract; ginger oil; gingerol; zingerone; or combinations thereof.

[0061] Examples of tingling agents include capsaicin; homocapsaicin, jambu oleoresin, zanthoxylum peperitum, saanshool-l, saanshool II, sanshoamide, piperine, piperidine, spilanthol, 4-(1~methoxymethyl)-2~phenyl-1 ,3~dioxolane, or combinations thereof.

[0062] In one aspect, the amount of sensate ranges from about 0.001 to about 5 wt.%, or from about 0.01 to about 4 wt.%, or from about 0.1 to about 3 wt.%, or from about 0.5 to about 2 wt.%, or from about 1 to about 1.5 wt.%, based on the total weight of the composition.

[0063] The dentifrice compositions of the present technology may include an effective amount of a pH adjusting agent and/or a pH buffering agent. pH modifying agents, as used herein, refer to agents that can be used to adjust the pH of the dentifrice compositions to a desired pH range. Such agents include acidifying agents to lower the pH, basifying agents to increase the pH and buffering agents to maintain the pH within a desired range. pH modifying agents may include alkali metal hydroxides, ammonium hydroxide, organic ammonium compounds, carbonates, sesquicarbonates, borates, silicates, phosphates, imidazole, and mixtures thereof. Specific pH agents include monosodium phosphate (monobasic sodium phosphate), trisodium phosphate (sodium phosphate tribasic dodecahydrate or TSP), sodium benzoate, benzoic acid, sodium hydroxide, potassium hydroxide, alkali metal carbonate salts, sodium carbonate, imidazole, pyrophosphate salts, sodium gluconate, lactic acid, sodium lactate, citric acid, sodium citrate, or phosphoric acid. [0064] In one aspect the amount of pH adjusting agent and/or buffer utilizing is an amount necessary to adjust and maintain the pH of the dentifrice compositions in a range from about 3.5 to about 10, or from about 4 to about 9.5, or from about 6 to about 9.

[0065] In some aspects, the dentifrice compositions may include at least one colorant. Colorants include pigments, dyes, lakes and agents imparting a luster or reflectivity such as pearling agents. Any orally acceptable colorant may be used, including without limitation talc, mica, magnesium carbonate, calcium carbonate, magnesium silicate, magnesium aluminum silicate, silica, titanium dioxide, zinc oxide, red, yellow, brown and black iron oxides, ferric ammonium ferrocyanide, manganese violet, ultramarine, titaniated mica, bismuth oxychloride, and the like. Food, Drug and Cosmetic (FD&C) colorants such as primary FD&C Blue No. 1 , FD&C Blue No. 2, FD&C Green No. 3, FD&C Yellow No. 5. FD&C Yellow No. 6, FD&C Red No. 3, FD&C Red No. 33 and FD& C Red No. 40 and lakes FD&C Blue No. 1 , FD&C Blue No. 2, FD&C Yellow No. 5, FD&C Yellow No. 6, FD&C Red No. 2. FD&C Red No. 3, FD& C Red No. 33, FD&C Red No. 40 and combinations thereof.

[0066] The one or more colorants are optionally present in a total amount of from about 0.001 to about 20 wt.%, or from about 0.01 to about 10 wt.%, or from about 0.1 to about 5 wt.%, based on the total weight of the composition.

[0067] The dentifrice compositions may include an anti-calculus agent, in one aspect, the anti-calculus agent is a phosphorous containing compound. Non-limiting examples include a pyrophosphate salt as a source of pyrophosphate ion. In one aspect, the composition comprises tetrasodium pyrophosphate (TSPP) or disodium pyrophosphate or combinations thereof. Other useful anticalculus agents include polycarboxylate polymers and polyvinyl methyl ether/maleic anhydride (PVME/MA) copolymers.

[0068] In one aspect, the amount of anti-calculus agent ranges from about 0.01 to about 5 wt.%, or from about 0.1 to about 2 wt. % of the pyrophosphate salt by weight of the total composition. [0069] In one aspect, the compositions of the present technology can contain an anti-microbiai (e.g., anti-bacterial) agent and/or a preservative. Anti-microbiai agents and preservatives improve the anti-microbiai characteristics of the dentifrice composition and improves storage life stability. Non-limiting exampies of anti-bacteriai and preservative agents are triclosan, chiorhexidine, cetylpyridinium chloride, benzalkonium chloride, stannous sails, essentiai oiis, zinc oxide, zinc citrate, benzyl alcohol, sodium benzoate, isobutyl para- hydroxybenzoate, isopropyi para-hydroxybenzoate, ethyl para-hydroxybenzoate, methyl paraben, ethyl paraben, propyl paraben, and mixtures thereof. Other useful anti-bacterial agents are disclosed in United States Patent No. 5,776,435. [0070] The anti-bacterial and/or preservative agents are optionally present in an antimicrobial effective total amount, typically ranging from about 0.05 to about 10 wt.%, or from about 0.1 to about 3 wt.%, or from about 0.5 to about 1 wt.%, based on the total weight of the composition.

[0071] In one aspect, the dentifrice compositions of the present technology can contain a whitening agent. Non-limiting examples of whitening agents that may be used include, for example, peroxides, metal chlorites, perborates, percarbonates, peroxyacids, hypochlorites, and mixtures thereof. In some embodiments, the whitening agent is hydrogen peroxide or a hydrogen peroxide source, for example, urea peroxide or a peroxide salt or complex (for example, peroxyphosphate, peroxycarbonate, perborate, peroxysilicate, or persulphate salts; for exampie calcium peroxyphosphate, sodium perborate, sodium carbonate peroxide, sodium peroxyphosphate, and potassium persulfate), or a hydrogen peroxide polymer complex (for example, a peroxide-polyvinyl pyrrolidone polymer complex).

[0072] In one aspect, the amount of whitening agent in the dentifrice compositions of the present technology ranges from about 1 to about 5 wt. %, or from about 0.25 to about 3 wt.%, or from about 0.4 to 2 wt.%, or from about 0.6 weight % to about 1 wt.%, based on the total weight of the composition.

[0073] In one aspect, the dentifrice compositions of the present technology optionally comprise a desensitizing, or tooth sensitivity protecting, agent. One or more such agents can be present, Suitable desensitizing agents include, without limitation, potassium sails such as potassium citrate, potassium tartrate, potassium chiaride, potassium sulfate and potassium nitrate. Oher suitabie desensitizing agents inciude sodium nitrate and stannous and strontium sails. Aiternativeiy, a local or systemic analgesic such as aspirin, codeine, acetaminophen, sodium saiicyiate or triethanolamine saiicyiate can be used aione or in combination with the foregoing desensitizing agents.

[0074] in one aspect, the desensitizing agent is utiiized in an amount ranging from about 0.1 to about 10 wt.%, or from about 0. 5 to about 7 wt.%, or from about 1 to about 5 wt.%, based on the total weight of the composition.

[0075] The dentifrice compositions of the present technoiogy are prepared by conventional methods for making dentifrice formulations. in one aspect, the dentifrice is formulated into a toothpaste or tooth gel which can be prepared by the hot process or the ambient process (cold process). The process can a batch process or continuous process. The hot process is described, for example, in United States Patent Nos. 4,353,890 and 6,187,293. A cold process for formulating toothpastes of the present technology are described below.

[0076] In toothpaste or gel form, the composition can be packaged in a conventional plastic laminated metal tube, a pump dispenser, a squeezable plastic container, and other conventional toothpaste and tooth gel dispensers. The toothpaste and gel formulations can be conveniently dispensed in ribbon- like form with good body and texture. The formulation does not overly sag over into the bristles of a toothbrush and is not lumpy or overly tacky.

[0077] It has been discovered that the replacement of all or a portion of traditional dentifrice humectants such as glycerin and sorbitol with the alkoxylated methyl glucoside polyols of the present technology results in stable, glossy, smooth textured easy to dispense toothpastes and gels from product containers.

[0078] The toothpaste and tooth gel compositions of the present technology are used in conventional manner. The compositions are brushed onto dental surfaces and subsequently rinsed away. The compositions generally contact the dental surfaces in a brushing motion for at least about 30, or at least about 60, or at least about 120 seconds.

[0079] The present technology is exemplified by the following examples that are merely for the purpose of illustration and are not to be regarded as limiting the scope of the technology or the way it can be practiced. Unless otherwise specified all weight percentages are expressed as 100 percent active material.

Test Methodology

Accelerated Stability Testing

Toothpaste samples (approximately 100 g) are loaded into gas impermeable collapsible toothpaste tubes (<|) 32, 120 g capacity, Anyang Feilong Pharmaceutical Co., Ltd.) with aluminum foil sealing the dispensing nozzle orifice and a screw cap securely engaged around the nozzle. The filled toothpaste tubes are placed in a stability chamber (Model KBF 240, Binder Inc., Bohemia N.Y.) and stored at 40°C and 75% relative humidity for test duration periods of 0, 1 , 2 and 3 months. Samples are evaluated after each test period for viscosity and appearance using the protocols described below.

Viscosity

[0080] Viscosity measurements are conducted by the Brookfield method employing a Brookfield Helipath™ Stand viscometer (Model RVDV-II +P), Amtek Brookfield, Middleboro, Main). The rotation speed of the test spindle is 5 revolutions per minute (rpm). The viscosity was measured at ambient room temperature (20 to 25°C). T-bar spindle sizes were selected in accordance with the standard operating recommendations from the manufacturer. For the viscosity measurements set forth in the examples a size 94 or 95 T-bar spindle was employed.

Appearance

[0081] Ribbons (3 cm in length) of the toothpastes subjected to the Stability Test protocol are extruded from the toothpaste tubes onto non-absorbent paper. Qualitative observations of the uniformity, texture and phase stability of the toothpaste extrudate are noted. To pass, the extruded ribbons of toothpaste must have a uniformly smooth texture (lump free) and exhibit no liquid phase separation.

Listing of Ingredients

[0082] The ingredients in the following table were utilized to prepare the toothpaste compositions set forth in the examples of the present technology.

Preparation A: (General Preparation Procedure for Calcium Carbonate-Based Toothpastes Prepared with an Alkoxylated Methyl Glucose Polyol)

[0083] Calcium carbonate-based toothpastes were formulated according to the following procedure using the ingredients and amounts set forth in Table 2. A salts solution containing trisodium phosphate, sodium saccharine and sodium monofluorophosphate were dissolved in phase 1 D.l. water under moderate stirring utilizing a RW 20 digital overhead stirrer (IKA Works, Inc, Wilmington, N.C). Benzyl alcohol was then added to the salt solution and mixed until dissolved. The salt solution, Methyl Gluceth-10 and phase 2 D.l. water were added to a Ross™ VMC-1 Multi-Shaft Mixer (Charles Ross & Son Company, Hauppauge, N.Y.) equipped with a jacketed mixing vessel equipped with a temperature control jacket, a sample addition port, a vacuum pump and planetary, disperser and emulsifier mixing blades. The ingredients were mixed at 50 rpm with the planetary blade for 10 minutes at ambient temperature. With the planetary blade still engaged at 50 rpm, the dispenser and emulsifier blade speeds were set to 1000 rpm and 3000 rpm, respectively. Sodium carboxymethylcellulose (Na CMC) was then added to the vessel through the addition port. The planetary blade speed was increased to 100 rpm and the disperser and emulsifier blades speeds were engaged at 4330 rpm and 4500 rpm, respectively. A vacuum (0.1 MPa) was placed over the mixing vessel and the contents were mixed at the set blade speeds for 60 minutes after which the mixing and vacuum cycle was stopped. Thickening silica was then added to the vessel contents and the planetary mixing blade was engaged and gradually increased from 10 to 100 rpm. Upon wetting out of the silica, a vacuum (0.1 MPa) was reapplied over the contents of the mixing vessel and the disperser blade was engaged at 5000 rpm for 5 minutes. The mixing cycle was stopped and CaCO₃ abrasive and flavorant were added to the vessel contents. The planetary blade was engaged, and the speed was gradually increased from 10 to 100 rpm. Upon wetting out of the CaCO₃ abrasive and flavorant powders, a vacuum (0.1 MPa) was placed over the vessel contents and the disperser blade was engaged at 5000 rpm for 20 minutes. In a separate container, sodium lauryl sulfate was dispersed in phase 3 D.l. water warmed to 60°C and added to the contents of the vessel. A vacuum (0.1 MPa) was placed over the vessel contents and the planetary mixing blade was engaged, and the speed was gradually increased from 12 rpm to 100 rpm. The disperser blade was engaged at a speed of 3000 rpm and the contents of the vessel were mixed for 30 to 60 minutes to ensure air bubble removal. Upon removal of air bubbles, the process was completed, and the toothpaste was discharged from the mixer. Viscosity measurements were made on the toothpaste composition approximately 24 hours after discharge from the mixer.

Preparation B: (General Preparation Procedure for Calcium Carbonate-Based Toothpastes Prepared with a Sorbitol Humectant)

[0084] Calcium carbonate-based toothpastes were formulated according to the following procedure using the ingredients and amounts set forth in Table 2. A salt solution containing trisodium phosphate, sodium saccharine and sodium monofluorophosphate were dissolved in phase 1 D.l. water under moderate stirring utilizing a RW 20 digital overhead stirrer (IKA Works, Inc, Wilmington, N.C). Benzyl alcohol was then added to the salt solution and mixed until dissolved. The salt solution, sorbitol and phase 2 D.l. water was added to a Ross™ VMC-1 Multi-Shaft Mixer (described in Preparation A). The ingredients were mixed at 50 rpm with the planetary blade for 5 minutes at ambient temperature. Dispense Na CMC through the side port under agitation in the liquid mixture: Planetary 100 rpm, Disperser at 3000 rpm and Emulsifier at 3000 rpm. After the Na CMC addition, the speed of the Planetary: 100 rpm; Disperser: 4330 rpm and Emulsifier: 4500. A vacuum (0.1 MPa) was placed over the mixing vessel and the contents were mixed at the set blade speeds for 80 minutes after which the mixing and vacuum cycle was stopped. Thickening silica was then added to the vessel contents and the planetary mixing blade was engaged and was gradually increased from 10 to 100 rpm. Upon the wetting out of the silica, a vacuum (0.1 MPa) was reapplied over the contents of the mixing vessel and the disperser blade was engaged at 5000 rpm for 5 minutes. The mixing cycle was stopped and CaCO₃ abrasive and flavorant were added to the vessel contents. The planetary blade was engaged, and the speed was gradually increased from 10 to 100 rpm. Upon the wetting out of the CaCO₃ abrasive and flavorant powders, a vacuum (0.1 MPa) was placed over the vessel contents and the disperser blade was engaged at 5000 rpm for 20 minutes. In a separate container, sodium lauryl sulfate was dispersed in phase 3 D.l. water warmed to 60°C and then added to the contents of the vessel. A vacuum (0.1 MPa) was placed over the vessel contents and the planetary mixing blade was engaged, and the speed was gradually increased from 12 rpm to 100 rpm. The disperser blade was engaged at a speed of 3000 rpm and the contents of the vessel were mixed for 30 to 60 minutes to ensure air bubble removal. Upon removal of air bubbles, the process was completed. The resulting toothpaste was discharged from the mixer and viscosity measurements were made approximately 24 hours after discharge.

Preparation C: (General Preparation Procedure for Abrasive Silica-Based Toothpastes Prepared with an Alkoxylated Methyl Glucose Polyol)

[0085] Abrasive silica-based toothpastes were formulated according to the following procedure using the ingredients and amounts set forth in Table 4. To a container equipped with a RW 20 digital overhead stirrer (IKA Works, Inc, Wilmington, N.C). were added PEG (1500 M.W.) and phase 1 D.l. water and mixed until fully dissolved. Sodium fluoride and sodium saccharine were then added to the PEG solution under moderate stirring until dissolved. The PEG solution, Methyl Gluceth-10 and phase 2 D.l. water were added to a Ross™ VMC-1 Multi-Shaft Mixer (described in Preparation A). The ingredients were mixed at 50 rpm with the planetary blade for 10 minutes at ambient temperature. The planetary blade speed was then increased to 100 rpm and the disperser and emulsifier blades were both engaged at 3000 rpm while Na CMC was added to the vessel through the addition port. Upon the addition of the sodium carboxymethylcellulose, the planetary blade speed was maintained at 100 rpm and the disperser and emulsifier blade speeds were increased to 4330 and 4500 rpm, respectively. A vacuum (0.1 MPa) was placed over the mixing vessel and the contents were mixed at the set blade speeds for 60 minutes after which the mixing and vacuum cycle was stopped. Abrasive and thickening silicas and a flavorant were then added to the vessel contents, and the planetary mixing blade was engaged and gradually increased from 10 to 100 rpm. Upon the wetting out of the silicas and flavorant, a vacuum (0.1 MPa) was reapplied over the contents of the mixing vessel and the disperser blade was engaged at 5000 rpm for 20 minutes. In a separate container, sodium lauryl sulfate was dispersed in phase 3 D.l. water warmed to 60° and added to the contents of the vessel. A vacuum (0.1 MPa) was placed over the vessel contents and the planetary mixing blade was engaged, and the speed was gradually increased from 12 rpm to 100 rpm. The disperser blade was engaged at a speed of 3000 rpm and the contents of the vessel were mixed for 30 to 60 minutes to ensure air bubble removal. Upon removal of air bubbles, the process was completed. The resulting toothpaste was discharged from the mixer and viscosity measurements were made approximately 24 hours after discharge.

Preparation D: (General Preparation Procedure for Abrasive Silica-Based Toothpastes Prepared with a Sorbitol Humectant)

[0086] Abrasive silica-based toothpastes were formulated according to the following procedure using the ingredients and amounts set forth in Table 4. The same procedure disclosed in Preparation C was utilized except sorbitol (70/30 sorbitol/water) was used to replace the alkoxylated methyl glucoside polyol and part of the phase 1 water component. The viscosity of the resulting toothpaste was measured approximately 24 hours after the toothpaste composition was discharged from the mixer.

Examples 1 to 7

[0087] The calcium carbonate-based toothpastes set forth in the table below were formulated with and without an alkoxylated methyl glucose polyol. The toothpaste formulations of Examples 1 to 4 and Comparative Examples 6 and 7 were prepared pursuant to Procedure A above. Comparative Example 5 containing sorbitol instead of the alkoxylated methyl glucoside polyol was prepared as outlined in Procedure B above. In Comparative Examples 6 and 7, the amount of the alkoxylated methyl glucoside polyol contained in the toothpaste formulation was outside of the desired range of 4 to 15.5 wt.% (based on the weight of the total formulation) for the calcium carbonate containing toothpastes of the present technology.

Examples 8 to 14

[0088] The viscosities and pH values of the toothpaste compositions formulated in Examples 1 to 7 were measured after aging at ambient room temperature and humidity (approximately 25°C and 60% relative humidity) for 24 hours. Viscosity measurements were again recorded after aging at ambient room temperature and humidity for 3 to 13 days as indicated in Table 3. In addition, accelerated stability testing of the toothpaste formulations was conducted as set forth in the test protocol described above. The results are presented in Table 3.

[0089] The toothpaste composition prepared with sorbitol (Comparative Example 12) and no alkoxylated methyl glucoside polyol while having a uniform and smooth appearance after 1 , 2 and 3-months exposure in the accelerated stability test, exhibited high a viscosity profile and was very dry. The toothpaste compositions of Comparative Example 13 (containing 16 wt.% of the alkoxylated methyl glucoside polyol underwent syneresis after a 1 -month exposure to the accelerated stability test conditions and further testing was terminated. At 6-months the toothpaste composition of Comparative Example 14 showed the onset of phase separation of water from the toothpaste solids.

Examples 15 and 16

[0090] The silica abrasive-based toothpaste formulations set forth in the table below were prepared with and without an alkoxylated methyl glucose polyol. The toothpaste composition of Example 15 (Procedure C) was formulated with an alkoxylated methyl glucose polyol and Comparative Example 16 (Procedure D) was formulated with sorbitol instead of the alkoxylated methyl glucoside polyol.

Examples 17 and 18

[0091] The viscosities of the toothpaste compositions formulated in Examples 15 and 16 were measured after aging at ambient room temperature and humidity (approximately 25°C and 60% relative humidity) for 24 hours. Viscosity measurements were again recorded after aging at ambient room temperature and humidity for 7 days as indicated in Table 5. In addition, accelerated stability testing of the toothpaste formulations was conducted as set forth in the test protocol described above. The results are presented in Table 5.

[0092] Silica abrasive toothpastes formulated with the alkoxylated methyl glucose polyol of the present technology compared to conventional silica abrasive containing toothpastes formulated with sorbitol are significantly more stable under accelerated age testing conditions.

Claims

What is claimed is:

1 . A dentifrice composition comprising: i) a humectant component comprising an alkoxylated methyl glucoside polyol in an amount ranging from about 4 to about 20 wt. %; or from about 6 to about 18 wt.%, or from about 8 to about 17 wt.%, or from about 10 to about 16 wt.%, or from about 12 to about 14 wt.%; ii) a dental abrasive component in an amount ranging from about 5 to about 50 wt.%, or from about 10 to about 45 wt.%, or from about 15 to about 40 wt.%, or from about 20 to about 35 wt.%; iii) a thickener component in an amount ranging from about 0.1 to about 10 wt. %, or from about 0.5 to about 8 wt.%, or about 0.75 to about 5 wt.%, or from about 1 to about 2.5 wt.%; iv) a detersive surfactant component in an amount ranging from about 0.1 to about 5 wt.%, or from about 0.25 to about 2.5 wt.%, or from about 0.4 to about 2.5 wt., or about 1 to about 2 wt.%; v) a fluoride ion source in an amount ranging from about 0.01 to about 10 wt.%, or from about 0.1 to about 7 wt.%, or from about 0.2 to about 5 wt.%, or from about 0.25 to about 1 .75 wt.%, or about 0.5 to about 1 .5 wt.%, or from about 0.75 to about 1.25 wt.%: vi) water in an amount ranging from about 0 to 50 wt.%, or from about 1 to about 45 wt.%, or from about 5 to about 40 wt.%, or from about 10 to about 35 wt.%, or from about 15 to about 25 wt.%; wherein all percentages are based on the weight of the total composition.

2. A dentifrice composition of claim 2, wherein said alkoxylated methyl glucoside polyol is represented by the formula:

3. A dentifrice composition of any of the previous claims wherein, said alkoxylated methyl glucoside polyol is methyl gluceth-10.

4. A dentifrice composition of any of the previous claims wherein, said dental abrasive component is selected from calcium carbonate, abrasive silica, and mixtures thereof.

5. A dentifrice composition of any of the previous claims wherein, said dental abrasive is selected from calcium carbonate and said alkoxylated methyl glucoside polyol is present in an amount ranging from about 4 to about 15.5 wt.%, or from about 5 to about 15 wt.%, or from about 6 to about 14 wt.%, or from about 7 to about 12 wt.%, or from about 8 to about 10 wt.%.

6. A dentifrice composition of any of the previous claims wherein, said dental abrasive is selected from abrasive silica and said alkoxylated methyl glucoside polyol is present in an amount from about 4 to about 20 wt.%, or from about 5 to about 18 wt.%, or from about 6 to about 16 wt.%, or from about 7 to about 14 wt.%, or from about 8 to about 12 wt.%.

7. A dentifrice composition of any of the previous claims, wherein said thickener component is selected from cellulosic thickeners, gums, seaweed extracts, acrylic thickeners, silica thickeners, and mixtures thereof.

8. A dentifrice composition of any of the previous claims, wherein said thickener is a cellulosic thickener selected from carboxymethyl cellulose, sodium carboxymethyl cellulose, hydroxypropyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, bacterial fermentation derived cellulose, microfibrous cellulose, and mixtures thereof; or wherein said thicker is a gum selected from guar, locust bean, gum Arabic, xanthan, tragacanth, karaya and cassia, and mixtures thereof; or wherein said thickener is a seaweed extract selected from kappa-carrageenan, kappa-2- carrageenan, iota-carrageenan, lambda-carrageenan, alginates, and mixtures thereof; or wherein said thickener is an acrylic thickener selected from linear or crosslinked homopolymers and copolymers comprising acrylic acid, and mixtures thereof; or wherein said thicker is a silica thickener.

8. A dentifrice composition of any of the previous claims, wherein said detersive surfactant component is selected from an anionic surfactant, cationic surfactant, zwitterionic surfactant, amphoteric surfactant, nonionic surfactant, and mixtures thereof.

9. A dentifrice composition of any of the previous claims, wherein said anionic surfactant is selected from a C₈-C₂₂ alkyl sulfate.

10. A dentifrice composition of any of the previous claims, wherein said anionic surfactant is sodium lauryl sulfate.

11. A dentifrice composition of any of the previous claims, wherein said anti- caries component comprises a fluoride moiety.

12. A dentifrice composition of any of the previous claims, wherein said anti- caries component is selected from sodium fluoride, potassium fluoride, zinc fluoride, ammonium fluoride, stannous fluoride, stannous chlorofluoride, barium fluoride, sodium fluorosilicate, ammonium fluorosilicate, sodium fluoroziconate, sodium monofluorophosphate, aluminum monofluorophosphate, aluminum difluorophosphate, and mixtures thereof.

13. A dentifrice composition of any of the previous claims, wherein the dentifrice is a toothpaste or a tooth gel.

14. A method for stabilizing a dentifrice composition containing an abrasive component selected from calcium carbonate, abrasive silica, and mixtures thereof by incorporating into said composition a humectant component comprising an alkoxylated methyl glucoside polyol in an amount ranging from about 4 to about 20 wt. %; or from about 6 to about 18 wt.%, or from about 8 to about 17 wt.%, or from about 10 to about 16 wt.%, or from about 12 to about 14 wt.%.

15. A method of claim 14, wherein said alkoxylated methyl glucoside polyol is represented by the formula:

16. A method of any one of claims 14 or 15 wherein, said alkoxylated methyl glucoside polyol is methyl gluceth-10.

17. A method of any one of claims 14 to 16 wherein, said dental abrasive is selected from calcium carbonate and said alkoxylated methyl glucoside polyol is present in an amount ranging from about 4 to about 15.5 wt.%, or from about 5 to about 15 wt.%, or from about 6 to about 14 wt.%, or from about 7 to about 12 wt.%, or from about 8 to about 10 wt.%.

18. A method of any one of claims 14 to 16 wherein, said dental abrasive is selected from abrasive silica and said alkoxylated methyl glucoside polyol is present in an amount ranging from about 4 to about 20 wt.%, or from about 5 to about 18 wt.%, or from about 6 to about 16 wt.%, or from about 7 to about 14 wt.%, or from about 8 to about 12 wt.%.

19. A method of any one of claims 14 to 18, wherein said dentifrice is a toothpaste or tooth gel.

20. Use of an alkoxylated methyl glucoside polyol for stabilizing a dentifrice composition against phase separation and/or moisture loss.

21 . A use as in claim 20 wherein, said alkoxylated methyl glucoside polyol is represented by the formula:

22. A use as in claims 20 to 21 wherein, said alkoxylated methyl glucoside polyol is methyl gluceth-10.

23. A use as in claims 20 to 22 wherein, said dentifrice composition comprises a dental abrasive component selected from calcium carbonate, abrasive silica, and mixtures thereof.

24. A use as in claims 20 to 23 wherein, said dental abrasive is selected from calcium carbonate and said alkoxylated methyl glucoside polyol is present in an amount ranging from about 4 to about 15.5 wt.%, or from about 5 to about 15 wt.%, or from about 6 to about 14 wt.%, or from about 7 to about 12 wt.%, or from about 8 to about 10 wt.%.

25. A use as in claims 20 to 24, wherein said dental abrasive is selected from abrasive silica and said alkoxylated methyl glucoside polyol is present in an amount from about 4 to about 20 wt.%, or from about 5 to about 18 wt.%, or from about 6 to about 16 wt.%, or from about 7 to about 14 wt.%, or from about 8 to about 12 wt.%.

26. A use as in claims 20 to 25, wherein said dentifrice is a toothpaste or tooth gel.