阅读说明：本技术 固体口腔护理组合物 (Solid oral care compositions ) 是由 R·巴赫帕勒 V·戈德 O·舍尔克 A·瓦拉沃卡尔 于 2020-03-16 设计创作，主要内容包括：本发明涉及一种用于清洁牙齿的固体口腔护理组合物,该组合物被配制成具有最佳脆碎度,其中在制造、运输和储存期间组合物的破损最小,同时易于被消费者咀嚼。公开了一种固体口腔护理组合物,其包含：(i)平均粒度在1至20微米范围内,优选在2至10微米范围内的一级碳酸钙；(ii)平均粒度在200至800微米范围内,优选在350至650微米范围内的二级碳酸钙,和(iii)包含麦芽糖醇的有机多元醇。一级碳酸钙占组合物的5至30重量％,二级碳酸钙占组合物的10至40重量％,且一级碳酸钙与二级碳酸钙的重量比在1∶1至1∶2的范围内。(The present invention relates to a solid oral care composition for cleaning teeth, which is formulated to have optimal friability, wherein breakage of the composition during manufacture, transport and storage is minimized while being easily chewed by a consumer. Disclosed is a solid oral care composition comprising: (i) primary calcium carbonate having an average particle size in the range of 1 to 20 microns, preferably in the range of 2 to 10 microns; (ii) (ii) a secondary calcium carbonate having an average particle size in the range of 200 to 800 microns, preferably in the range of 350 to 650 microns, and (iii) an organic polyol comprising maltitol. The primary calcium carbonate comprises 5 to 30% by weight of the composition, the secondary calcium carbonate comprises 10 to 40% by weight of the composition, and the weight ratio of the primary calcium carbonate to the secondary calcium carbonate is in the range of 1: 1 to 1: 2.)

1. A solid oral care composition comprising:

(i) primary calcium carbonate having an average particle size in the range of 1 to 20 microns, preferably in the range of 2 to 10 microns;

(ii) secondary calcium carbonate having an average particle size in the range of 200 to 800 microns, preferably in the range of 350 to 650 microns; and

(iii) an organic polyol comprising maltitol, wherein the primary calcium carbonate comprises 5 to 30 weight percent of the composition, wherein the secondary calcium carbonate comprises 10 to 40 weight percent of the composition, and the weight ratio of the primary calcium carbonate to the secondary calcium carbonate is in the range of 1: 1 to 1: 2.

2. The composition of claim 1 comprising an additional organic polyol selected from the group consisting of glycerol, sorbitol, xylitol, and mixtures thereof.

3. The composition of claim 2, wherein the additional organic polyol is xylitol.

4. The composition according to claim 3, wherein the weight ratio of xylitol to maltitol is between 1: 0.5 and 1: 2.

5. The composition of any preceding claim, wherein the organic polyol comprises 20 to 60 wt% of the composition.

6. The composition of any of the preceding claims further comprising a foaming agent selected from anhydrous surfactants selected from sodium lauryl sulfate, sodium lauryl sulfoacetate, cocamidopropyl betaine, sodium a-olefin sulfonate, dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate, and mixtures thereof.

7. The composition of claim 6, wherein the foaming agent is sodium lauryl sulfate.

8. The composition of claim 6 or 7, wherein the blowing agent comprises 0.1 to 5 wt% of the composition.

9. The composition of any one of the preceding claims, in the form of a compressed tablet.

10. A non-therapeutic method of cleaning teeth comprising the step of chewing a composition as claimed in any one of the preceding claims.

11. A composition according to any one of the preceding claims 1 to 9 for use in cleaning teeth.

Technical Field

The present invention relates to a solid oral care composition, more particularly to a tablet composition that is chewed and then optionally brushed to provide cleaning of the oral cavity. The composition is formulated so that it has low friability during manufacture, transport and storage of the composition, but can be easily chewed by a person to disintegrate in the mouth to provide the desired cleaning.

Background

Oral care compositions such as toothpastes, tooth powders, oral care tablets, mouthwashes and the like are manufactured to provide one or more benefits to the oral care chamber, the primary benefit being cleaning of the oral cavity, particularly the teeth, gums and oral mucosa. Oral care compositions are sometimes referred to as dentifrices, which generally contain an orally acceptable abrasive. Other ingredients, such as humectants, antibacterial agents, flavoring agents, preservatives, fluoride, and water, are also included to provide other benefits. Most oral care compositions on the market contain large amounts of water, which increases costs due to shipping, adequate packaging and the need for large amounts of preservatives. Efforts have been made in the past to market environmentally acceptable products such as dentifrices and tablets.

EP3131640(Unilever, 2015) relates to a solid oral care composition comprising calcium carbonate and carboxymethyl cellulose.

EP3131639(Unilever, 2015) relates to a solid oral care composition comprising calcium carbonate and polyethylene oxide. The polymer causes the tablet to disintegrate rapidly.

WO2015158639 a1(Unilever) discloses oral care tablets for cleaning teeth as a replacement for toothpaste. The composition comprises calcium carbonate and carrageenan, wherein the weight ratio of carrageenan to calcium carbonate is from 1: 20 to 1: 100. Carrageenan accelerates the disintegration of the tablet.

WO2005110378 a1(Huber) also discloses tablets for cleaning teeth. The tablet contains calcium carbonate, a super disintegrant; and sugar alcohols. When immersed in water, the tablets have a friability of less than about 2% and disintegrate in less than about 60 seconds.

While the tablet compositions disclosed in the above-mentioned patent publications provide the desired cleaning and other benefits expected from such oral care compositions, the present inventors have found that products made using the techniques disclosed in the above-mentioned prior art have a degree of friability above acceptable during manufacture, transport and storage. The present inventors have conducted extensive experiments to arrive at the present invention which involves the use of two different grades of calcium carbonate together with polyols including maltitol, which provides the desired balance between strength required to minimize breakage or friability during manufacture and transport, while being less chewy. The above properties must be met while also ensuring that undesirable organoleptic characteristics such as gritty or chalky mouthfeel are minimized.

It is an object of the present invention to provide a solid oral care composition having improved friability.

Disclosure of Invention

The present invention provides a solid oral care composition comprising:

(i) primary calcium carbonate having an average particle size in the range of 1 micron to 20 microns;

(ii) secondary calcium carbonate having an average particle size in the range of 200 to 800 microns and

(iii) an organic polyol comprising maltitol, wherein the primary calcium carbonate comprises 5-30% by weight of the composition and wherein the secondary calcium carbonate comprises 10-40% by weight of the composition, and the weight ratio of primary calcium carbonate to secondary calcium carbonate is in the range of 1: 1 to 1: 2.

The invention also relates to a method of cleaning teeth comprising the step of chewing the composition of the invention.

Detailed Description

These and other aspects, features and advantages will become apparent to those of ordinary skill in the art upon review of the following detailed description and appended claims. For the avoidance of doubt, any feature of one aspect of the invention may be used in any other aspect of the invention. The word "comprising" is intended to mean "including", but not necessarily "consisting of …" or "consisting of …". In other words, the listed steps or options need not be exhaustive. It should be noted that the examples given in the following description are intended to illustrate the present invention, and are not intended to limit the present invention to these examples per se. Similarly, all percentages are weight/weight percentages unless otherwise indicated. Except in the operating and comparative examples, or where otherwise explicitly indicated, all numbers in this description and in the claims indicating amounts of material or conditions of reaction, physical properties of materials and/or use are to be understood as modified by the word "about". Numerical ranges expressed as "x to y" are understood to include x and y. When multiple preferred ranges are described in the form of "x to y" for a particular feature, it is to be understood that all ranges combining the different endpoints are also contemplated.

The present invention relates to solid oral care compositions, preferably in the form of tablets. More preferably, it is in the form of a compressed tablet.

The compositions of the present invention comprise calcium carbonate as a desirable abrasive for mechanically abrading the surface of teeth and removing residues and plaque deposited thereon. The calcium carbonate used in the present invention has two grades:

according to the invention, micron refers to micrometer. The particle sizes reported herein are measured using a dry dispersion method (Malvern Mastersizer). The primary calcium carbonate has an average particle size in the range of 1 micron to 20 microns, preferably in the range of 2 microns to 10 microns. The most preferred particle size of the first stage has a D of about 5 microns₅₀Wherein D is₁₀Less than 1 micron and D₉₀Is 20 microns.

The secondary calcium carbonate has an average particle size in the range of 200 to 800 microns, preferably in the range of 350 to 650 microns. Most preferred of the two stagesParticle size having a D of about 500 microns₅₀Wherein D is₁₀Is 200 microns and D90 is 800 microns.

The above particle size is the particle size of the primary particles of calcium carbonate. "Primary particle" refers to an individual particle, defined as the smallest discrete particle (e.g., an individual crystal) that can be seen by electron microscopy analysis. The primary particles may combine under certain conditions to form larger secondary structures such as aggregates or agglomerates. For the purposes of the present invention, suitable sources of particulate calcium carbonate include crystalline calcium carbonate.

The term "crystalline" (in the context of particulate calcium carbonate) generally refers to particulate calcium carbonate in which at least 50 wt%, preferably at least 75 wt%, more preferably at least 90 wt%, most preferably more than 95 wt% and ideally more than 99 wt% of the calcium carbonate particles are in crystalline form. The term "crystal" refers to a substantially fully dense solid composed of atoms arranged in an ordered repeating array bounded by planes (the extrinsic manifestation of internal structures). Crystals can be identified and characterized by standard techniques known to those skilled in the art, such as X-ray diffraction.

The crystalline calcium carbonate suitable for use in the present invention may be obtained naturally (by extraction and processing of natural ores) or synthetically (by chemical precipitation). There are three main crystalline polymorphs: calcite, aragonite and less common vaterite. The vaterite form of calcium carbonate is metastable and may irreversibly convert to calcite and aragonite. Each of these crystalline forms has a number of different morphologies (crystal habits). Calcite crystalline polymorph is the most commonly used crystalline form of calcium carbonate. Over 300 crystalline forms of calcite have been reported in the literature.

Particle (e.g. crystal) size can be determined by standard techniques known to those skilled in the art such as sedimentation. For the present invention, particle size was determined using a Malvern Mastersizer. In the context of the present application, the average particle size measurement relates to D₅₀。

Suitable sources of crystalline calcium carbonate of the above defined size and shape include naturally ground calcium carbonate abrasives, typically available from sedimentary rocks such as limestoneOr chalk or metamorphic rocks such as marble, in mining and mechanical milling. Natural calcium carbonate is typically a calcite polymorph having a crystal morphology that can be generally characterized as rhombohedral. Preferred natural ground calcium carbonate abrasives of the type defined above are selected from ground limestone, chalk or marble optionally refined or partially refined to remove impurities. Commercially available examples of primary calcium carbonates include those made by OMYA^TMAG company under the name OMYACARE^TM5AV of those materials sold. These are finely ground high purity white marble abrasives having an average particle size of about 5 microns. Commercially available examples of secondary calcium carbonates include those made by OMYA^TMAG company under the name OMYASCRUB^TMThose sold at 20 KA. These are finely ground high purity white marble abrasives having an average particle size of about 500 microns.

Other types of particulate calcium carbonate may also be suitable, depending on the particular balance of cleaning and abrasion required from a consumer's perspective.

The primary calcium carbonate in the composition of the present invention comprises from 5 to 30% by weight of the composition, more preferably from 10 to 25% by weight. The secondary calcium carbonate comprises from 10 to 40 weight percent of the composition, more preferably from 15 to 30 weight percent. The total amount of all types of calcium carbonate is preferably from 15 to 70 wt%, more preferably from 30 to 70 wt%, most preferably from 30 to 60 wt%, based on the total weight of the composition. The weight ratio of primary calcium carbonate to secondary calcium carbonate is in the range of 1: 1 to 1: 2, more preferably in the range of 1: 1.2 to 1: 1.8.

The composition of the present invention comprises an organic polyol comprising maltitol. The organic polyol according to the present invention refers to a polyol having two or more hydroxyl groups in the molecule. Maltitol is an organic polyol included in the compositions of the invention. The composition preferably comprises at least one or more polyols. The additional polyol may be selected from one or more of sucrose, dextrose, maltose, fructose, glycerol, sorbitol, xylitol, mannitol, lactitol, isomalt, erythritol, polyethylene oxide, polypropylene glycol, propylene glycol and hydrogenated partially hydrolyzed polysaccharides such as hydrogenated starch hydrolysates. Preferred organic polyols for use in this context are non-cariogenic polyols selected from one or more of glycerol, sorbitol or xylitol. Among these, the most preferred additional polyol is xylitol. A highly preferred composition comprises a mixture of maltitol and xylitol. These materials act as binders to aid in the compression of the composition during processing. They also act as humectants. The humectant helps to prevent the composition from hardening or crystallizing upon exposure to air. They also help to give the composition a moist feel in the mouth and in some cases may impart a desirable sweetness. The inventors have learned through their extensive experiments that the optimum friability of the solid oral care composition of the invention results from the selective combination of two grades of inorganic particles of calcium carbonate combined with the polyol maltitol and preferably comprising another polyol which may be xylitol. Thus, when xylitol and maltitol are included in the composition of the invention, the weight ratio of xylitol to maltitol is preferably in the range of 1: 0.5 to 1: 2, more preferably in the range of 1: 0.8 to 1: 1.4.

Maltitol preferably constitutes from 10 to 50% by weight of the composition, more preferably from 15 to 30% by weight. Additional polyols, such as xylitol, if included, preferably constitute from 10 to 30 weight percent of the composition, more preferably from 15 to 25 weight percent.

The total amount of organic polyol preferably comprises from 20 to 60% by weight of the composition, preferably from 25 to 50% by weight.

Details of xylitol and maltitol as preferred organic polyols for use in the present invention are given below.

Xylitol exists as a white granular solid comprising crystalline isotretinoin particles having an average diameter of about 0.4 to 0.6 mm. It is odorless with a sweet taste that imparts a cooling sensation. Xylitol is also commercially available in both powdered form and in several granular directly compressible forms. Xylitol is used as a non-cariogenic sweetener in a variety of pharmaceutical dosage forms, including tablets, syrups, and coatings. It is also widely used as a substitute for sucrose in foods and as a base for pharmaceutical candies. Xylitol finds increasing application in chewing gum, mouth rinses and toothpaste as an agent for reducing plaque and tooth decay (caries). Xylitol is highly effective in enhancing the flavor of tablets and syrups, as well as masking unpleasant or bitter flavors associated with certain pharmaceutically active ingredients and excipients. Xylitol particles are used as diluents in tablet formulations where they can provide the desired sweetness and cooling sensation to the chewable tablet without the "chalky" texture experienced by some other tablet diluents.

Maltitol occurs in the form of a white, tasteless, sweet, anhydrous crystalline powder. It is a disaccharide consisting of one glucose unit linked to one sorbitol unit via an alpha- (1-4) linkage. The crystal structure is orthorhombic. Maltitol is widely used in the pharmaceutical industry for the formulation of oral dosage forms. It is a non-cariogenic bulk (bulk) sweetener with sweetness similar to sucrose, and is well suited for use as a diluent for different oral dosage forms, wet granulation and sugar-free hard coatings.

Suitable blowing agents may preferably be used to form the composition. Preferred blowing agents include surfactants. The surfactant helps to increase the dissolution rate of the solid oral care composition when contacted with saliva and helps to lather the composition during use.

Suitable surfactants include anionic surfactants such as sodium, magnesium, ammonium or ethanolamine salts of: c₈To C₁₈Alkyl sulfates (e.g. sodium lauryl sulfate), C₈To C₁₈Alkyl sulfosuccinates (e.g. dioctyl sodium sulfosuccinate), C₈To C₁₈Alkyl sulfoacetates (such as sodium lauryl sulfoacetate), C₈To C₁₈Alkyl sarcosinates (such as sodium lauryl sarcosinate), C ₈To C₁₈Alkyl phosphates (which may optionally contain up to 10 ethylene oxide and/or propylene oxide units) and sulfated monoglycerides. Other suitable surfactants include nonionic surfactants such as optionally polyethoxylated sorbitan esters of fatty acids, ethoxylated fatty acids, esters of polyethylene oxide, ethoxylates of fatty acid monoglycerides and diglycerides, and ethylene oxide/propylene oxide block polymers. Other suitable surfactant packagesAmphoteric surfactants such as betaines or sulfobetaines are included.

Preferred surfactants for use in the present invention include those anhydrous surfactants selected from the group consisting of sodium lauryl sulfate, sodium lauryl sulfoacetate, cocamidopropyl betaine, sodium a-olefin sulfonate, dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate, and mixtures thereof. Mixtures of any of the above materials may also be used.

The total amount of surfactant incorporated in the compositions of the present invention is generally from about 0.1 to about 5%, more preferably from 0.5 to 3%, based on the total weight of the composition.

The composition of the invention may additionally comprise modified cellulose or modified starch, preferably modified cellulose. The most preferred modified cellulose for use in the compositions of the present invention is carboxymethylcellulose, preferably sodium carboxymethylcellulose (SCMC). When included, SCMC comprises 0.1 to 3 wt%, more preferably 0.5 to 2 wt% of the composition. When included, the SCMC is included in an amount such that the weight ratio of SCMC to calcium carbonate is from 1: 20 to 1: 100, more preferably from 1: 30 to 1: 50.

The composition may also include various additional ingredients to improve aspects such as ease of processing, product performance, and/or consumer acceptability.

The compositions of the present invention are generally non-aqueous. By "non-aqueous" is generally meant that no significant amount of water is intentionally added to the composition. However, the term "non-aqueous" does not imply that small amounts of water may not be present, for example as a consequence of being associated with hygroscopic raw materials. Thus, for the purposes of the present invention, the term "non-aqueous" generally means that water is present in an amount of no greater than about 5 weight percent, more preferably no greater than about 3 weight percent, based on the total weight of the composition.

The solid oral care compositions of the present invention are generally in the form of discrete, single unit doses, such as pills, lozenges or tablets. Such single unit doses are typically 200mg to 5000mg, preferably 250mg to 2000mg, more preferably 500mg to 1500mg in size.

The compositions according to the invention are particularly suitable as carriers for oral care actives which may be physically or chemically incompatible with water or may function less effectively in an aqueous environment.

Specific examples of oral care actives that may be particularly suitable for inclusion in the compositions of the present invention are as follows.

A water-soluble or slightly water-soluble source of zinc ions may be included in the composition to act as an antimicrobial agent. Suitable zinc salts that may be included are zinc chloride, zinc acetate, zinc gluconate, zinc sulfate, zinc fluoride, zinc citrate, zinc lactate, zinc oxide, zinc monoglycerol oleate, zinc tartrate, zinc pyrophosphate and zinc maleate. The most preferred zinc salts are zinc citrate and zinc sulfate. The zinc salt may be included in an amount of 0.1 to 5%, preferably 1 to 4%, by weight of the composition.

Oral care enzyme systems such as hydrogen peroxide-producing enzyme systems (e.g., the oxidoreductase glucose oxidase), amyloglucosidase, dextranase and/or non-water soluble dextranase, optionally in the presence of a zinc ion providing compound and/or 8-hydroxyquinoline derivative, lactoperoxidase, lactoferrin, lysozyme and mixtures thereof may also be included.

A fluoride source is also preferably included in the solid oral care compositions of the present invention. May include fluorides such as sodium fluoride, stannous fluoride, sodium monofluorophosphate, zinc ammonium fluoride, stannammonium fluoride, calcium fluoride, cobalt ammonium fluoride, and mixtures thereof. The most preferred fluoride source is sodium fluoride or sodium monofluorophosphate, with sodium fluoride being most preferred. When included, the fluoride source comprises 0.01 to 2 weight percent, more preferably 0.1 to 1 weight percent of the composition.

The compositions of the present invention may also contain other optional ingredients commonly used in the art, such as anticalculus agents, buffering agents, flavoring agents, sweetening agents, coloring agents, opacifiers, preservatives, anti-sensitivity agents, antibacterial agents, and the like.

The solid oral care compositions of the present invention are used to clean the surfaces of the oral cavity. The composition is an oral care composition that should not be intentionally swallowed for purposes of systemic administration of therapeutic agents, but is applied to the oral cavity for treatment of the oral cavity, followed by rinsing. Typically, the composition is used in conjunction with a cleaning implement, such as a toothbrush, typically by applying it to the bristles of the toothbrush and then brushing the accessible surfaces of the oral cavity.

The tablets of the invention are preferably manufactured using a compaction process which subjects the composition to a pressure in the range of 1 to 8 tonnes. Preferably, the tablets are not coated.

According to another aspect of the present invention, there is provided a non-therapeutic method of cleaning teeth comprising the step of chewing the composition of the present invention. Preferably, the composition is chewed for about 10 seconds to about 5 minutes, more preferably about 3 seconds to about 2 minutes. The teeth are then preferably brushed with a toothbrush. Thereafter the composition is not swallowed but is expectorated from the oral cavity. The oral cavity can thereafter be rinsed with water to remove substantially all of the chewed composition from the mouth.

The compositions claimed herein are also claimed herein for use in cleaning teeth.

The invention is further illustrated with reference to the following non-limiting examples.

Detailed Description

Examples

The following three tablet compositions were prepared as shown in table 1.

TABLE 1

Composition (I)	Example A	Example B	Example 2
				SLS powder	2.00	2.00	2.00
Menthol	0.50	0.50	0.50
				Mint	4.80	4.80	4.80
Calcium carbonate (grade 1)	84.39	40.00	19.39
				Calcium carbonate (2 grade)	0.00	44.39	23.00
Saccharin sodium salt	0.45	0.45	0.45
				Xylitol, its preparation method and use	------	------	20.00
Maltitol	------	------	22.00
				Polyethylene glycol 90M	1.00	1.00	1.00
Zinc sulfate heptahydrate	1.25	1.25	1.25
				Citric acid zinc salt trihydrate	2.00	2.00	2.00
Sodium fluoride	0.31	0.31	0.31
				Magnesium stearate	0.70	0.70	0.70
PVP K 30	2.00	2.00	2.00
				Minor substances	To 100	To 100	To 100

The SLS powder is sodium lauryl sulfate.

Calcium carbonate (grade 1) is calcium carbonate with an average particle size of 5 microns.

Calcium carbonate (grade 1) is calcium carbonate with an average particle size of 500 microns.

The samples were tested for friability using the following equipment and procedure:

the friability of the compressed uncoated tablets was measured. The measurement of tablet friability complements other tests such as breaking force and physical strength of the tablet formulation. Friability testing indicates how much mechanical stress a tablet can withstand during its manufacture, distribution and handling by the customer.

The Friability apparatus used to measure Friability was a Dual cartridge Friability Tester (Model Dual dry Friability Tester) from Electrolab, india. The friability apparatus works on the principle of wear and impact to provide stress to the tablets. The tablets rolled over each other to create friction and the tablets dropped from a height of 6 inches to create an impact on the tablets. The test was run for 100 revolutions, which indicated 100 impacts and wear on the tablets.

The percent weight loss was then calculated using the following formula:

for tablets to be considered commercially useful, it is acceptable that the mass loss of a single assay or the average of three or five assays should be less than 1.0%.

The data for the three samples prepared are summarized in table 2 below:

TABLE 2

The data in table 2 above show that the composition according to the invention (example 1) provides an acceptable friability (less than 1%) whereas the compositions outside the invention (examples a and B) do not.