CA2480595A1 - Zinc citrate beads in oral compositions - Google Patents
Zinc citrate beads in oral compositions Download PDFInfo
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- CA2480595A1 CA2480595A1 CA002480595A CA2480595A CA2480595A1 CA 2480595 A1 CA2480595 A1 CA 2480595A1 CA 002480595 A CA002480595 A CA 002480595A CA 2480595 A CA2480595 A CA 2480595A CA 2480595 A1 CA2480595 A1 CA 2480595A1
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- Prior art keywords
- beads
- composition according
- weight
- zinc salt
- gum
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/025—Explicitly spheroidal or spherical shape
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/27—Zinc; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
Abstract
An oral product, particularly for anti-tartar use, is provided which include s from about 0.001 to about 20%of beads which include zinc salt, the zinc salt having a weight average particle size ranging from 0.01 to 5mm, and a dental base.
Description
ZINC CITRATE BEADS IN ORAL COMPOSITIONS
The invention concerns anti-tartar dental compositions based on zinc citrate which have improved taste.
U.S. Patent 4,022,880 (Vinson et al.), U.S. Patent 4,647,452 (Ritchey et al.) and U.S. Patent 5,372,803 (Williams et al.) all disclose toothpastes comprising zinc citrate.
A major drawback of zinc citrate formulations is that the zinc ion imparts a relatively bitter taste. Smokers are particularly sensitive to the adverse taste.
Accordingly, it is an object of the present invention to provide an oral composition formulated with a zinc anti-tartar salt characterized by an improved taste.
The present invention thus provides an oral product comprising:
(i) from 0.001% to 20% of beads which include a zinc salt having a weight average particle size ranging from about 0.01 to about 5 mm; and (ii) a dental base.
The bitter taste of zinc salts can be improved by incorporating the zinc salt in the form of relatively large active beads. On an equal zinc salt weight basis, the beads are at least as effective in anti-tartar activity as solubilized or dispersed non-complexed zinc salts of the known art.
Zinc salts usable for the present invention may include inorganic or organic counterions. Inorganic zinc salts include counterions such as halides (e. g. chloride, bromide and iodide), sulfates, nitrates, phosphates and combinations thereof. Preferably, the counterion is organic and suitable organic counterions include C2-C2p compounds, especially carboxylates. Preferred organic counterions include citrates, malates, malonates, maleates, adipates, succinates, acetates, propionates, lactates, tartrates, glycolates and combinations thereof. Most especially preferred is zinc citrate trihydrate.
Amount of the beads may range from 0.01 to 20%, preferably from 0.5 to 10%, optimally from 1 to 5% by weight of the total oral product.
Optionally, a gum may be incorporated into the beads of the present invention. Illustrative gums are polysaccharides including sodium carboxymethyl cellulose (CMC), hydroxyethylcellulose, methylcellulose, ethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, gum tragacanth, gum arabic, gum karaya, pectin, carageenan, guar, xanthan gum, starch and combinations thereof. Most preferred are the cellulose type gums, especially sodium carboxymethyl cellulose (CMC). All molecular weight types of sodium CMC
may be useful, although the medium viscosity grade such as the 9M grade is most suitable.
Beads of the present invention normally will contain essentially only zinc citrate. In a less preferred but useful embodiment, the beads may be formed by the complexion of the zinc salt with a gum in the presence of water to form gel particles. Relative weight ratios of the zinc salt to gum in this preferred embodiment ranges from 10,000:1 to 10:1, preferably from 1,000:1 to 100:1 by weight.
In some embodiments of the present invention, water may be present within the beads. In those situations, the relative weight ratios of the zinc salt to water in the beads may range from 50:1 to 1:50, preferably from 20:1 to 1:1, optimally from 10:1 to 6:1 by weight.
Typically the amount of zinc salt in the beads is 1000.
However, in some embodiments the amount of zinc salt in the beads may range from 15 to 990, sometimes from 50 to 950, but optimally from 90 to 1000 by weight of the beads. V~Then a gum is present, amounts of the gum within the bead may range from 0.001 to 20, preferably from 0.1 to 1%, optimally from 0.25 to 0.5% by weight of the beads. The remainder of the bead composition generally is water present in amounts from 1 to 60%, preferably from 2 to 40%, optimally from 5 to 20% by weight of the beads.
Weight average particle size of the beads and also of the zinc salt may range from 0.01 to 5 mm, preferably from 0.05 to 3 mm, optimally from 0.1 to 2 mm. Bulk density of the beads may range from 0.75 to 0.95, preferably from 0.80 to 0.90, optimally from 0.81 to 0.84 gm/CC.
Beads according to the present invention are prepared prior to introduction. into a dental base with other ingredients of the oral product. Zinc salt and any optional ingredients such as gum and water can be formed by mixing in a Hobart-type blending apparatus.
In one embodiment, the beads are visually distinct in the dental base. This may be accomplished by the beads being opaque and the base being substantially transparent.
Alternatively, the beads may appear as clear bodies colored differently from a transparent or opaque base.
Besides the beads, the oral product will contain a dental base in an amount of SO to 99% by weight. Ingredients of the dental base may include humectants, thickeners, abrasives, anti-caries agents, surfactants, colorants, flavorants, opacifiers, water and a variety of special actives (e. g.
desensitization agents such as potassium nitrate, peroxides and anti-bacterials such as triclosan).
Surfactants useful herein may be of the anionic, nonionic, cationic, zwitterioniC or amphoteriC type. Most preferred are sodium lauryl sulphate, sodium dodecylbenzene sulfonate and sodium lauryl sarcosinate. Amounts of the surfactant may range from 0.5 to 10%, preferably from 1 to 5o by weight of the dental base.
Humectants useful herein are usually polyols. Illustrative of this category are sorbitol, maltitol, mannitol, glycerin, propylene glycol, xylitol, hydrogenated corn syrup, polyethylene glycols and mixtures thereof. Amounts of the humectant may range from 1 to 600, preferably from 5 to 50%, optimally from 10 to 40o by weight of the dental base.
The invention concerns anti-tartar dental compositions based on zinc citrate which have improved taste.
U.S. Patent 4,022,880 (Vinson et al.), U.S. Patent 4,647,452 (Ritchey et al.) and U.S. Patent 5,372,803 (Williams et al.) all disclose toothpastes comprising zinc citrate.
A major drawback of zinc citrate formulations is that the zinc ion imparts a relatively bitter taste. Smokers are particularly sensitive to the adverse taste.
Accordingly, it is an object of the present invention to provide an oral composition formulated with a zinc anti-tartar salt characterized by an improved taste.
The present invention thus provides an oral product comprising:
(i) from 0.001% to 20% of beads which include a zinc salt having a weight average particle size ranging from about 0.01 to about 5 mm; and (ii) a dental base.
The bitter taste of zinc salts can be improved by incorporating the zinc salt in the form of relatively large active beads. On an equal zinc salt weight basis, the beads are at least as effective in anti-tartar activity as solubilized or dispersed non-complexed zinc salts of the known art.
Zinc salts usable for the present invention may include inorganic or organic counterions. Inorganic zinc salts include counterions such as halides (e. g. chloride, bromide and iodide), sulfates, nitrates, phosphates and combinations thereof. Preferably, the counterion is organic and suitable organic counterions include C2-C2p compounds, especially carboxylates. Preferred organic counterions include citrates, malates, malonates, maleates, adipates, succinates, acetates, propionates, lactates, tartrates, glycolates and combinations thereof. Most especially preferred is zinc citrate trihydrate.
Amount of the beads may range from 0.01 to 20%, preferably from 0.5 to 10%, optimally from 1 to 5% by weight of the total oral product.
Optionally, a gum may be incorporated into the beads of the present invention. Illustrative gums are polysaccharides including sodium carboxymethyl cellulose (CMC), hydroxyethylcellulose, methylcellulose, ethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, gum tragacanth, gum arabic, gum karaya, pectin, carageenan, guar, xanthan gum, starch and combinations thereof. Most preferred are the cellulose type gums, especially sodium carboxymethyl cellulose (CMC). All molecular weight types of sodium CMC
may be useful, although the medium viscosity grade such as the 9M grade is most suitable.
Beads of the present invention normally will contain essentially only zinc citrate. In a less preferred but useful embodiment, the beads may be formed by the complexion of the zinc salt with a gum in the presence of water to form gel particles. Relative weight ratios of the zinc salt to gum in this preferred embodiment ranges from 10,000:1 to 10:1, preferably from 1,000:1 to 100:1 by weight.
In some embodiments of the present invention, water may be present within the beads. In those situations, the relative weight ratios of the zinc salt to water in the beads may range from 50:1 to 1:50, preferably from 20:1 to 1:1, optimally from 10:1 to 6:1 by weight.
Typically the amount of zinc salt in the beads is 1000.
However, in some embodiments the amount of zinc salt in the beads may range from 15 to 990, sometimes from 50 to 950, but optimally from 90 to 1000 by weight of the beads. V~Then a gum is present, amounts of the gum within the bead may range from 0.001 to 20, preferably from 0.1 to 1%, optimally from 0.25 to 0.5% by weight of the beads. The remainder of the bead composition generally is water present in amounts from 1 to 60%, preferably from 2 to 40%, optimally from 5 to 20% by weight of the beads.
Weight average particle size of the beads and also of the zinc salt may range from 0.01 to 5 mm, preferably from 0.05 to 3 mm, optimally from 0.1 to 2 mm. Bulk density of the beads may range from 0.75 to 0.95, preferably from 0.80 to 0.90, optimally from 0.81 to 0.84 gm/CC.
Beads according to the present invention are prepared prior to introduction. into a dental base with other ingredients of the oral product. Zinc salt and any optional ingredients such as gum and water can be formed by mixing in a Hobart-type blending apparatus.
In one embodiment, the beads are visually distinct in the dental base. This may be accomplished by the beads being opaque and the base being substantially transparent.
Alternatively, the beads may appear as clear bodies colored differently from a transparent or opaque base.
Besides the beads, the oral product will contain a dental base in an amount of SO to 99% by weight. Ingredients of the dental base may include humectants, thickeners, abrasives, anti-caries agents, surfactants, colorants, flavorants, opacifiers, water and a variety of special actives (e. g.
desensitization agents such as potassium nitrate, peroxides and anti-bacterials such as triclosan).
Surfactants useful herein may be of the anionic, nonionic, cationic, zwitterioniC or amphoteriC type. Most preferred are sodium lauryl sulphate, sodium dodecylbenzene sulfonate and sodium lauryl sarcosinate. Amounts of the surfactant may range from 0.5 to 10%, preferably from 1 to 5o by weight of the dental base.
Humectants useful herein are usually polyols. Illustrative of this category are sorbitol, maltitol, mannitol, glycerin, propylene glycol, xylitol, hydrogenated corn syrup, polyethylene glycols and mixtures thereof. Amounts of the humectant may range from 1 to 600, preferably from 5 to 50%, optimally from 10 to 40o by weight of the dental base.
Thickeners useful herein may be the same gums as utilized to complex with the zinc salts. However, these gums will be formulated into the dental base rather than into the pre-formed beads. Illustrative thickeners include sodium carboxymethyl cellulose, ethylcellulose, carageenan, xanthan gum, pectin, chemically modified starches and acrylates. The latter may be crosslinked polyacrylates such as Carbopol~
934. Inorganic thickeners are exemplified by silica aerogels and magnesium aluminum silicate, commercially available as Veegum~. Amounts of the thickener may range from 0.01 to 300, preferably from 0.1 to 200, optimally from 0.5 to 5% by weight of the dental base.
A fluoride anti-caries compound normally is usually present as part of the dental base. Illustrative of such fluoride compounds are sodium fluoride, potassium fluoride, calcium fluoride, stannous fluoride, stannous monofluorophosphate, sodium monofluorophosphate and copper fluoride. Most preferred is sodium fluoride. These sources should release anywhere from 25 to 5,000 ppm of fluoride ion. The anti-caries compound will normally be present in an amount from 0.01 to 5%, preferably from 0.1 to 2.5%, optimally from 0.2 to 1.5% by weight of the dental base.
Abrasives may also be present in the dental base.
Illustrative materials include sodium metaphosphate, dicalcium phosphate, calcium pyrophosphate, silica, alumina, chalk, insoluble bicarbonate salts and mixtures thereof.
Amounts of the abrasive may range from 1 to 800, preferably from 5 to 50o by weight of the dental base.
934. Inorganic thickeners are exemplified by silica aerogels and magnesium aluminum silicate, commercially available as Veegum~. Amounts of the thickener may range from 0.01 to 300, preferably from 0.1 to 200, optimally from 0.5 to 5% by weight of the dental base.
A fluoride anti-caries compound normally is usually present as part of the dental base. Illustrative of such fluoride compounds are sodium fluoride, potassium fluoride, calcium fluoride, stannous fluoride, stannous monofluorophosphate, sodium monofluorophosphate and copper fluoride. Most preferred is sodium fluoride. These sources should release anywhere from 25 to 5,000 ppm of fluoride ion. The anti-caries compound will normally be present in an amount from 0.01 to 5%, preferably from 0.1 to 2.5%, optimally from 0.2 to 1.5% by weight of the dental base.
Abrasives may also be present in the dental base.
Illustrative materials include sodium metaphosphate, dicalcium phosphate, calcium pyrophosphate, silica, alumina, chalk, insoluble bicarbonate salts and mixtures thereof.
Amounts of the abrasive may range from 1 to 800, preferably from 5 to 50o by weight of the dental base.
When the oral compositions are gels, structurants may be necessary. Particularly useful as a structurant are polyoxyethylene-polyoxypropylene copolymers such as those sold under the trademark Pluronic~. These materials are also known as Poloxamers and employed in amounts from 5 to 30%, preferably from 18 to 25% by weight of the dental base.
Flavors may also be part of the dental base. These flavors may be based on oils of spearmint and peppermint. Examples of other flavoring materials include menthol, clove, wintergreen, eucalyptus and aniseed. Flavors may range in amount from 0.1 to 5% by weight of the dental base.
Sweetening agents may also be included in the dental base.
Illustrative agents include saccharin, sodium cyclamate, aspartame, acesulfame, xylitol and combinations thereof at levels from 0.1 to 10% by weight of the dental base.
Other additives may also be incorporated into the dental base. These may be anti-tartar agents, colorants, preservatives, silicones, other synthetic or natural polymers such as Gantre~ S97~, and mixtures thereof: Amounts of these other ingredients may range from 0.01 to 20o by weight of the dental base.
Water may be present in the dental base in amounts from 1 to 95%, preferably from 10 to 600, optimally from 20 to 50o by weight of the dental base.
The term "comprising" is meant not to be limiting to any subsequently stated elements but rather to encompass non-specified elements of major or minor functional importance.
In other words the listed steps, elements or options need not be exhaustive. V~lhenever the words "including" or "having" are used, these terms are meant to be equivalent to "comprising" as defined above.
The following examples will more fully illustrate the embodiments of this invention. All parts, percentages and proportions referred to herein and in the appended claims are by weight unless otherwise illustrated.
Zinc salt beads of the present invention were prepared in several different ways. One procedure utilized a Hobart bowl. Zinc citrate was added to the bowl and a 2% CMC
solution was slowly added with mixing until the beads formed. They were then air dried and sieved. A second method for preparation was via a ribbon blender, again adding a 2o solution of CMC to the dry zinc citrate.
Fluidized bed technology can also be utilized for manufacture of the beads. By this procedure zinc citrate was suspended in the fluid bed reactor while a nozzle sprayed a 2o solution of CMC. The spray drier utilized for this purpose was a GPCG-5, ex Glatt Technologies with a Schlick 924 nozzle. This model was able to produce 5-7 kilogram batches. The 2o CMC solution was sprayed using a peristaltic pump along with pressurized air at the nozzle to _ g _ atomize the spray. Achievement of optimum results required swift introduction of the CMC, use of cool air to fluidize, and maintenance of the product temperature during drying so that it stayed below 40°C. The relatively cool air prevented solids from sticking together before the beads were formed. During drying, the temperature quickly rose after water was removed. Care was taken not to over-dry which could lead to a frail bead. When the temperature reached 35°C, the batch was considered dried.
A typical gel dentifrice composition incorporating the beads of this invention is described below.
TABLE I
Component Weight Sorbitol 56.33 Syloid 63X~ 10.0 Syloid 244 ~ 9.0 Polyethylene glycol (1500 M.W.) 5.00 Ethyl alcohol 2.1 Sodium lauryl sulfate 1.6 Menthol 1.0 Sodium monofluorophosphate 0.8 Cellulose gum 0.4 Sodium saccharin 0.3 Beads (Zinc Citrate/CMC in 200/1 ratio) 0.5 Water Balance An opaque toothpaste with the beads of this invention has a formula as described below.
~'PT'QT.'G~ T T
Component Weight Sorbitol 15.0 Glycerin 3.0 Calcium phosphate dehydrate, dibasic 33.5 Anhydrous calcium phosphate, dibasic 5.0 Titanium dioxide 1.5 Sodium lauryl phosphate 1.5 Carboxymethyl cellulose 1.2 Sodium monofluorophosphate 0.8 Peppermint oil 0.6 Sodium saccharin 0.4 Beads (Zinc Citrate/CMC in 300/1 ratio) 1.0 Water Balance A comparative taste test is reported under this Example.
Two formulas were evaluated. The first was according to Example 2 wherein zinc citrate was present in the form of complexed insoluble beads. A comparative experiment utilized the same formula as in Example 2 except that an equivalent amount of zinc citrate was solubilized within the formula rather than present as insoluble beads.
A flavor tasting panel was assembled consisting of thirteen persons. They rated the zinc citrate bead and the non-bead solubilized toothpaste after brushing, according to a series of organoleptiC attributes. Ratings were on a scale of 1 to 5, where 1 = poor and 5 = excellent. After brushing with both products, the panelists chose their preference. Table III below lists results of the flavor test. Values provided in the second and third column are average ratings except for the "preference" entry where 9 people chose the bead product, 3 people chose the control (zinc citrate solubilized) and 1 person had no preference.
mTnT n r-r-r Flavor Test SENSORY PERCEPTION ZINC CITRATE BEADS ZINC CITRATE
SOLUBILIZED
Flavor 4.00 3.31 Strength 3.92 3.77 Foam 3.38 3.54 After Taste 3.46 2.92 Feel Clean 4.00 3.69 Impact 3.92 3.38 Overall Liking 3.85 3.31 Preference 9.00 3.00 The tests indicate that the zinc citrate in bead form was favored in six of the seven taste categories. Only foam was found to be better in the comparative formula. The overall preference, by a wide margin, was for zinc citrate in the bead form rather~than solubilized.
Zinc citrate beads were prepared in a Chilsonator~. This equipment compacts the zinc citrate powder by forcing the powder between two counter rotating rolls. As the volume decreases through a region of maximum pressure, the material is formed into a solid compact or sheet. As the rolls turn toward each other, the material in a slip region moves downward at a rate less than the surface speed of the rolls.
In a nip region, the materials are caught or trapped by the rolls and move at a same speed as the roll surface, this forces the material through the region of maximum pressure, which is on a line between the centers of the two rolls.
After compaction, the resultant material is fed into a FitzMill~ granulator to gently cut the compacted material into beads which are separated by screens into appropriate sizes.
For the present Example, the Chilsonator~ was operated at a roll speed of 5.0 rpm, a Vertical Screw Feed of 80 rpm, a Horizontal Screw Feed of 15 rpm, and a pressure of 700 psi.
The angle of repose of zinc citrate was 45°. The loose density of the zinc citrate bead was 0.61 g/cc. The compact thickness of the resultant ribbon from the Chilsonator~
before milling was 0.15 inches. After granulation, the resultant particles were sieved to obtain samples of different average particle size. These sizes were evaluated in a dental base outlined under Table I above.
Twelve people participated in a bead evaluation panel. All brushed their teeth with four products containing different particle size beads, all of which dentifrices were fielded blind. The study was cross-over in nature, the products being randomized and panelists brushing with two products during the course of one day and then two more products the following day. After each brushing, a brief questionnaire was filled out. The tables below display the results. The term "sensory" refers to a combination score of flavor while brushing, aftertaste and mouthfeel while brushing.
TABLE IV
Particle Size of Zinc Citrate Beads vs. Sensory Average Particle (mm) Sensory Score 1.35 17 0.65 66 0.225 5g < 0.15 25 TABLE V
Panelist Rating of Excellent For Overall Liking Average Particle Size (mm) % Rates Excellent 1.35 0 0.65 25 0.225 25 < 0.15 TABLE VI
Panelists Rating For Texture Average Particle Size (mm) % Texture Rating 1.35 32 0.65 91 0.225 91 < 0.15 83 Overall sensory properties peaked in the average particle size area between 0.65 and 0.225 mm. This was also the area within which maximum ratings for overall liking and texture were given.
Flavors may also be part of the dental base. These flavors may be based on oils of spearmint and peppermint. Examples of other flavoring materials include menthol, clove, wintergreen, eucalyptus and aniseed. Flavors may range in amount from 0.1 to 5% by weight of the dental base.
Sweetening agents may also be included in the dental base.
Illustrative agents include saccharin, sodium cyclamate, aspartame, acesulfame, xylitol and combinations thereof at levels from 0.1 to 10% by weight of the dental base.
Other additives may also be incorporated into the dental base. These may be anti-tartar agents, colorants, preservatives, silicones, other synthetic or natural polymers such as Gantre~ S97~, and mixtures thereof: Amounts of these other ingredients may range from 0.01 to 20o by weight of the dental base.
Water may be present in the dental base in amounts from 1 to 95%, preferably from 10 to 600, optimally from 20 to 50o by weight of the dental base.
The term "comprising" is meant not to be limiting to any subsequently stated elements but rather to encompass non-specified elements of major or minor functional importance.
In other words the listed steps, elements or options need not be exhaustive. V~lhenever the words "including" or "having" are used, these terms are meant to be equivalent to "comprising" as defined above.
The following examples will more fully illustrate the embodiments of this invention. All parts, percentages and proportions referred to herein and in the appended claims are by weight unless otherwise illustrated.
Zinc salt beads of the present invention were prepared in several different ways. One procedure utilized a Hobart bowl. Zinc citrate was added to the bowl and a 2% CMC
solution was slowly added with mixing until the beads formed. They were then air dried and sieved. A second method for preparation was via a ribbon blender, again adding a 2o solution of CMC to the dry zinc citrate.
Fluidized bed technology can also be utilized for manufacture of the beads. By this procedure zinc citrate was suspended in the fluid bed reactor while a nozzle sprayed a 2o solution of CMC. The spray drier utilized for this purpose was a GPCG-5, ex Glatt Technologies with a Schlick 924 nozzle. This model was able to produce 5-7 kilogram batches. The 2o CMC solution was sprayed using a peristaltic pump along with pressurized air at the nozzle to _ g _ atomize the spray. Achievement of optimum results required swift introduction of the CMC, use of cool air to fluidize, and maintenance of the product temperature during drying so that it stayed below 40°C. The relatively cool air prevented solids from sticking together before the beads were formed. During drying, the temperature quickly rose after water was removed. Care was taken not to over-dry which could lead to a frail bead. When the temperature reached 35°C, the batch was considered dried.
A typical gel dentifrice composition incorporating the beads of this invention is described below.
TABLE I
Component Weight Sorbitol 56.33 Syloid 63X~ 10.0 Syloid 244 ~ 9.0 Polyethylene glycol (1500 M.W.) 5.00 Ethyl alcohol 2.1 Sodium lauryl sulfate 1.6 Menthol 1.0 Sodium monofluorophosphate 0.8 Cellulose gum 0.4 Sodium saccharin 0.3 Beads (Zinc Citrate/CMC in 200/1 ratio) 0.5 Water Balance An opaque toothpaste with the beads of this invention has a formula as described below.
~'PT'QT.'G~ T T
Component Weight Sorbitol 15.0 Glycerin 3.0 Calcium phosphate dehydrate, dibasic 33.5 Anhydrous calcium phosphate, dibasic 5.0 Titanium dioxide 1.5 Sodium lauryl phosphate 1.5 Carboxymethyl cellulose 1.2 Sodium monofluorophosphate 0.8 Peppermint oil 0.6 Sodium saccharin 0.4 Beads (Zinc Citrate/CMC in 300/1 ratio) 1.0 Water Balance A comparative taste test is reported under this Example.
Two formulas were evaluated. The first was according to Example 2 wherein zinc citrate was present in the form of complexed insoluble beads. A comparative experiment utilized the same formula as in Example 2 except that an equivalent amount of zinc citrate was solubilized within the formula rather than present as insoluble beads.
A flavor tasting panel was assembled consisting of thirteen persons. They rated the zinc citrate bead and the non-bead solubilized toothpaste after brushing, according to a series of organoleptiC attributes. Ratings were on a scale of 1 to 5, where 1 = poor and 5 = excellent. After brushing with both products, the panelists chose their preference. Table III below lists results of the flavor test. Values provided in the second and third column are average ratings except for the "preference" entry where 9 people chose the bead product, 3 people chose the control (zinc citrate solubilized) and 1 person had no preference.
mTnT n r-r-r Flavor Test SENSORY PERCEPTION ZINC CITRATE BEADS ZINC CITRATE
SOLUBILIZED
Flavor 4.00 3.31 Strength 3.92 3.77 Foam 3.38 3.54 After Taste 3.46 2.92 Feel Clean 4.00 3.69 Impact 3.92 3.38 Overall Liking 3.85 3.31 Preference 9.00 3.00 The tests indicate that the zinc citrate in bead form was favored in six of the seven taste categories. Only foam was found to be better in the comparative formula. The overall preference, by a wide margin, was for zinc citrate in the bead form rather~than solubilized.
Zinc citrate beads were prepared in a Chilsonator~. This equipment compacts the zinc citrate powder by forcing the powder between two counter rotating rolls. As the volume decreases through a region of maximum pressure, the material is formed into a solid compact or sheet. As the rolls turn toward each other, the material in a slip region moves downward at a rate less than the surface speed of the rolls.
In a nip region, the materials are caught or trapped by the rolls and move at a same speed as the roll surface, this forces the material through the region of maximum pressure, which is on a line between the centers of the two rolls.
After compaction, the resultant material is fed into a FitzMill~ granulator to gently cut the compacted material into beads which are separated by screens into appropriate sizes.
For the present Example, the Chilsonator~ was operated at a roll speed of 5.0 rpm, a Vertical Screw Feed of 80 rpm, a Horizontal Screw Feed of 15 rpm, and a pressure of 700 psi.
The angle of repose of zinc citrate was 45°. The loose density of the zinc citrate bead was 0.61 g/cc. The compact thickness of the resultant ribbon from the Chilsonator~
before milling was 0.15 inches. After granulation, the resultant particles were sieved to obtain samples of different average particle size. These sizes were evaluated in a dental base outlined under Table I above.
Twelve people participated in a bead evaluation panel. All brushed their teeth with four products containing different particle size beads, all of which dentifrices were fielded blind. The study was cross-over in nature, the products being randomized and panelists brushing with two products during the course of one day and then two more products the following day. After each brushing, a brief questionnaire was filled out. The tables below display the results. The term "sensory" refers to a combination score of flavor while brushing, aftertaste and mouthfeel while brushing.
TABLE IV
Particle Size of Zinc Citrate Beads vs. Sensory Average Particle (mm) Sensory Score 1.35 17 0.65 66 0.225 5g < 0.15 25 TABLE V
Panelist Rating of Excellent For Overall Liking Average Particle Size (mm) % Rates Excellent 1.35 0 0.65 25 0.225 25 < 0.15 TABLE VI
Panelists Rating For Texture Average Particle Size (mm) % Texture Rating 1.35 32 0.65 91 0.225 91 < 0.15 83 Overall sensory properties peaked in the average particle size area between 0.65 and 0.225 mm. This was also the area within which maximum ratings for overall liking and texture were given.
Claims (10)
1. An oral product comprising:
(i) from 0.001% to 20% of beads which comprise from 50 to 100% by weight of a zinc salt with an organic counterion, the beads having a weight average particle size ranging from 0.1 to 5 mm; and (ii) a dental base.
(i) from 0.001% to 20% of beads which comprise from 50 to 100% by weight of a zinc salt with an organic counterion, the beads having a weight average particle size ranging from 0.1 to 5 mm; and (ii) a dental base.
2, The composition according to claim 1, wherein the zinc salt is zinc citrate trihydrate.
3. The composition according to claim 1 or claim 2 wherein the zinc salt has a weight average particle size of from 0.1 to 2 mm.
4. The composition according to any preceding claim, wherein the beads further comprise a gum.
5. The composition according to claim 4, wherein the gum is a cellulose.
6. The composition according to claim 5, wherein the gum is sodium carboxymethyl cellulose.
7. The composition according to claim 4, wherein the weight ratio of zinc salt to gum ranges from 1000:1 to 100:1.
8. The composition according to any preceding claim, wherein the dental base comprises a material selected from the group consisting of humectants, thickeners.
surfactants, colorants, flavorants, anti-caries agent, abrasives, opacifiers, water and combinations thereof.
surfactants, colorants, flavorants, anti-caries agent, abrasives, opacifiers, water and combinations thereof.
9. The composition according to any preceding claim, wherein the beads are opaque and the dental base is substantially transparent.
10. The composition according to any preceding claim, wherein the zinc salt ranges from 90 to 100% by weight of the beads.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/132,046 | 2002-04-25 | ||
| US10/132,046 US6592852B1 (en) | 2002-04-25 | 2002-04-25 | Zinc citrate beads in oral compositions |
| PCT/EP2003/004240 WO2003090702A1 (en) | 2002-04-25 | 2003-04-23 | Zinc citrate beads in oral compositions |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2480595A1 true CA2480595A1 (en) | 2003-11-06 |
Family
ID=22452196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002480595A Abandoned CA2480595A1 (en) | 2002-04-25 | 2003-04-23 | Zinc citrate beads in oral compositions |
Country Status (8)
| Country | Link |
|---|---|
| US (2) | US6592852B1 (en) |
| EP (1) | EP1496850A1 (en) |
| CN (1) | CN1319509C (en) |
| AU (1) | AU2003222306A1 (en) |
| BR (1) | BR0308955A (en) |
| CA (1) | CA2480595A1 (en) |
| WO (1) | WO2003090702A1 (en) |
| ZA (1) | ZA200407495B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MXPA05005335A (en) * | 2002-11-22 | 2005-07-25 | Firmenich & Cie | Oral compositions which mask the salty taste of salts. |
| US20040101490A1 (en) * | 2002-11-22 | 2004-05-27 | Noville Inc. | Oral compositions which mask the salty taste of sodium bicarbonate |
| US20050170013A1 (en) * | 2004-02-04 | 2005-08-04 | Douglas Jerry A. | Composition for treating a dermatological inflammatory response and method of preparation thereof |
| SG169990A1 (en) * | 2005-12-21 | 2011-04-29 | Colgate Palmolive Co | Improved oral compositions comprising zinc citrate and/or tocopherol agents |
| US7687650B2 (en) | 2006-02-03 | 2010-03-30 | Jr Chem, Llc | Chemical compositions and methods of making them |
| US7897800B2 (en) * | 2006-02-03 | 2011-03-01 | Jr Chem, Llc | Chemical compositions and methods of making them |
| AU2006337161B2 (en) | 2006-02-03 | 2012-06-07 | Obagi Cosmeceuticals Llc | Anti-aging treatment using copper and zinc compositions |
| US20070209263A1 (en) * | 2006-03-10 | 2007-09-13 | Hohlbein Douglas J | Method of relating different products by a common feature |
| PL1837009T3 (en) * | 2006-03-22 | 2009-10-30 | Procter & Gamble | Oral zinc compositions |
| JP4214159B2 (en) * | 2006-06-29 | 2009-01-28 | 住友ゴム工業株式会社 | Pneumatic tire |
| US7867522B2 (en) | 2006-09-28 | 2011-01-11 | Jr Chem, Llc | Method of wound/burn healing using copper-zinc compositions |
| US8273791B2 (en) | 2008-01-04 | 2012-09-25 | Jr Chem, Llc | Compositions, kits and regimens for the treatment of skin, especially décolletage |
| US20160184354A1 (en) | 2009-01-23 | 2016-06-30 | Jr Chem, Llc | Rosacea treatments and kits for performing them |
| US20110008271A1 (en) * | 2009-07-13 | 2011-01-13 | Jr Chem, Llc | Rosacea treatments using polymetal complexes |
| IN2012DN02657A (en) | 2009-10-29 | 2015-09-11 | Colgate Palmolive Co | |
| JP2013529633A (en) * | 2010-06-23 | 2013-07-22 | コルゲート・パーモリブ・カンパニー | Encapsulation of ingredients in a lactose matrix to form an effective encapsulating agent |
| WO2012064319A1 (en) | 2010-11-08 | 2012-05-18 | Colgate-Palmolive Company | Oral compositions containing microaggregates |
| US8952057B2 (en) | 2011-01-11 | 2015-02-10 | Jr Chem, Llc | Compositions for anorectal use and methods for treating anorectal disorders |
| BR112015031726A2 (en) * | 2013-06-24 | 2017-07-25 | Procter & Gamble | smudge-proof oral care composition |
| MX2016006399A (en) * | 2013-11-22 | 2016-08-01 | Procter & Gamble | Regimen for providing smooth tooth feel. |
| EP3071581A1 (en) * | 2013-11-22 | 2016-09-28 | The Procter & Gamble Company | Regimen for controlling or reducing dentine hypersensitivity |
| CN105078851A (en) * | 2015-09-24 | 2015-11-25 | 丹东康齿灵牙膏有限公司 | Toothpaste without adding preservative and inhibiting bacteria by means of plant essential oil component and preparation |
| US10383807B2 (en) | 2016-05-20 | 2019-08-20 | The Procter & Gamble Company | Regimen for providing smooth tooth feel |
| BR112022017654A2 (en) | 2020-03-03 | 2022-10-18 | Unilever Ip Holdings B V | AQUEOUS TOOTHPASTE GEL WITHOUT ALCOHOL |
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| US4022880A (en) | 1973-09-26 | 1977-05-10 | Lever Brothers Company | Anticalculus composition |
| US4749575A (en) * | 1983-10-03 | 1988-06-07 | Bio-Dar Ltd. | Microencapsulated medicament in sweet matrix |
| US4647452A (en) | 1985-11-08 | 1987-03-03 | Lever Brothers Company | Oral compositions of salicylamides and zinc salts for the synergistic inhibition of dental plaque |
| JPH0629173B2 (en) * | 1986-11-20 | 1994-04-20 | 花王株式会社 | Granules |
| US5059416A (en) * | 1989-06-26 | 1991-10-22 | Warner-Lambert Company | Zinc compound delivery system with improved taste and texture |
| DE4305713A1 (en) * | 1993-02-25 | 1994-09-01 | Hoechst Ag | Method and device for evenly distributing a small amount of liquid on bulk materials |
| US5330748A (en) * | 1993-05-19 | 1994-07-19 | Church & Dwight Co., Inc. | Dentifrices containing zinc oxide particles |
| US5372803A (en) | 1993-09-02 | 1994-12-13 | Chesebrough-Pond's Usa Co., Division Of Conopco, Inc. | Dental compositions with zinc and bicarbonate salts |
| US5958458A (en) * | 1994-06-15 | 1999-09-28 | Dumex-Alpharma A/S | Pharmaceutical multiple unit particulate formulation in the form of coated cores |
| SK281514B6 (en) * | 1994-09-21 | 2001-04-09 | Unilever N. V. | Oral compositions containing agglomerates |
| ZA962939B (en) * | 1995-04-12 | 1997-10-13 | Quest Int | Oral care compositions. |
| EP0747037B1 (en) * | 1995-06-08 | 2002-11-06 | Sara Lee/DE N.V. | Mouth-care products |
| US6368586B1 (en) * | 1996-01-26 | 2002-04-09 | Brown University Research Foundation | Methods and compositions for enhancing the bioadhesive properties of polymers |
| US6432449B1 (en) * | 1998-05-18 | 2002-08-13 | Amgen Inc. | Biodegradable sustained-release alginate gels |
| GB9810806D0 (en) * | 1998-05-21 | 1998-07-22 | Boots Co Plc | Odour absorbing agent |
| US6284283B1 (en) * | 1999-10-21 | 2001-09-04 | Alkermes Controlled Therapeutics, Inc. | Method of producing sub-micron particles of biologically active agents and uses thereof |
| KR100309604B1 (en) | 1999-12-20 | 2001-11-03 | 홍지준 | Lithium secondary battery |
| US6316029B1 (en) * | 2000-05-18 | 2001-11-13 | Flak Pharma International, Ltd. | Rapidly disintegrating solid oral dosage form |
-
2002
- 2002-04-25 US US10/132,046 patent/US6592852B1/en not_active Expired - Lifetime
- 2002-12-27 US US10/331,666 patent/US6682720B2/en not_active Expired - Lifetime
-
2003
- 2003-04-23 CN CNB038093464A patent/CN1319509C/en not_active Expired - Lifetime
- 2003-04-23 WO PCT/EP2003/004240 patent/WO2003090702A1/en not_active Application Discontinuation
- 2003-04-23 BR BR0308955-0A patent/BR0308955A/en not_active Application Discontinuation
- 2003-04-23 CA CA002480595A patent/CA2480595A1/en not_active Abandoned
- 2003-04-23 AU AU2003222306A patent/AU2003222306A1/en not_active Abandoned
- 2003-04-23 EP EP03717317A patent/EP1496850A1/en not_active Withdrawn
-
2004
- 2004-09-17 ZA ZA200407495A patent/ZA200407495B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CN1319509C (en) | 2007-06-06 |
| EP1496850A1 (en) | 2005-01-19 |
| WO2003090702A1 (en) | 2003-11-06 |
| BR0308955A (en) | 2005-01-04 |
| US6592852B1 (en) | 2003-07-15 |
| US6682720B2 (en) | 2004-01-27 |
| CN1649564A (en) | 2005-08-03 |
| US20030202945A1 (en) | 2003-10-30 |
| AU2003222306A1 (en) | 2003-11-10 |
| ZA200407495B (en) | 2006-06-28 |
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| Date | Code | Title | Description |
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| EEER | Examination request | ||
| FZDE | Discontinued |