FIELD OF THE INVENTION
[0001] The present invention relates generally to oral care compositions, and more specifically
to oral care compositions usable for cleaning the oral cavity.
BACKGROUND OF THE INVENTION
[0002] Oral hygiene compositions fall into two main categories: dentifrices, and mouthwashes
or rinses. Dentifrices generally contain an insoluble dentally acceptable abrasive
which is utilized to physically cleanse the surface of the teeth. Dentifrices are
generally provided in the form of solid or pasty preparations which can be readily
applied to a toothbrush, for example, powders, pastes or viscous gels.
[0003] Known mouthwash or mouth rinse compositions usually are solutions containing small
amounts of colorings, flavorings and antibacterial or other active ingredients. These
solutions have found use as breath-freshening, anti-cavity, antiseptic and/or anti-plaque
mouth rinses, or gargle preparations and are commonly used in addition to conventional
tooth cleansing dentifrices.
[0004] While mouth rinses and abrasive dentifrices have been produced as separate products
for many years, a satisfactory form of combined product is desired in which an effective
amount of abrasive is maintained in an acceptable stable suspension having a sufficiently
low viscosity that the preparation can be swished between and around teeth.
[0005] There remains, therefore, a need for oral compositions, combining the benefits of
both a toothpaste and a mouthwash.
SUMMARY OF THE INVENTION
[0007] The present invention relates to oral care compositions consisting essentially of:
- a) from 5% to about 10% by weight of a insoluble particulate such as a nonabrasive
particle or dentally acceptable abrasive;
- b) from 0.01% to 5% by weight of suspending polymer which is a mixture of 1) xanthan
gum with 2) microcrystalline cellulose; a microcrystalline cellulose and carboxy methylcellulose
sodium mixture; a mixture of microcrystalline cellulose and a microcrystalline cellulose
and carboxy methylcellulose sodium mixture; or mixtures of various microcrystalline
cellulose and carboxy methylcellulose sodium mixtures;
- c) from 0.1% to 5% of a surfactant system, wherein the surfactant system comprises
a combination of alkyl sarcosines, alkyl polyglucosides and alkylamidopropyl betaine
surfactants; and
- d) at least 45% of a liquid carrier,
wherein said composition has a tan delta of less than 1 at frequencies 0.1 to 100
rads
-1 as measured by an RFSII rheometer with couette geometry at a temperature of 25°C.
[0008] In other embodiments, the present invention relates to oral care compositions consisting
of:
- a) from 5% to 10% by weight of a insoluble particulate such as a nonabrasive particle
or dentally acceptable abrasive;
- b) from 0.01% to 5% by weight of suspending polymer which is a mixture of 1) xanthan
gum with 2) microcrystalline cellulose; a microcrystalline cellulose and carboxy methylcellulose
sodium mixture; a mixture of microcrystalline cellulose and a microcrystalline cellulose
and carboxy methylcellulose sodium mixture; or mixtures of various microcrystalline
cellulose and carboxy methylcellulose sodium mixtures;
- c) from 0.1% to 5% of a surfactant system, wherein the surfactant system comprises
a combination of alkyl sarcosines, alkyl polyglucosides and alkylamidopropyl betaine
surfactants; and
- d) at least 45% of a liquid carrier,
wherein said composition has a tan delta of less than 1 at frequencies 0.1 to 100
rads
-1 as measured by an RFSII rheometer with couette geometry at a temperature of 25°C.
[0009] In addition, other embodiments of the present invention relate to oral care compositions
as defined in the claims for use in a method of cleaning the oral cavity where an
effective amount of the oral care compositions of the present invention are: i) introduced
into the oral cavity (such as by sipping a quantity of the composition), ii) swished
around the oral cavity for a sufficient amount of time to coat the teeth and mucosal
surfaces of the oral cavity and iii) a portion, substantial portion or the bulk of
the composition being expelled, swallowed or, otherwise removed from the oral cavity.
As used herein the term "bulk of the composition" means that portion of the composition
which is not retained by the hard and soft tissues of the oral cavity. Optionally,
the teeth can be brushed with a toothbrush if so desired.
DETAILED DESCRIPTION OF THE INVENTION
[0010] The oral care compositions of the present invention can comprise, consist of, or
consist essentially of the essential elements and limitations of the invention described
herein, as well any of the additional or optional ingredients, components, or limitations
described herein.
[0011] The term "comprising" (and its grammatical variations) as used herein is used in
the inclusive sense of "having" or "including" and not in the exclusive sense of "consisting
only of' The terms "a" and "the" as used herein are understood to encompass the plural
as well as the singular.
[0012] All percentages, parts and ratios are based upon the total weight of the composition
of the present invention, unless otherwise specified. All such weights as they pertain
to the listed ingredients are based on the active level and, therefore, do not include
carriers or by-products that may be included in commercially available materials,
unless otherwise specified.
[0013] Unless indicated otherwise, all measurements and tests described herein are conducted
at a temperature of 25°C (or about 25°C).
[0014] The term "safe and effective amount" as used herein means an amount of a compound
or composition such as a topical or system active sufficient to significantly induce
a positive benefit, for example, an antimicrobial effect, but low enough to avoid
serious side effects, i.e., to provide a reasonable benefit to risk ratio, within
the scope of sound judgment of the skilled artisan.
[0015] As used herein the phrase "dentally acceptable" means the compound, substance or
device may be administered to or into the oral cavity and/or surfaces of the oral
cavity, including the teeth and gums, without substantial harmful effects to the oral
cavity and/or its surfaces.
[0016] As used herein the terms "formulation" and "composition" are used interchangeably.
[0017] All viscosity measurements are obtained using an RFSII rheometer (TA Instruments,
New Castle, DE) with couette geometry.
[0018] In certain embodiments, the present invention is a liquid gel dentifrice having rheological
properties such that the liquid gel dentifrice is swishable in the mouth.
[0019] The oral care compositions of the present invention, including the essential and
optional components thereof, are described in detail hereinafter.
Insoluble Particulate
[0020] In certain embodiments, the oral care compositions of the present invention comprise
a safe and effective amount of a water insoluble particulate. The water insoluble
particulate can be an abrasive particle (such as a dentally acceptable abrasive) or
non-abrasive particulate.
In certain embodiments, abrasive particles include, but are not limited to, water
insoluble calcium salts such as calcium carbonate, and various calcium phosphates,
alumina, silica, synthetic resins and mixtures thereof. In further embodiments, the
dentally acceptable abrasive is selected from the group consisting of water insoluble
calcium salts, alumina, silica, synthetic resins and mixtures thereof. Suitable dentally
acceptable abrasives may generally be defined as those having a radioactive dentine
abrasion value (RDA) of from about 30 to about 250 at the concentrations used in the
compositions of the present invention. In certain embodiments, abrasives are non-crystalline,
hydrated, silica abrasives, particularly in the form of precipitated silica or milled
silica gels available commercially, for example, under the trade names ZEODENT (J.
M. Huber Corporation, Edison, NJ), and SYLODENT (W.R. Grace & Co., New York, NY),
respectively. In certain embodiments, the dentally acceptable abrasive is precipitated
or milled silica. Tthe compositions according to the present invention comprise from
5% to 10% by weight of the abrasive.
[0021] Alternatively, the insoluble particulate is a non-abrasive particulate which is visible
to the unaided eye and stable in the compositions of the present invention.
[0022] The non-abrasive particulate can be of any size, shape, or color, according to the
desired characteristic of the product, so long as it is distinctively detected as
an individual particle by the unaided eye. The non-abrasive particulates will typically
have the shape of a small round or substantially round ball, however, platelet or
rod-shaped configurations are also contemplated herein. Generally, a non-abrasive
particulate has an average diameter of from 50 µm to 5000 µm, optionally from 100
µm to 3000 µm, or optionally, from 300 µm to 1000 µm. By the terms "stable" and/or
"stability", it is meant that the abrasive or non-abrasive particulates are not disintegrated,
agglomerated, or separated under normal shelf conditions. In certain embodiments,
the terms "stable" and/or "stability" further mean that the compositions of present
invention contain no visible (to the unaided eye) signs of sedimentation of the insoluble
particulates after 8 weeks, optionally 26 weeks, optionally 52 weeks, at room temperature.
[0023] The non-abrasive particulates herein are typically incorporated in the present compositions
at levels of from 0.01% to 25%, optionally, from 0.01% to 5%, or optionally, from
0.05% to 3%, by weight of the composition.
[0024] The non-abrasive particulate herein will typically comprise a structural material
and/or, optionally, an encompassed material.
[0025] The structural material provides a certain strength to the non-abrasive particulates
so that they retain their distinctively detectable structure in the compositions of
the present invention under normal shelf conditions. In one embodiment, the structural
material further can be broken and disintegrated with very little shear on the teeth,
tongue or oral mucosa upon use.
[0026] The non-abrasive particulates can be solid or liquid, filled or un-filled, as long
as they are stable in the compositions of the present invention. The structural material
used for making the non-abrasive particulates varies depending on the compatibility
with other components, as well as material, if any, to be encompassed in the non-abrasive
particulates. Exemplary materials for making the non-abrasive particulates herein
include: polysaccharide and saccharide derivatives such as crystalline cellulose,
cellulose acetate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose
nitrate, ethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxypropylmethylcellulose
phthalate, methyl cellulose, sodium carboxymethylcellulose, gum acacia (gum arabic),
agar, agarose, maltodextrin, sodium alginate, calcium alginate, dextran, starch, galactose,
glucosamine, cyclodextrin, chitin, amylose, amylopectin, glycogen, laminaran, lichenan,
curdlan, inulin, levan, pectin, mannan, xylan, alginic acid, arabic acid, glucommannan,
agarose, agaropectin, prophyran, carrageenen, fucoidan, glycosaminoglycan, hyaluronic
acid, chondroitin, peptidoglycan, lipopolysaccharide, guar gum, starch, and starch
derivatives; oligosaccharides such as sucrose, lactose, maltose, uronic acid, muramic
acid, cellobiose, isomaltose, planteose, melezitose, gentianose, maltotriose, stachyose,
glucoside and polyglucoside; monosaccharides such as glucose, fructose, and mannose;
synthetic polymers such as acrylic polymers and copolymers including polyacrylamide,
poly(alkyl cyanoacrylate), and poly(ethylene-vinyl acetate), and carboxyvinyl polymer,
polyamide, poly(methyl vinyl ether-maleic anhydride), poly(adipyl-L-lysine), polycarbonate,
polyterephthalamide, polyvinyl acetate phthalate, poly(terephthaloyl-L-lysine), polyarylsulfone,
poly(methylmethacrylate), poly(ε-caprolactone), polyvinylpyrrolidone, polydimethylsiloxane,
polyoxyethylene, polyester, polyglycolic acid, polylactic acid, polyglutamic acid,
polylysine, polystyrene, poly(styrene-acrylonitrile), polyimide, and poly(vinyl alcohol);
and other material such as fat, fatty acid, fatty alcohol, milk solids, molasses,
gelatin, gluten, albumin, shellac, caseinate, bees wax, carnauba wax, spermaceti wax,
hydrogenated tallow, glycerol monopalmitate, glycerol dipalmitate, hydrogenated castor
oil, glycerol monostearate, glycerol distearate, glycerol tristearate, 12-hydroxystearyl
alcohol, protein, and protein derivatives; and mixtures thereof. Components herein
may be described in other sections as useful components for the present composition.
In certain embodiments, the components as described in this section form the structure
of the non-abrasive particulates so as to not be substantially dissolved or dispersed
from the particulates and into the compositions of the present invention under normal
shelf conditions.
[0027] In other embodiments, the structural material herein comprises components selected
from the group consisting of polysaccharides and their derivatives, saccharides and
their derivatives, oligosaccharides, monosaccharides, and mixtures thereof, or optionally,
comprises components are having various degrees of water solubility. In some embodiments,
the structural material comprises lactose, cellulose, and hydroxypropyl methylcellulose.
[0028] Suitable non-abrasive particulates also include organogel particles as described
in detail in
U.S. Pat. No. 6,797,683. Non-abrasive particulates that are organogel particles typically comprise a structural
material selected from poloxamer compounds (i.e. polyoxypropylene-polyoxyethylene
block copolymer such as Pluronic F-127 available from BASF), waxes (e.g., beeswax,
paraffin, water-insoluble wax, carbon-based wax, silicone wax, microcrystalline wax,
etc.), triglycerides, acid triglycerides, polymers, fluoroalkyl (meth)acrylate polymers
and copolymers, acrylate polymers, ethylene/acrylate copolymers, polyethylene, polypropylene
polymers and copolymers, fatty acids, fatty alcohols, fatty acid esters, fatty acid
ethers, fatty acid amides, alkylene polyhydric alcohols, fatty acid amide of an alkanolamine,
glyceryl monostearate, (aryl-substituted)sugars, dibenzyl sorbitol (or mannitoal,
rabbitol, etc.), condensates and precondensates of lower monohydric alcohols, trihydroic
alcohols, lower polyglycols, propylene/ethylene polycondensates, and the like. Optionally,
structural material for non-abrasive particulates that are organogel particles include
beeswax, carnauba wax, low molecular weight ethylene homopolymers (e.g. Polywax 500,
Polywax 1000, or Polywax 2000 polyethylene materials available from Baker Petrolite
Corp.), or paraffin wax.
[0029] The non-abrasive particulates herein may encompass, contain, or be filled with an
encompassed material. Such encompassed material can be water soluble or water insoluble.
Suitable encompassed materials include benefit agents as described herein such as:
oral care actives, vitamins, pigments, dyes, antimicrobial agents, chelating agents,
optical brighteners, flavors, perfumes, humectants, and mixtures thereof. The encompassed
materials herein are substantially retained within the non-abrasive particulates,
and are substantially not dissolved from the particulates and into the compositions
of the present composition under normal shelf conditions.
[0030] Particularly useful commercially available non-abrasive particulates herein are those
with tradenames Unisphere and Unicerin available from Induchem AG (Switzerland), and
Confetti Dermal Essentials available from United-Guardian Inc. (NY, USA). Unisphere
and Unicerin particles are made of microcrystalline cellulose, hydroxypropyl cellulose,
lactose, vitamins, pigments, and proteins. Upon use, the Unisphere and Unicerin particles
can be disintegrated with very little shear and with practically no resistance, and
readily disperse in the compositions of the present invention.
[0032] In certain embodiments, the abrasive and/or nonabrasive particles have a density
different or, optionally, substantially different from the carrier in which it is
formulated.
Suspending Agent
[0033] In certain embodiments, the oral care compositions according to the present invention
also contain at least one suspending polymer as defined in the claims, suitable for
maintaining solid particles (such as abrasives) in a substantially stable suspension
during storage without over-thickening the composition.
The suspending polymer is a mixture of 1) xanthan gum with 2) microcrystalline cellulose;
a microcrystalline cellulose and carboxy methylcellulose sodium mixture; a mixture
of microcrystalline cellulose and a microcrystalline cellulose and carboxy methylcellulose
sodium mixture; or mixtures of microcrystalline cellulose and carboxy methylcellulose
sodium mixtures
[0034] Suitable suspending agents include xanthan, available commercially for example under
the trade names, respectively, KELCOGEL and KELTROL (CP Kelco U.S., Inc. Atlanta,
GA). In specific embodiments the xanthan gum has the following specifications:
| Particle Size |
As measured using Tyler Standard Screen Scale |
| -80 mesh (180 µm) |
≥ 95% through |
| Loss on Drying |
≤ 15.0% |
| Solution pH |
|
| -1% gum in deionized water |
from 6.0 to 8.0 |
| Transmittance |
≥ 85% |
| -1% gum in deionized water (600 nm) |
| Pyruvic Acid |
≥ 1.5% |
| Assay |
from 91.0% to 108.0% xanthan gum |
| Ash |
from 6.5% to 16.0% |
| Heavy Metals |
≤ 10.0 mg/kg (ppm) |
| Lead |
≤ 2.0 mg/kg (ppm) |
| Arsenic |
≤ 2.0 mg/kg (ppm) |
| Mercury |
≤ 1.0 mg/kg (ppm) |
| Cadmium |
≤ 1.0 mg/kg (ppm) |
| Isopropyl Alcohol |
≤ 500 mg/kg (ppm) |
| Cellulase Activity |
< 0.02 Absorbance Units (AU) |
| Bacteria* |
|
| -48 hours |
≤ 100 cfu/g |
| - 5 days |
≤ 500 cfu/g |
| Fungal (Yeast and Mold) Count |
≤ 100 cfu/g |
| Coliform |
Negative by Most Probable Number (MPN) |
| Escherichia coli |
Not present in 25 g |
| Salmonella spp. |
Not present in 25 g |
| Staphylococcus aureus |
Not present in 1.0 g |
| Pseudomonas aeruginosa |
Not present in 1.0 g |
| *Total viable mesophilic aerobic count |
[0035] Xanthan gums falling within the scope of such specifications include, but are not
limited to, Keltrol CG-T xanthan gum as described in CP Kelco's product data sheet
document no. 385-X (effective date 06 December 2006).
[0036] Suitable suspending agents also include microcrystalline cellulose or a mixture of
microcrystalline cellulose and carboxymethylcellulose sodium. Microcrystalline cellulose
and mixtures of microcrystalline cellulose and carboxymethylcellulose sodium (hereinafter
MCC/CMC) are available from FMC Corporation (Philadelphia, PA) under the trade name
Avicel®. In certain embodiments, such mixtures have a ratio of microcrystalline cellulose
to carboxymethylcellulose sodium of from 20:1 to abut 1:1, optionally, from 15:1 to
3:1, or optionally, from 10:1 to 5:1.
[0037] In specific embodiments, microcrystalline cellulose and carboxymethylcellulose sodium
is Avicel CL-611 (85% microcrystalline cellulose with 70% colloidal content, co-processed
with 15% low viscosity carboxymethyl cellulose). Other useful colloidal MCC/CMCs include,
but not limited to, Avicel PC-611 (85% microcrystalline cellulose with 70% colloidal
content, co-processed with 15% low viscosity carboxymethyl cellulose); Avicel® RC
581 (89% microcrystalline cellulose with 70% colloidal content, co-processed with
11% medium viscosity carboxymethyl cellulose); Avicel® RC 591 (88% microcrystalline
cellulose with 70% colloidal content, co-processed with 12%, 50/50 medium/low viscosity
carboxymethyl cellulose); and Avicel® RC 501 (91% microcrystalline cellulose with
70% colloidal content, co-processed with 9% medium viscosity carboxymethyl cellulose).
Mixtures of the above MCC/CMC mixtures may also be used.
[0038] The suspending agent is a mixture of 1) xanthan gum with 2) a microcrystalline cellulose;
a MCC/CMC mixture; mixtures of the microcrystalline cellulose and MCC/CMC; or mixtures
of the various MCC/CMC mixtures.
[0039] In specific embodiments, the ratio of 1) the xanthan gum to 2) the microcrystalline
cellulose; MCC/CMC mixture; mixtures of the microcrystalline cellulose and MCC/CMC;
or mixtures of the various MCC/CMC mixtures is from 0.5:1 to 25:1, optionally, from
1:1 to 20:1, optionally from 1:1 to 10:1.
[0040] The compositions of the present invention comprise from 0.01 to 5%, optionally from
0.05% to 3%, optionally from 0.05% to 1%, or optionally from 0.05% to 0.5%, by weight
of the composition of a suspending agent.
Surfactant System
[0041] Surfactants, which are surface active agents, are incorporated into the compositions
of the present invention to aid wetting, to improve the cleansing capability of the
compositions, to produce a cosmetically acceptable foam in use, to solubilize flavoring
oils when present and to improve the extent and quality of foaming produced by the
oral compositions of the present invention.
[0042] The present invention incorporates a surfactant system to provide adequate foam generation
and/or consistency. The surfactant system is capable of providing adequate foam generation
and/or consistency even after a portion, substantial portion or the bulk of the composition
of the present invention is expectorated, swallowed or otherwise removed from the
oral cavity, the form being generated from the remaining film of the composition on
the teeth, tongue or other oral or mucosal surfaces of the mouth.
[0043] Surfactants suitable for use in the surfactant system are those that are reasonably
stable and generate appropriate foam throughout a wide pH range. In certain embodiments,
the surfactant is a combination of anionic, nonionic, amphoteric surfactants. Anionic
surfactants useful herein include, but are not limited to, sarcosine type surfactants
or sarcosinates; taurates such as sodium methyl cocoyl taurate; alkyl sulfates such
as sodium trideceth sulfate or sodium lauryl sulfate; sodium lauryl sulfoacetate;
sodium lauroyl isethionate; sodium laureth carboxylate; sodium dodecyl benzenesulfonate
and mixtures thereof. Many suitable anionic surfactants are disclosed in
U.S. Pat. No. 3,959, 458, to Agricola, et al.
[0044] Nonionic surfactants which can be used in the compositions of the present invention
include, but are not limited to, compounds produced by the condensation of alkylene
oxide groups (hydrophilic in nature) with an organic hydrophobic compound which may
be aliphatic or alkyl-aromatic in nature. Examples of suitable nonionic surfactants
include, but are not limited to, alkyl polyglucosides; block copolymers such as ethylene
oxide and propylene oxide copolymers e.g. Poloxamers; ethoxylated hydrogenated castor
oils available commercially for example under the trade name CRODURET (Croda Inc.,
Edison, NJ), and/or ethoxylated sorbitan esters such as PEG-80 sorbitan laurate or
those available commercially for example under the trade name TWEEN (Croda, Edison,
NJ); fatty alcohol ethoxylates; polyethylene oxide condensates of alkyl phenols; products
derived from the condensation of ethylene oxide with the reaction product of propylene
oxide and ethylene diamine; ethylene oxide condensates of aliphatic alcohols; long
chain tertiary amine oxides; long chain tertiary phosphine oxides; long chain dialkyl
sulfoxides; and mixtures thereof.
[0045] The amphoteric surfactants useful in the present invention include, but are not limited
to, derivatives of aliphatic secondary and tertiary amines in which the aliphatic
radical can be a straight chain or branched and wherein one of the aliphatic substituents
contains from about 8 to about 18 carbon atoms and one contains an anionic water-solubilizing
group, e.g., carboxylate, sulfonate, sulfate, phosphate, or phosphonate. Examples
of suitable amphoteric surfactants include, but are not limited alkylimino-diproprionates,
alkylamphoglycinates (mono or di), alkylamphoproprionates (mono or di), alkylamphoacetates
(mono or di), N-alkyl β-aminoproprionic acids, alkylpolyamino carboxylates, phosphorylated
imidazolines, alkyl betaines, alkylamido betaines, alkylamidopropyl betaines, alkyl
sultaines, alkylamido sultaines, and mixtures thereof. In certain embodiments, the
amphoteric surfactant is selected from the group consisting of alkylamidopropyl betaines,
amphoacetates such as sodium lauroamphoacetate and mixtures thereof. Mixtures of any
of the above mentioned surfactants can also be employed. A more detailed discussion
of anionic, nonionic and amphoteric surfactants can be found in
U.S. Pat. Nos. 7,087,650 to Lennon;
7,084,104 to Martin et al.;
5,190,747 to Sekiguchi et al.; and
4,051,234, Gieske, et al..
[0046] In some embodiments, it may also be possible to include cationic surfactants. Suitable
cationic surfactants include, but are not limited to, cetyl trimethylammonium chloride
(CTAB), hexadecyltrimethylammonium bromide (HDTAB), stearyl dimethylbenzylammonium
chloride, lauryl dimethylbenzylammonium chloride, cetyl dimethylethylammonium halide,
cetyl dimethylbenzylammonium halide, cetyl trimethylammonium halide, dodecyl ethyldimethylammonium
halide, lauryl trimethylammonium halide, coconut alkyltrimethylammonium halide, and
N,N-C
8-20-dialkyldimethylammonium halide. Other suitable compounds for the cationic surfactant
include bis(hydrogenated tallow alkyl) dimethylammonium chloride which is known to
adsorb onto the surface with hydrophobic groups oriented away from it, 2-hydroxydodecyl-2-hydroxyethyl
dimethyl ammonium chloride and N-octadecyl-N,N',N'-tris-(2-hydroxyethyl)-1,3-diaminopropane
dihydrofluoride.
[0047] The surfactant system of the present invention comprises a combination of alkyl sarcosines,
alkyl polyglucosides, and alkylamidopropyl betaine surfactants.
[0048] In some embodiments, the anionic surfactant is an alkyl sarcosine which typically
has an alkyl group containing from 10 to 24, optionally from 12 to 20, optionally
15 to 18 carbon atoms. Salts can be readily formed by reacting the alkyl sarcosines
with an appropriate base, such as sodium, potassium, ammonium hydroxide, monoethanol
amine, diethanol amine or triethanol amine. Some representative examples of sodium
alkyl sarcosines which can be used include sodium lauroyl sarcosinates, sodium cocoyl
sarcosinates, sodium myristol sarcosinates sodium oleoyl sarcosinates sodium stearyl
sarcosinates and similar sarcosinates. In specific embodiments, the oral care compositions
of the present invention incorporate sodium lauroyl sarcosinate as the sarcosine surfactant.
Sodium lauroyl sarcosinate is commercially available from Chattem Chemicals, Inc.
as Hamposyl® L-30.
[0049] In some other embodiments, the nonionic surfactant is an alkyl polyglucosides nonionic
surfactant. In specific embodiments, the present invention incorporates long chain
alkyl polyglucosides. Suitable long chain alkyl polyglucosides include condensation
products of (a) a long chain alcohol containing from 6 to 22, optionally from 8 to
14 carbon atoms, with (b) glucose or a glucose-containing polymer. The alkyl polyglucosides
have about 1 to about 6 glucose residues per molecule of alkyl glucoside. Suitable
alkyl polyglucosides include, but are not limited to, coco glucoside, decyl glucoside,
and lauryl glucoside. In other specific embodiments, the oral care compositions of
the present invention incorporate lauryl glucoside as the alkyl polyglucosides. Lauryl
glucoside is commercially available from Cognis Corp. as Plantaren 1200 N UP.
[0050] In some embodiments, the amphoteric surfactant is an alkylamidopropyl betaine as
represented by the following structural formula

wherein R
1 is a long chain alkyl radical having from 1 to 18, optionally from 10 to about 16
carbon atoms. In specific embodiments, the alkylamidopropyl betaine incorporated into
the oral care compositions of the present invention is cocamidopropyl betaine.
[0051] In certain embodiments, the anionic, nonionic and amphoteric surfactants are incorporated
into the surfactant system at a ratio of from 80:10:10 to 20:40:40, optionally 60:20:20
to 40:30:30, or optionally 50:25:25.
[0052] The surfactants or surfactant systems are present at a level of from 0.1% to 5%,
or optionally from 0.2% to 2.5% by weight of the composition.
[0053] In some embodiments, the surfactant systems or surfactant(s) are incorporated into
the compositions of the present invention and screened using a specific foam generation
and screening test.
Foam Generation and Screening Test
[0054] The foam generation and screening test used to characterize the foams of the present
invention comprises the steps of diluting a composition comprising the surfactant
systems or surfactant(s) of the present invention with an artificial saliva solution
comprising:
| Sodium Chloride |
1.2236 gm |
| Potassium Chloride |
1.215 gm |
| Calcium Chloride |
0.3178 gm |
| Potassium Phosphate Monobasic |
2.7532 gm |
| Potassium Phosphate Dibasic |
3.5053 gm |
| Deionized Water |
2000 ml |
such that the mixture comprises 80% of the surfactant containing composition and 20%
of the artificial saliva solution, the mixture is then blended for 10 seconds using
a Oster 14-speed blender (model number 6855) on the easy clean speed setting (speed
setting No. 1).
[0055] A 0.005 gram sample of the foam from the surface of the mixture inside the blender
was removed using a spatula.
[0056] The 0.005 gram foam sample was placed on a 25mm x 75mm glass slide having two 0.634mm
PET spacers positioned on each corner of the slide. A second slide was placed onto
the first slide and spaced by the PET spacers ensuring that there was a monolayer
of foam between the two slides.
[0057] The slide was mounted on the Olympus optical microscope (model BX-51 with Discover
Details 5 Image Analysis software stage), adjusting the microscope to reflectance
mode and capturing the image using the 5X objective and then analyzed.
[0058] Foams generated from compositions incorporating the surfactant(s) or surfactant systems
of the present invention and using the foam generation and screening test described
above have a bubble size distribution such that for each 0.005 grams of foam, at least
30, optionally 50, optionally 65, optionally 80, optionally 100, optionally 125, optionally
150, optionally 175, or optionally 200 bubbles have a diameter of less than 50 microns
and additionally, or alternatively, wherein the foams have a bubble size distribution
such that for each 0.005 grams of foam occupying an area of 25mm x 75mm x 1.270mm,
at least 90%, optionally at least 95%, optionally at least 98% of the bubbles have
a diameter of less than 50 microns.
[0059] In alternative embodiments, the above mentioned surfactants are incorporated singly
or in various other combinations.
Foam Enhancing Agents
[0060] In certain embodiments, the composition of the present invention incorporates a foam
enhancing agent to further increase the number or percentage of bubbles having a diameter
of less than 50 microns in the bubble size distribution generated by the surfactants
or surfactant systems of the present invention.
[0061] Suitable foam enhancing agents include, but are not limited to, natural seaweed extract,
natural seed gum, natural plant exudates, natural plant extracts, natural fiber extracts,
biosynthetic gums, gelatins, biosynthetic process starch or cellulosic materials,
alginates, carrageenans, guar, locust, tara, arabic gum, ghatti gum, agar gum, pectin,
other like hydrocolloid source material, salts thereof, or mixtures thereof. Suspending
agents mentioned above may also be useful as foam enhancing agents. In specific embodiments,
the foam enhancing agent is selected from the group consisting of alginates, carrageenans,
salts thereof or mixtures thereof. In certain other embodiments, the foam enhancing
agent is carrageenan.
[0062] The foam enhancing agent(s) are present at a level of from 0.001% to 12%, optionally
from 0.01% to 8%, optionally from 0.1% to 5%, or optionally from 0.2 to 2.5% by weight
of the oral care composition.
[0063] In some embodiments, when the foam enhancing agents are incorporated into the compositions
of the present invention with the above-mentioned surfactant systems or surfactant(s)
and screened using the foam generation and screening test, the foams generated by
the screening test have a bubble size distribution such that for each 0.005 grams
of foam at least 150, optionally 200, optionally 225, optionally 250, optionally 275,
optionally 300, optionally 325, optionally 350, optionally 375, or optionally 400
bubbles have a diameter of less than 50 microns and additionally, or alternatively,
wherein the foams generated by the screening test have a bubble size distribution
such that for each 0.005 grams of foam occupying an area of 25mm x 75mm x 1.270mm,
at least 90%, optionally at least 95%, optionally at least 98% of the bubbles have
a diameter of less than 50 microns.
Gas Generating Agents or Materials
[0064] In certain embodiments, gas is used to generate foam in the oral cavity. This is
specifically useful in embodiments in which the teeth are manually cleaned with a
clean instrument, such as a toothbrush, after a portion, substantial portion or the
bulk of the composition has been removed (expectorated) from the oral cavity.
The oral composition may comprise a foam generating agent or materials. The foam generating
agent or materials may be gas generating agent or materials. Foamable embodiments
may include gas-generating materials such as, but limited to, peroxide generating
compounds; alkali metal bicarbonate salts such as sodium or potassium bicarbonate
in combination with organic acids; compressed air, butane, isopentane, nitrous oxide
or carbon dioxide; volatile hydrocarbons or mixture of volatile hydrocarbons (of typically
3 to 6 carbons in chain length); and mixtures thereof. Further, gas generating agent
or materials may be selected from the group consisting of peroxide generating compounds;
alkali metal bicarbonate salts such as sodium or potassium bicarbonate in combination
with organic acids; compressed air, butane, isopentane, nitrous oxide or carbon dioxide;
volatile hydrocarbons or mixture of volatile hydrocarbons; and mixtures thereof.
[0065] Suitable peroxide generating compounds include, but not limited to, peroxides such
as hydrogen peroxide, urea peroxide, calcium peroxide and mixtures thereof; perborates
such as sodium perborate, potassium perborate and mixtures thereof; percarbonates
such as sodium percarbonate, potassium percarbonate and mixtures thereof; metal chlorites
such as calcium chlorite, barium chlorite, magnesium chlorite, lithium chlorite or
sodium chlorite, potassium chlorite and mixtures thereof; peroxyacids such as peroxyacetic
acid; and mixtures thereof.
[0066] In some embodiments gas can be generated by mixing two or more separated formulations
prior (or just prior) to usage such as by combining acids such as tartaric acid, citric
acid, fumaric acid, adipic acid, malic acid, oxalic acid, or sulfamic acid and mixtures
thereof with carbonate salts such as sodium carbonate, calcium carbonate, magnesium
carbonate, ammonium carbonate, potassium carbonate, sodium bicarbonate, calcium bicarbonate
and mixtures thereof to produce an effervescent reaction.
[0067] In yet another embodiment gas can be generated in-vivo during usage by incorporating
gaseous liquids such as carbonated liquids into the product during manufacture and/or
just prior to usage. In this embodiment the invention can either be a single formulation
or two or more formulations kept separated from each other and mixed prior (or just
prior) to usage.
[0068] In still other embodiments, the compositions of the present invention are free of
or essentially free of gas-generating agents or materials. "Essentially free" as used
with respect to gas-generating agents or materials is defined as formulations having
less than 5%, optionally, 3%, optionally, 1%, optionally, 0.01% or zero percent, by
weight of the total composition of a gas-generating agent or material.
Rheological Properties
[0069] In some embodiments, the oral care compositions or formulations are stable and pourable
for rinsing, having rheological properties including the ability to suspend particles,
pour easily, and be swishable in the mouth without negative viscosity build. These
formulations also provide adequate substantivity such that the formulation material
is retained in mouth, post expectoration (or removal), so that, if toothbrushed, the
brushing experience meets consumer expectations (i.e., adequate foaming, body, mouthfeel
etc.) for improving the post rinse and/or brush-sensory experience.
[0070] Dynamic mechanical rheological properties as a function of frequency and temperature
are useful tools for predicting the overall physical stability of concentrated colloidal
dispersions containing particulates.
[0071] By using dynamic rheology, the prediction of physical stability can often be accomplished
in less than three (3) hours. The dynamic or oscillatory rheology technique is performed
in two parts. First, a strain sweep test (frequency constant, strain variable) defines
the linear viscoelastic range (LVR). Second, frequency scans (from 0.01 to 5.0 Hz)
are performed at various temperatures, from 5 to 49°C (40-120°F). In certain embodiments,
the frequency scans are performed in the LVR. Dynamic rheology measurements yield
data on the elastic (G') and viscous (G") moduli. Plotting the elastic to viscous
moduli ratio as a function of frequency and temperature generates a plot which is
a "fingerprint" of the dispersion's colloidal stability. The G'/G" ratios correlate
well with observed physical stability properties. Then Tan (delta) is calculated by
the ratio of G" to G', or tan (delta) = G"/G'. This represents the viscous fraction
to elastic fraction of the suspension.
[0072] The oral care compositions of the present invention have a Tan delta of less than
1, optionally less than 0.75, optionally less than 0.5, at frequencies of between
0.1 to 100 rads
-1 as measured by an RFSII rheometer (TA Instruments, New Castle, DE) with couette geometry.
[0073] "Pourability" of oral care formulations is defined as the capability of moving in
a continuous flow. The terms "Swishing" "Swishable" or "Swishability of' as they relate
to the oral care compositions of the present invention mean moving or the ability
to move the composition with sufficient force to produce a sibilant, or hissing, sound
by movement i) through and/or around the teeth and/or ii) around the oral cavity,
where such movement can occur for a period of time without noticeable tiring or fatiguing
of the jaw muscles of the user.
[0074] Steady state viscosity measurements give information on relevant ranges of viscosities
that may provide consumer acceptable pourability and swishability in the mouth. In
certain embodiments, the compositions of the present invention have a pourability
(first) viscosity of less than 2000 centipoise, optionally less than 1500 centipoise,
optionally less than 1000, optionally less than 700, optionally less than 500 centipoise,
optionally less than 300 centipoise, at a shear rate of 10s
-1. In certain embodiments, the compositions of the present invention have a swishability
(second) viscosity of less than 1000 centipoise, optionally less than 500 centipoise,
optionally less than 300, optionally less than 150, optionally less than 100 centipoise,
optionally less than 50 centipoise at a shear rate of 100s
-1.
[0075] In certain embodiments, the compositions of the present invention are shear thinning.
Shear thinning is an effect where viscosity decreases with increasing rate of shear
stress. Materials that exhibit shear thinning are called pseudoplastic.
[0076] In certain embodiments of the present invention, the oral care compositions as herein
described are used regularly, from 1 to 4, optionally from 2 to 3, times daily, in
place of a conventional dentifrice. A typical usage involves introducing a safe and
effective amount or quantity (for example, at least 1, optionally, at least 5, optionally,
at least 10, optionally, at least 15, optionally, at least 20 milliliters) of the
oral care composition into the oral cavity, swishing the composition around the oral
cavity and/or through the teeth for sufficient time to coat the teeth, and expelling,
swallowing or otherwise removing a portion or substantial portion of the composition
from the mouth. The composition is swished around the oral cavity and/or through the
teeth for at least 10, optionally, at least 20, optionally, at least 30, optionally,
at least 50, optionally, at least 75, optionally, at least 100, optionally, at least
120, times or swishing cycles within a period of at least 1, optionally, at least
5, optionally, at least 10, optionally, at least 15, optionally, at least 20, optionally,
at least 30, optionally, at least 45, optionally, at least 60, optionally, at least
90 seconds.
[0077] Optionally, the teeth are brushed with a tooth cleaning instrument such as a toothbrush
for a sufficient amount of time to provide desired cleaning. In certain embodiments,
it has been found that, upon introduction and removal of a portion, substantial portion
or the bulk of the compositions of the present invention from the oral cavity, sufficient
composition remains on the teeth, tongue and/or oral tissues or mucosa of the mouth
to give a satisfactory foaming and abrasive action, when optionally used in conjunction
with a toothbrush, and to provide a long-lasting fresh mouth feel after use.
Optional Ingredients
Oral Care Actives
[0078] In certain embodiments, the compositions of the present invention further contain
oral care actives. In certain embodiments, the oral care actives include, but are
not limited to, anti-plaque agents, fluoride ion sources such as sodium fluoride,
sodium monofluorophosphate and amine fluorides (providing, for example, 1-1500 ppm
of fluoride ion, optionally 200-1150 ppm of fluoride ion); anti-calculus agents such
as water-soluble pyrophosphate salts, optionally, specific alkali metal pyrophosphates;
chelating agents; tooth desensitization agents which reduce tooth sensitivity including
potassium salts such as potassium oxalate, potassium nitrate and potassium chloride
(for example 1% to 5% by weight) and strontium salts such as strontium chloride and
strontium acetate (for example 2% to 10% by weight); tooth whitening agents and vitamins
such as vitamin A.
[0079] In certain embodiments, suitable anti-plaque and/or anti-gingivitis agents include,
but are not limited to, oral care enzymes, non-ionic antibacterial agents such as
bromochlorophene and triclosan and cationic agents such as cetylpyridinium chloride
and chlorhexidine salts, and mixtures thereof. Furthermore, it is known that certain
water-insoluble flavoring oils such as anethole, eucalyptol, methyl salicylate, thymol
and menthol have an antibacterial effect at high concentrations. In certain embodiments,
the oral care compositions of the present invention comprise from 0.001% to 1%, optionally
from 0.01% to 0.5% by weight of a non-ionic antibacterial agent. In some embodiments,
the water-insoluble anti-tartar agents comprise zinc salts such as zinc citrate. In
certain embodiments, the compositions of the present invention can comprise from 0.1%
to 1% of a water-insoluble anti-calculus agent.
Carriers and Carrier Ingredients
[0081] In certain embodiments, the compositions according to the present invention may comprise
at least 45%, optionally, at least 60%, optionally, at least 80% to 99%, or, optionally,
at least 80% to 90% by weight of a liquid carrier, but it will be understood by those
skilled in the art that this proportion depends to a large extent on the proportion
of abrasive incorporated into the composition. In certain embodiments, the liquid
carrier may be in the form of a solution, emulsion or microemulsion of components
and, in some embodiments, contain at least about 5% by weight water, optionally, at
least about 10% by weight water. In certain embodiments, alcohol such as ethanol may
optionally form part of the liquid carrier, for example, from about 5% to about 35%
by weight of the liquid carrier, and, in some embodiments, is particularly useful
in oral care compositions having a high flavor impact and breath-freshening and/or
antiseptic properties. Optionally, the liquid carrier of the present invention is
an orally acceptable liquid carrier. The phrase "orally acceptable" means that the
carrier is suitable for application to the surfaces of the oral cavity or ingestion
by a living organism including, but not limited to, mammals and humans without undue
toxicity, incompatibility, instability, allergic response, and the like.
[0082] In specific embodiments, the compositions of the present invention can be in the
form of mouthrinses, mouthwashes, gels, liquid gels, liquid dentifrices and the like.
[0083] In certain embodiments, the liquid carrier contains humectants, substances that promote
retention of moisture, to enhance the mouthfeel of the product and to prevent drying
out. In some embodiments, humectants include, but are not limited to, glycerin, sorbitol
and glycols such as propylene glycol and polyethylene glycol, and mixtures thereof.
In other embodiments, alternatively or in addition to the humectant, the liquid carrier
may contain silicone oils, for example, in an amount of from about 0.1% to about 5%
by weight. In certain clear product embodiments, where the refractive index is an
important consideration, the refractive index of abrasive system can be chosen or
made to match the refractive index of the carrier or solvent system.
[0084] In certain embodiments, the oral care compositions of the present invention may contain
flavoring agents commonly in the form of oils commercially available as mouthwash,
mouth rinse, and toothpaste flavors. In some embodiments, flavoring agents include,
but are not limited to, peppermint, spearmint, aniseed, menthol, eucalyptus, clove,
thymol and wintergreen, and mixtures thereof. In certain embodiments, high levels
of flavoring oils can be incorporated into the oral care compositions of the present
invention by forming an emulsion in the liquid carrier. This is particularly advantageous
in certain embodiments, where the compositions are required to have little or no alcohol
content but which need to have a high flavor impact. Conventional oral care compositions
containing high flavoring concentrations generally utilize substantial levels of alcohol
to dissolve the flavoring oils. In certain embodiments of the present invention, high
flavoring content may also be desirable where oral care compositions contain an unpleasant
tasting active ingredient, for example an agent to reduce tooth sensitivity such as
strontium chloride, potassium nitrate and/or potassium oxalate or an anti-tartar agent
such as tetrapotassium pyrophosphate salts. In certain embodiments, the oral care
compositions according to the invention contain from 0.01% to 1.5%, optionally, from
0.1% to 1% by weight of the flavoring agent.
[0085] In certain embodiments, the oral care compositions of the invention incorporate colorings,
which may be soluble coloring agents conventionally used in mouthwashes or dentifrices
or may be the insoluble particulates such as color pigments or whitening agents such
as titanium dioxide, pearlizing agents such as mica, or mixtures thereof. Color pigments
are generally available in a wider range of colors and are less susceptible to fading
than soluble coloring agents and may therefore be used to advantage in the compositions
of the present invention.
[0086] In certain embodiments, the pH of the oral care compositions according to the present
invention is generally in the range of from 3.5 to 10.0, or optionally, from 4.0 to
8.0. In other embodiments, if desired, the pH can be controlled with acid, for example
citric acid, or base, for example sodium hydroxide, or buffered, for example with
citrate, phosphate, benzoate or bicarbonate buffering salts.
[0087] Various other materials may optionally be incorporated into certain embodiments of
the compositions of the present invention which will be well known to those skilled
in the art. These include, for example, at least one of sweeteners such as saccharin
and aspartame; preservatives such as sodium benzoate and parabens. In certain embodiments,
these optional additives may together comprise from 0.01% to 10%, optionally, from
0.1% to 5% by weight of the composition.
[0088] In certain embodiments, the compositions of the present invention are free of or
essentially free of bioavailability affecting compounds. As used herein, "bioavailability
affecting compound", means compounds that negatively affect the bioavailability of
any incorporated oral care actives such as by binding the oral care actives or inactivating
the oral care actives. "Essentially free" as used with respect to bioavailability
affecting compounds is defined as formulations having less than 5%, optionally, 3%,
optionally, 1%, or optionally, 0.01%, by weight of the total composition of a bioavailability
affecting compound. In certain embodiments, the bioavailability affecting compound
can include, but is not limited to, chemically unmodified clays, water soluble calcium
salts, water soluble magnesium salts, water soluble aluminum salts, carbonate salts
and mixtures thereof. In other embodiments, the oral care compositions of the present
invention are free of or essentially free of chemically unmodified clays.
[0089] In certain embodiments, the compositions of the present invention are also free of
or essentially free of gellan gum. "Essentially free" as used with respect to gellan
gum is defined as formulations having less than 5%, optionally, 3%, optionally, 1%,
or optionally, 0.01%, by weight of the total composition of the gellan gum. Gellan
gum tends to be negatively affected by such manufacturing processes as formulation
reproducibility and mass production formulation scale-up. Specifically, gellan gum
requires significant shear forces (such as the forces provided by a Silverson L4RT
high shear mixer at rpm ranges of from 5500 - 9800 rpm) for uniform dispersion of
the gum in solvents such as water. Accomplishing such shear is typically dependent
on the specific equipment used and mixers such as propeller mixers generally used
in some labs and/or as part of standard mass production processes will not provide
the consistent and efficient shear necessary to hydrate the gellan gum for activity.
[0090] In certain embodiments, the compositions according to the invention may be shaken
prior to use or, alternatively, provide stable suspensions during use without being
shaken prior to use.
[0091] In other embodiments, the compositions according to the present invention are pourable,
pleasant tasting suspensions which remain physically stable after storage, or in still
further embodiments, after long-term storage, for example, for over 3 months at ambient
temperatures and in particular have suitable sedimentation times, for example, greater
than 3, 6, 12, or 24 months.
[0092] In certain embodiments, a further advantage of the oral care compositions according
to the present invention relates to their ease of manufacture compared to the manufacture
of conventional dentifrices such as toothpastes. It is well known in the art that
stringent production methods are required to obtain a satisfactory toothpaste product,
for example manufacture must be carried out under vacuum to prevent the formation
of air bubbles which produce a visually unacceptable product and may lead to oxidation
of the flavorings and syneresis (the process by which a liquid is separated from a
gel owing to further coagulation) of the product. In contrast, certain embodiments
of the oral care compositions of the present invention are easily formulated by dispersing
the abrasive into a mixture of surfactant, suspending agent and liquid carrier, under
normal production conditions without the need for an external vacuum or vacuumed environment.
[0093] The oral care compositions according to the invention are illustrated by the following
examples.
EXAMPLES
[0094] The oral compositions of the present invention as described in following examples
illustrate specific embodiments of compositions of the present invention, but are
not intended to be limiting thereof.
EXAMPLE 1
Oral Care Formulations and Preparation.
[0095] A series of oral care compositions, listed in Tables 1 through 5 below, were formulated.
Table 1: Liquid Gel Dentifrices
| Formulation |
1-1* |
1-2* |
| Ingredient |
w/w% |
w/w% |
| Deionized Water |
55.2906 |
55.5706 |
| Citric acid |
0.1000 |
0.01000 |
| Sorbitol solution |
20.0000 |
20.0000 |
| Sodium Saccharin |
0.1170 |
0.1170 |
| Silica |
5.0000 |
4.0000 |
| Keltrol CG-T Xanthan gum |
0.3000 |
----- |
| P TIC Xanthan gum |
----- |
0.3000 |
| Ethyl alcohol |
18.3030 |
18.3030 |
| Menthol |
0.0323 |
0.0323 |
| Thymol |
0.0639 |
0.0639 |
| Methyl salicylate |
0.0660 |
0.0660 |
| Eucalyptol |
0.0922 |
0.0922 |
| Mint Flavor |
0.0850 |
0.0850 |
| FD&C Green |
----- |
0.0100 |
| N-Propanol |
----- |
0.5000 |
| Polaxamer 407 |
0.2500 |
0.2500 |
| Sodium lauryl sulfate |
0.3000 |
0.6000 |
| TOTAL |
100.0000 |
100.0000 |
[0096] The comparative liquid gel dentifrices of Table 1 were prepared according to the
following steps. In Step A, using a first suitable beaker (herein after referring
to it as the main beaker), a quantity of deionized water was added to the main beaker,
sprinkle in the citric acid and mixed until it dissolved. A Silverson L4RT high shear
mixer (Silverson Machines Inc. East Longmeadow, MA) was used to disperse the gums
by sprinkling them in slowly, and mixed for 5 to 10 minutes. Once gums were dispersed,
the mixer was switched to a Caframo mixer (Caframo Limited Wiarton, Ontario, Canada),
and mixing continued. Sorbitol and saccharin sodium were added, and the solution was
mixed well until homogeneous. Then, the silica was added and mixed well until it was
uniformly distributed.
[0097] In Step B (the alcohol phase), in a second suitable beaker, ethanol, n-propanol,
thymol, menthol, methyl salicylate, eucalyptol, mint flavor and Poloxamer 407 were
combined, and mixed well until homogeneous.
[0098] In Step C (the surfactant blend), in a third suitable beaker, deionized water and
sodium lauryl sulfate, were combined and mixed until the mixture was visually clear
to the unaided eye.
[0099] In the final step, the contents of the second beaker (from Step B) were added to
the main beaker (of Step A) and mixed well until homogenous. Finally, the contents
of the third beaker (of Step C) were added to the main beaker and mixed until the
batch was homogeneous.
Table 2: Liquid Gel Dentifrices
| Formulation |
2-1 |
2-2 |
| Ingredient |
w/w% |
w/w% |
| Deionized Water |
52.3541 |
48.7400 |
| Disodium EDTA |
0.3000 |
0.3000 |
| Sodium Fluoride |
0.1878 |
0.1878 |
| Avicel CL-611 microcrystalline cellulose/ carboxy methylcellulose sodium |
1.0000 |
0.7000 |
| 1% Solution Keltrol CG-T Xanthan gum |
10.0000 |
15.0000 |
| Carrageenan |
0.0500 |
0.0500 |
| Sorbitol solution |
20.0000 |
20.0000 |
| Sucralose solution |
0.1200 |
0.1200 |
| Sodium Saccharin |
0.1170 |
0.1170 |
| Silica |
5.0000 |
5.0000 |
| Sodium Lauroyl Sarcosinate |
0.8000 |
0.8000 |
| Lauryl glucoside |
0.8000 |
0.8000 |
| Cocamidopropyl betaine |
0.4000 |
0.4000 |
| Ethyl alcohol |
8.4211 |
6.5264 |
| Polaxamer 407 |
----- |
0.2500 |
| Menthol |
----- |
0.0646 |
| Thymol |
----- |
0.1278 |
| Methyl salicylate |
----- |
0.1320 |
| Eucalyptol |
----- |
0.1844 |
| Mint Flavor |
0.4500 |
0.5000 |
| TOTAL |
100.0000 |
100.0000 |
[0100] The liquid gel dentifrices of Table 2 were prepared according to the following steps.
In Step A, the disodium EDTA, sodium fluoride, cocamidopropyl betaine, sodium lauroyl
sarcosinate, and deionized water were mixed in a first beaker until all solids were
dissolved.
[0101] In Step B, xanthan gum, in the form of a powder, was added to deionized water in
a second beaker to create a 1% solution. Mixing was performed in a Silverson L4RT
high shear mixer (Silverson Machines Inc. East Longmeadow, MA) until all solids were
dissolved.
[0102] In Step C, deionized water was added to a third beaker. Using the Silverson L4RT
high shear mixer, the carrageenan was dispersed in the water by sprinkling it in slowly,
and mixing until homogeneous. The Avicel CL-611 microcrystalline cellulose/ sodium
carboxy methylcellulose was sprinkled in, and the Silverson L4RT high shear mixer
continued to operate until the mixture was homogeneous. The mixer was switched to
Caframo mixer (Caframo Limited Wiarton, Ontario, Canada) and mixing continued. Sorbitol,
sodium saccharin, and sucralose were added, and the solution was mixed well until
homogeneous. The lauryl glucoside was melted, and added to the batch, and mixing was
continued until homogeneous. The xanthan gum solution (Step B, second beaker) was
added to the batch, and mixing continued until homogenous. Then, the silica was added
and mixed until the batch was homogeneous.
[0103] In Step D (the alcohol phase), in a fourth beaker, ethanol and mint flavor (for formula
11706-093), or ethanol, mint flavor, thymol, menthol, methyl salicylate, eucalyptol,
and Poloxamer 407 (for formula 11706-094) were combined, and mixed until homogeneous.
[0104] In the final step, the contents of the fourth beaker (from Step D) were added to
the third beaker (of Step C) and mixed well until homogenous. Finally, the contents
of the first beaker (of Step A) were added to the main beaker and mixed until the
batch was homogeneous.
Table 3: Liquid Gel Dentifrices
| Formulation |
3-1* |
| Ingredient |
w/w% |
| Deionized Water |
70.1995 |
| Sodium Saccharin |
0.1000 |
| Sodium Fluoride |
0.0500 |
| DI Water |
5.0000 |
| Glycerine |
10.0000 |
| Methylparaben |
0.2000 |
| Montmorillonite clay |
3.5000 |
| Silica |
10.0000 |
| Sodium Lauryl Sulfate |
0.5000 |
| Dye |
0.0005 |
| Mint Flavor |
0.4500 |
| TOTAL |
100.0000 |
[0105] The comparative liquid gel dentifrices of Table 3 were prepared according to the
following steps. In Step A, the sodium saccharin, sodium fluoride, and deionized water
were mixed in a first beaker until all solids were dissolved.
[0106] In Step B, the glycerine was added to a second beaker, and mixing started. Methylparaben
was added, and the solution was mixed until homogeneous. Then the montmorillonite
clay was added to the batch, and mixing continued until homogeneous. The contents
of the first beaker (Step A) were added to the batch of second beaker, and mixing
continued until homogeneous. Then, the silica was added to the second beaker and mixed
until the batch was homogeneous. Finally, the sodium lauryl sulfate, flavor, and dye
were sequentially added to the second beaker and mixed until the batch was homogeneous.
Table 4: Liquid Gel Dentifrices
| Formulation |
4-1* |
| Ingredient |
w/w% |
| Deionized Water |
62.0366 |
| Disodium EDTA |
0.3000 |
| Sodium Fluoride |
0.0500 |
| Acryate copolymer |
3.3500 |
| Carrageenan |
0.0500 |
| Sorbitol solution |
20.0000 |
| Sucralose solution |
0.1200 |
| Sodium Saccharin |
0.1170 |
| Silica |
5.0000 |
| Sodium Lauroyl Sarcosinate |
0.8000 |
| Lauryl glucoside |
0.8000 |
| Cocamidopropyl betaine |
0.4000 |
| Ethyl alcohol |
6.5264 |
| Mint Flavor |
0.4500 |
| TOTAL |
100.0000 |
[0107] The comparative liquid gel dentifrices of Table 4 were prepared according to the
following steps. In Step A, the disodium EDTA, sodium fluoride, cocamidopropyl betaine,
sodium lauroyl sarcosinate, and deionized water were mixed in a first beaker until
all solids were dissolved.
[0108] In Step B, deionized water was added to a second beaker. Using a Silverson L4RT high
shear mixer (Silverson Machines Inc. East Longmeadow, MA), the carrageenan was dispersed
in the water by sprinkling them in slowly, and mixing until homogeneous. The mixer
was switched to Caframo mixer (Caframo Limited Wiarton, Ontario, Canada) and mixing
continued. The acryate copolymer was added, and the solution was mixed until homogeneous.
Sorbitol, sodium saccharin, and sucralose were added, and the solution was mixed until
homogenous. The lauryl glucoside was melted, and added to the batch, and mixing was
continued until homogeneous. Then, the silica was added to the second beaker and mixed
until the batch was homogeneous.
[0109] In Step C (the alcohol phase), in a third beaker, ethanol and mint flavor were combined,
and mixed until homogeneous.
[0110] In the final step, the contents of the third beaker (from Step C) were added to the
second beaker (of Step B) and mixed until homogenous. Finally, the contents of the
first beaker (of Step A) were added to the second beaker and mixed until the batch
was homogeneous.
Table 5: Liquid Gel Dentifrices
| Formulation |
5-1* |
| Ingredient |
w/w% |
| Deionized Water |
54.3806 |
| Citric Acid |
0.0100 |
| Sorbitol solution |
20.0000 |
| Sodium Saccharin |
0.1170 |
| Hydroxypropyl methylcellulose |
1.0000 |
| Silica |
5.0000 |
| Ethyl alcohol |
18.3030 |
| Polaxamer 407 |
0.2500 |
| Menthol |
0.0323 |
| Thymol |
0.0639 |
| Methyl salicylate |
0.0660 |
| Eucalyptol |
0.0922 |
| Mint Flavor |
0.0850 |
| Sodium Lauryl Sulfate |
0.6000 |
| TOTAL |
100.0000 |
[0111] The comparative liquid gel dentifrices of Table 5 were prepared according to the
following steps. In Step A, the sodium lauryl sulfate and deionized water were mixed
in a first beaker until all solids were dissolved.
[0112] In Step B, deionized water was added to a second beaker. Using a Silverson L4RT high
shear mixer (Silverson Machines Inc. East Longmeadow, MA), the hydroxypropyl methylcellulose
was dispersed in the water by sprinkling them in slowly, and mixing until homogeneous.
Sorbitol and sodium saccharin were added, and the solution was mixed well until homogeneous.
Then, the silica was added the second beaker and mixed until the batch was homogeneous.
[0113] In Step C (the alcohol phase), in a third beaker, ethanol, mint flavor, thymol, menthol,
methyl salicylate, eucalyptol, and Poloxamer 407 were combined, and mixed until homogeneous.
[0114] In the final step, the contents of the third beaker (from Step C) were added to the
second beaker (of Step B) and mixed well until homogenous. Finally, the contents of
the first beaker (of Step A) were added to the main beaker and mixed until the batch
was homogenous.
Table 6: Inventive Liquid Gel Dentifrices
| Formulation |
6-1* |
6-2* |
6-3* |
| Ingredient |
w/w% |
w/w% |
w/w% |
| Deionized Water |
58.1687 |
58.8237 |
58.8237 |
| Sorbitol (70% Solution) |
20.0000 |
20.0000 |
20.0000 |
| Iota Carrageenan |
-------- |
-------- |
-------- |
| 35% Hydrogen Peroxide solution |
-------- |
-------- |
-------- |
| Ethyl alcohol (200 proof) |
10.0000 |
10.0000 |
10.0000 |
| Hydrated silica |
-------- |
-------- |
-------- |
| Sodium lauroyl sarcosinate |
0.4000 |
-------- |
-------- |
| Lauryl Glucoside |
0.4000 |
-------- |
0.2750 |
| Cocamidopropyl betaine |
0.2000 |
-------- |
0.7400 |
| Sodium trideceth sulfate |
-------- |
1.3300 |
-------- |
| PEG-80 sorbitan laurate |
-------- |
0.2750 |
-------- |
| Sodium lauroamphoacetate |
-------- |
0.7400 |
-------- |
| Sodium methyl cocoyl taurate |
-------- |
-------- |
1.3300 |
| Sodium Fluoride |
0.1613 |
0.1613 |
0.1613 |
| Sucralose Solution |
0.1200 |
0.1200 |
0.1200 |
| Sodium Saccharin |
0.1000 |
0.1000 |
0.1000 |
| Flavor |
0.4500 |
0.4500 |
0.4500 |
| TOTAL |
100.0000 |
100.0000 |
100.0000 |
[0115] The comparative liquid gel dentifrices of Table 6 were prepared according to the
following steps. In Step A, the surfactant or surfactant combinations (using the sodium
lauroyl sarcosinate, cocamidopropyl betaine, sodium trideceth sulfate, PEG-80 sorbitan
laurate, and/or sodium methyl cocoyl taurate as listed in Table 8), sodium fluoride,
and deionized water were mixed in a first beaker until all solids were dissolved.
[0116] In Step B, deionized water was added to a second beaker. Using a Silverson L4RT high
shear mixer (Silverson Machines Inc. East Longmeadow, MA), the carrageenan were sprinkled
in, and the Silverson L4RT high shear mixer continued to operate until the mixture
was homogeneous. The mixer was switched to Caframo mixer (Caframo Limited Wiarton,
Ontario, Canada) and mixing continued. Sorbitol, sodium saccharin, and sucralose were
added, and the solution was mixed well until homogeneous. The lauryl glucoside (if
required by the formulation in Table 6) was melted, and added to the batch, and mixing
was continued until homogeneous. Then, the silica (if required by the formulation
in Table 6) was added and mixed until the batch was homogeneous.
[0117] In Step C (the alcohol phase), in a third beaker, ethanol and mint flavor were combined,
and mixed until homogeneous.
[0118] In the final step, the contents of the third beaker (from Step C) were added to the
second beaker (of Step B) and mixed well until homogenous. Finally, the contents of
the first beaker (of Step A) and the hydrogen peroxide solution (as in the case of
Formulation 8-1) were added to the main beaker and mixed until the batch was homogeneous.
Table 7: Comparative Liquid Gel Dentifrices
| Formulation |
7-1* |
| Ingredient |
w/w% |
| Deionized Water |
58.5687 |
| Sorbitol (70% Solution) |
20.0000 |
| High acyl gellan gum |
--- |
| Iota Carrageenan |
--- |
| Ethyl alcohol (200 proof) |
10.0000 |
| Hydrated silica |
--- |
| Sodium lauryl sulfate |
0.6000 |
| Sodium Fluoride |
0.1613 |
| Sucralose Solution |
0.1200 |
| Sodium Saccharin |
0.1000 |
| Flavor |
0.4500 |
| TOTAL |
100.0000 |
[0119] The comparative liquid gel dentifrices of Table 7 were prepared according to the
following steps. In Step A, the sodium lauryl sulfate, sodium fluoride, and deionized
water were mixed in a first beaker until all solids were dissolved.
[0120] In Step B, deionized water was added to a second beaker. Using a Silverson L4RT high
shear mixer (Silverson Machines Inc. East Longmeadow, MA), the carrageenan were sprinkled
in, and the Silverson L4RT high shear mixer continued to operate until the mixture
was homogeneous. The mixer was switched to Caframo mixer (Caframo Limited Wiarton,
Ontario, Canada) and mixing continued. Sorbitol, sodium saccharin, and sucralose were
added, and the solution was mixed well until homogeneous. Then, the silica (if required
by the formulation in Table 7) was added and mixed until the batch was homogeneous.
[0121] In Step C (the alcohol phase), in a third beaker, ethanol and mint flavor were combined,
and mixed until homogeneous.
[0122] In the final step, the contents of the third beaker (from Step C) were added to the
second beaker (of Step B) and mixed well until homogenous. Finally, the contents of
the first beaker (of Step A) was added to the main beaker and mixed until the batch
was homogeneous.
[0123] The list of ingredients, and their trade names and sources, are shown on Table 8.
Table 8: Ingredients list.
| Ingredient |
Trade Name |
Source |
| |
|
|
| Acrylate copolymer |
Aqua SF-1 (30%) |
Lubrizol Corp. |
| Carrageenan |
Genuvisco TPC-1 |
CP Kelco |
| Citric acid |
Citric acid anhydrous |
DSM Nutritional Products Inc |
| Cocamidopropyl betaine |
Tegobetaine CKD |
Degussa |
| Deionized Water |
NA |
In-house |
| Disodium EDTA |
Disodium EDTA |
Cognis Corporation |
| Dye |
FD&C Green #3 |
Sensient Colors |
| Ethyl alcohol |
Alcohol USP 195 proof |
Pharmco Products |
| Ethyl alcohol |
Alcohol USP 200 proof |
Pharmco Products |
| Ethyl alcohol |
Alcohol USP 195 proof |
Pharmco Products |
| Eucalyptol |
Eucalyptol |
Ungerer and Company |
| Flavor - Mint |
N&A SNO Mint 11397 |
Firmenich |
| Flavor - Mint |
N&A Wintergreen Mint 539274T |
Firmenich |
| Flavor - Peppermint |
N&A Peppermint Tingle 539314T |
Firmenich |
| Glycerin |
Glycerin |
Cognis Corporation |
| Hydrated silica |
Zeodent 113 |
J. M. Huber Corporation |
| Hydrated silica/TiO2 |
Sylodent 750 |
Grace Davison |
| Hydrogen Peroxide (35% solution) |
Peralkali |
Degussa |
| Hydroxypropyl methylcellulose K100M |
Methocel K100M |
Dow Chemical |
| Hydroxypropyl methylcellulose |
Methocel 40-202 PCG |
Dow Chemical |
| Lauryl glucoside |
Plantaren 1200 N UP |
Cognis Corp. |
| Low acyl gellen gum |
Kelcogel CG-LA |
CP Kelco |
| Menthol |
L-Menthol, nat. USP/FCC |
Polarome International |
| Methylparaben |
Nipagin M |
Mallinckrodt Baker Inc. |
| Methyl salicylate |
Methyl salicylate NF |
Rhodia Inc. |
| Microcrystalline cellulose/carboxy methylcellulose sodium |
Avicel CL-611 |
FMC Corporation |
| Montmorillonite clay |
Gelwhite H |
Southern Clay Inc. |
| N-Propanol |
N-Propanol |
Penta Manufacturing Company |
| Polaxamer 407 |
Pluronic F-127 |
BASF Corporation |
| Sodium Fluoride |
Sodium Fluoride Powder |
Mallinckrodt Baker Inc. |
| Sodium lauroyl sarcosinate |
Hamposyl L-95 |
Chattem Chemicals, Inc. |
| Sodium lauryl sulfate |
Emicol LZ N |
Huntsman |
| Sodium lauryl sulfate |
Stepanol WA |
Stepan Company |
| Sodium saccharin |
Saccharin Sodium Granular, USP |
PMC Specialties Group |
| Sodium saccharin |
Syncal GS |
PMC Specialties |
| Sorbitol |
Sorbitol solution (70%), USP |
SPI Polyols, Inc. |
| Sucralose |
Sucralose solution (25%) |
McNeil |
| Thymol |
Thymol |
Symrise |
| Xanthan gum |
Keltrol CG-T |
Monsanto Company |
| Xanthan gum |
P TIC pre-hydrated rapid - 3 powder |
TIC Gums |
EXAMPLE 2
Rheology Testing
[0124] Formulations described in Example 1 were tested for their rheological properties.
The same instrumentation was used for both the oscillatory and steady shear measurements.
The instrument used was a strain controlled oscillatory rheometer (model RFSII, TA
Instruments, New Castle, DE). Couette and parallel plate geometries were used in all
of the testing.
[0125] Steady shear viscosity was measured to probe the time dependence and pseudoplasticity
of the samples over a broad range of shear rates from 0.02/s to 100/s. These measurements
were intended to cover the range of consumer use at both room temperature and body
temperature, such as physical appearance, pourability, and tooth swishing. Measurements
were made at 0.02, 0.1, 0.5, 1, 10, 25, 50 and 100 s
-1 for all samples.
[0126] For the dynamic oscillatory measurements, the strain sweeps were completed at a frequency
of 10 radians/s to determine the viscoelastic region and the frequencies were done
in the linear region or near at a strain of 0.02 at RT. The estimation of stability
was based on the strength of the gel network. If there was no relaxation, and tan
(delta) < 1.0, stability was deemed to be good.
[0127] Table 9 shows the results of viscosity and tan delta values for various formulations.
Table 9: Viscosity (shear rates 10/s and 100/s) and Tan delta (frequencies 0.1 and
100 radians/s).
| Formulation |
Comment |
Viscosity at 10/s (cP) |
Viscosity at 100/s (cP) |
Tan delta at 0.1 rad/s |
Tan delta at 100 rad/s |
| |
|
|
|
|
|
| 1-1* |
0.3% Keltrol Xanthan |
525 |
102 |
0.69 |
0.02 |
| 1-2* |
0.3% TIC Xanthan |
|
|
1.05 |
0.34 |
| 2-1 |
1% Avicel 611, 0.1% Keltrol Xanthan |
391 |
86 |
0.60 |
0.44 |
| 2-2 |
0.7% Avicel 611, 0.15% Keltrol Xanthan |
382 |
80 |
0.68 |
0.43 |
| 3-1* |
Montmorillonite Clay |
172 |
42 |
0.62 |
0.40 |
| 4-1* |
Acrylate Copolymer |
89 |
54 |
4.15 |
0.82 |
| 5-1* |
1% HPMC |
|
|
26.01 |
1.00 |
[0128] The table shows that formulations 1-1*, 2-1, 2-2, and 3-1* all met the tan delta
criteria of less than 1.0 at frequencies 0.1 to 100 rads
-1, and additionally meet the viscosity criteria at a shear rate of 10s
-1 of less than 700 centipoise, and the viscosity criteria at a shear rate of 100s
-1 of less than 150 centipoise. Formulation 3-1 contained clay.
EXAMPLE 3
Stability Testing
[0129] All formulations from Example 1 were checked initially and, if no obvious visible
(to the unaided eye) signs of sedimentation had occurred, at 1 month, 2 months, 3
months, with the following parameters measured each time:
- 1) Appearance
- 2) taste
- 3) viscosity
- 4) sedimentation
- 5) pH
[0130] Formulations 1-1*, 2-1, 2-2 all had no obvious visible (to the unaided eye) signs
of sedimentation at 1 month, 2 months, and 3 months. Formulations 4-1 and 5-1, each
having tan delta values greater than 1 at 0.1 rads, showed visible (to the unaided
eye) sedimentation.
EXAMPLE 4
[0131] The oral care compositions of the present invention can also be formed in gel mouth
rinses. An example of a gel mouth rinse is provided in Table 10.
TABLE 10: Gel Mouth rinse
| Ingredient |
w/w% |
| Deionized Water |
66.6255 |
| Disodium EDTA |
0.3000 |
| Sodium Fluoride |
0.1878 |
| Alcohol |
8.4211 |
| Avicel CL-611 |
0.7000 |
| Xanthan Gum |
0.1500 |
| Carrageenan |
0.0500 |
| Sorbitol |
20.0000 |
| Sucralose |
0.1200 |
| Sodium Saccharin |
0.1170 |
| Sodium Lauroyl Sarcosinate |
0.8000 |
| Cocamidopropyl Betaine |
0.4000 |
| Lauryl Glucoside |
0.8000 |
| Agar, Vitamin E Actate, Pigment |
0.0500 |
| Poloxamer 407 |
0.2500 |
| Menthol |
0.0840 |
| Thymol |
0.1278 |
| Methyl Salicylate |
0.1320 |
| Eucalyptol |
0.1844 |
| Flavor |
0.5000 |
| Color |
0.0004 |
| Total |
100.0000 |
[0132] The gel mouth rinse of Table 10 was prepared according to the following steps. In
Step A, the disodium EDTA, sodium fluoride, cocamidopropyl betaine, sodium lauroyl
sarcosinate, and deionized water were mixed in a first beaker until all solids were
dissolved.
[0133] In Step B, xanthan gum, in the form of a powder, was added to deionized water in
a second beaker to create a 1% solution. Mixing was performed in a Silverson L4RT
high shear mixer (Silverson Machines Inc. East Longmeadow, MA) until all solids were
dissolved.
[0134] In Step C, deionized water was added to a third beaker. Using the Silverson L4RT
high shear mixer, the carrageenan was dispersed in the water by sprinkling them in
slowly, and mixing until homogeneous. The Avicel CL-611 microcrystalline cellulose/
sodium carboxy methylcellulose was sprinkled in, and the Silverson L4RT high shear
mixer continued to operate until the mixture was homogeneous. The mixer was switched
to Caframo mixer (Caframo Limited Wiarton, Ontario, Canada) and mixing continued.
sorbitol, sodium saccharin, and sucralose were added, and the solution was mixed well
until homogeneous. The lauryl glucoside was melted, and added to the batch, and mixing
was continued until homogeneous. The xanthan gum solution (Step B, second beaker)
was added to the batch, and mixing continued until homogenous. Then, the agar, vitamin
E actate, pigment was added and mixed until the batch was homogeneous.
[0135] In Step D (the alcohol phase), in a fourth beaker, ethanol and mint flavor, or ethanol,
mint flavor, thymol, menthol, methyl salicylate, eucalyptol, and Poloxamer 407 were
combined, and mixed until homogeneous.
[0136] In the final step, the contents of the fourth beaker (from Step D) were added to
the third beaker (of Step C) and mixed well until homogenous. Finally, the contents
of the first beaker (of Step A) were added to the main beaker and mixed until the
batch was homogeneous.