CN116807908A - Oral care liquid compositions containing high-density solid particles and suspension methods - Google Patents
Oral care liquid compositions containing high-density solid particles and suspension methods Download PDFInfo
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Abstract
The present application provides an oral care liquid composition comprising high density solid particles and a method of suspending, the composition comprising: 1) high density solid particles, 2) a suspending agent system, 3) an orally acceptable carrier; wherein the density of the solid particles is 1.2-3.9g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The viscosity of the oral care liquid composition is less than or equal to 3000mpa.s; the suspension system comprises xanthan gum, gellan gum and sodium chloride. The suspending agent system in the oral care liquid composition can enable high-density solid particles (the density is 1.2-3.9g/cm 3 ) Stably and uniformly suspendFloat in the composition formulation.
Description
Technical Field
The application relates to the technical field of oral care, in particular to an oral care liquid composition containing high-density solid particles and a method for stably suspending the high-density solid particles in the oral care liquid composition.
Background
The addition of functional or decorative ingredients to a laundry product is a common practice to enhance consumer acceptance or use experience, wherein maintaining the added ingredients in suspension in the product formulation is one of the very consumer attractive product presentation forms that utilize a suspending agent system to uniformly and stably disperse the functional or decorative ingredients in the product formulation to enhance the efficacy of the functional ingredients or to enhance the cosmetic appearance of the product.
For example, commercial sakura shower gels of corolline use acrylate copolymers as suspending agent systems to uniformly distribute the sakura petals throughout the product formulation and remain stable throughout the commercial period.
For example, chinese patent application CN13271921a (example 2) discloses two oral care compositions comprising petals, which can be distributed substantially uniformly throughout a suspended oral care composition by adding composition (2) with 0.5% xanthan gum as suspending agent, as compared to composition (1).
For another example, chinese application CN113967190 discloses a suspension mouthwash, the mouthwash formulation comprising probiotics, to solve the problem of sedimentation of the probiotics, gellan gum and potassium nitrate are added as suspending agents to the formulation.
In summary, solid particle suspended products are common, but the above products are characterized by either high viscosity of the product formulation or low density of suspended particles, and the oral care solutions require lower viscosity (viscosity less than or equal to 3000 mpa.s) to better deliver actives or better flow in the oral cavity, under which conditions it is still challenging to keep high density solid particles such as mica or polymer particles stably suspended in the composition.
Disclosure of Invention
The first technical problem to be solved by the present application is to provide an oral care liquid composition comprising high density solid particles. The application is directed to a relatively low viscosity (viscosity less than or equal to 3000 Pa.s) oral care liquid composition capable of providing high density solid particles (density of 1.2-3.9g/cm 3 ) Uniformly suspended and stable in the composition formulation.
The second problem addressed by the present application is to provide a method of stabilizing high density solid particles in suspension in an oral care liquid composition.
In order to solve the first technical problem, the application adopts the following technical scheme:
an oral care liquid composition comprising high density solid particles comprising:
1) The high-density solid particles are used as a material,
2) The suspension agent system is used for preparing the suspension agent,
3) An orally acceptable carrier;
wherein,,
the density of the solid particles is 1.2-3.9g/cm 3 ；
The viscosity of the oral care liquid composition is less than or equal to 3000mpa.s;
the suspension system comprises xanthan gum, gellan gum and sodium chloride.
As a preferred embodiment, the suspension system further comprises a methyl vinyl ether maleic anhydride copolymer (hereinafter abbreviated to Gantrez).
As a preferred embodiment, the methyl vinyl ether maleic anhydride copolymer is present in the composition in an amount of 0.3 to 2% by weight.
In a preferred embodiment, the oral care liquid composition has a pH in the range of 5.9 to 9.5.
As a more preferred embodiment, the oral care liquid composition has a pH in the range of 7.4 to 8.6.
As a preferred embodiment, the oral care liquid composition comprises a pH adjustor for adjusting the pH of the composition formulation to between 5.5 and 9.5; the pH regulator includes, but is not limited to, one or more of sodium hydroxide, hydrochloric acid, sulfuric acid, citric acid and salts thereof, lactic acid and salts thereof, phosphoric acid and salts thereof, phthalic acid and salts thereof, pyrophosphoric acid and salts thereof, triphosphoric acid and salts thereof, polyphosphoric acid and salts thereof, citric acid and salts thereof, acetic acid and salts thereof.
As a preferred embodiment, the gellan gum is present in the composition at a weight ratio of from 0.01 to 0.1%.
As a more preferred embodiment, the xanthan gum is present in the composition in an amount of 0.01 to 0.1% by weight.
As a preferred embodiment, the sodium chloride is present in the composition in an amount of 0.2 to 0.8% by weight.
As a more preferred embodiment, the sodium chloride is present in the composition in an amount of 0.2 to 0.6% by weight.
As a preferred embodiment, the high density solid particles are one or more of solid pearling agent particles, solid pigment particles, solid opacifying agent particles, organic polymer particles.
As a more preferred embodiment, the solid pearling agent or solid pigment is one or more of mica, silica, carbon powder, titanium dioxide, zinc oxide, hydroxyapatite;
as a more preferred embodiment, the organic polymer is one or more of polylactic acid, corn starch, microcrystalline cellulose, hydroxyethyl methylcellulose, polymethyl methacrylate, polyglutamic acid, sodium hyaluronate, polyacrylate, fish gelatin, gum arabic, paraffin oil.
As a preferred embodiment, the high density solid particles comprise 0.05 to 0.5% by weight of the composition.
As a preferred embodiment, the oral care liquid composition is a liquid toothpaste or mouthwash.
To solve the second technical problem described above, the present application provides a method for suspending high density solid particles in an oral care liquid composition: xanthan gum, gellan gum and sodium chloride were used as suspending agent systems.
Unless otherwise indicated, all starting materials herein are commercially available, and the equipment used in the present application may be conventional in the art or may be conventional in the art.
The beneficial effects of the application are that
In contrast to the prior art, the present application provides an oral care liquid composition comprising a specific suspension system which allows for the suspension of high density solid particles (density of 1.2-3.9g/cm 3 ) Stably and uniformly suspended in the composition formulation.
Detailed Description
In order to more clearly illustrate the present application, the present application will be further described with reference to preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and that this application is not limited to the details given herein.
All percentages and ratios used herein are by weight of the total composition unless otherwise specified. Unless otherwise indicated, all percentages, ratios, and levels of ingredients referred to herein are based on the actual level of the ingredient and do not include solvents, fillers, or other materials that may be combined with the ingredients in commercially available products.
The term "comprising" herein means that other steps and ingredients may be added that do not affect the end result.
The term "preferably" and its variants herein refer to embodiments of the application that are capable of providing particular benefits under particular circumstances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the detailed description of one or more preferred embodiments does not represent additional embodiments, but rather is intended to exclude additional embodiments from the scope of the present application.
The specific conditions are not noted in the embodiment of the application, and the method is carried out according to the conventional conditions or the conditions suggested by manufacturers; the reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
As one aspect of the present application, an oral care liquid composition comprising high density solid particles of the present application comprises:
1) The high-density solid particles are used as a material,
2) The suspension agent system is used for preparing the suspension agent,
3) An orally acceptable carrier;
wherein,,
the density of the solid particles is 1.2-3.9g/cm 3 ；
The viscosity of the oral care liquid composition is less than or equal to 3000mpa.s;
the suspension system comprises xanthan gum, gellan gum and sodium chloride.
As used herein, the term "oral care liquid composition" refers to an oral care liquid composition having a viscosity of less than or equal to 3000 Pa.s. Those skilled in the art will appreciate that stable suspension of high density solid particles is readily achieved in highly viscous compositions such as gel-like compositions (viscosity typically >20000 mpa.s) for toothpastes, jellies, body washes and the like. However, for oral care liquid compositions having a viscosity of less than or equal to 3000mpa.s, achieving stable suspension of high density solid particulates is a significant challenge. The application is characterized in that: in the oral care liquid composition with the viscosity less than or equal to 3000 Pa.s, stable suspension of the high-density solid particles is realized.
High density solid particles
High density solid particles are organic solids, inorganic solids, or a solid mixture of both in any form that are used for decoration in oral care compositions or as delivery actives. The high density solid particles are present in the oral care composition formulation in a non-dissolved form.
In certain embodiments, the high density solid particles have a density in the range of 1.2-3.9g/cm 3 Such as but not limited to 1.2-3.5g/cm 3 ，1.2-3g/cm 3 ，1.2-2.5g/cm 3 ，1.2-2.0g/cm 3 ，1.2-1.5g/cm 3 ，1.5-3.9g/cm 3 ，1.5-3.5g/cm 3 ，1.5-3g/cm 3 ，1.5-2.5g/cm 3 ，1.5-2.0g/cm 3 ，2.0-3.9g/cm3，2.0-3.5g/cm 3 ，2.0-3g/cm 3 ，2.0-2.5g/cm 3 ，2.5-3.9g/cm 3 ，2.5-3.5g/cm 3 ，2.5-3g/cm 3 。
In certain embodiments, the high density solid particles comprise, by mass, 0.05-0.5%, such as, but not limited to, 0.05-0.45%,0.05-0.4%,0.05-0.35%,0.05-0.3%,0.05-0.25%,0.05-0.2%,0.05-0.15%,0.05-0.1%,0.1-0.5%,0.1-0.45%,0.1-0.4%,0.1-0.35%,0.1-0.3%,0.1-0.25%,0.1-0.2%,0.1-0.15%,0.15-0.5%,0.15-0.45%,0.15-0.4%,0.15-0.35%, 0.15-0.25%,0.15-0.2%,0.2-0.5%, 0.1-0.3%, 0.25-0.25%, 0.1-0.25%, 0.2%, 0.25% and 0.25% of the composition.
In certain embodiments, the high density solid particles are one or more of solid pearlescent agent particles, solid pigment particles, solid opacifier particles, organic polymer particles.
In certain more preferred embodiments, the solid pearlescent agent or solid pigment is one or more of mica, silica, carbon dust, titanium dioxide, zinc oxide, hydroxyapatite.
In certain more preferred embodiments, the organic polymer is one or more of polylactic acid, corn starch, microcrystalline cellulose, hydroxyethyl methylcellulose, polymethyl methacrylate, polyglutamic acid, sodium hyaluronate, polyacrylate, fish gelatin, gum arabic, paraffin oil.
Gellan gum
Gellan gum is a hydrocolloid polysaccharide produced by the aerobic fermentation process of carbohydrates by microorganisms including Sphingomonas (Sphingomonas elodea), pseudomonas polymorpha (Pseudomonas elodea), and the like. The molecular structure is a linear chain based on repeating D-glucose, D-glucuronic acid and L-rhamnose units. In the natural state, gellan gum is highly acylated. Gellan gum has been publicly sold in the market.
In certain embodiments, the gellan gum is a low acyl gellan gum that is at least partially deacylated.
In certain embodiments, the gellan gum is present in the oral care liquid composition in a weight ratio of 0.01-0.1%, such as, but not limited to, 0.02-0.1%,0.025-0.1%,0.03-0.1%,0.04-0.1%,0.05-0.1%,0.06-0.1%,0.07-0.1%,0.075-0.1%,0.08-0.1%,0.09-0.1%,0.01-0.09%,0.02-0.09%,0.025-0.09%,0.03-0.09%,0.04-0.09%,0.05-0.09%,0.06-0.09%,0.07-0.09%,0.075-0.09%,0.01-0.08%, 0.025-0.08%,0.03-0.08%,0.04-0.08%,0.05-0.08%, 0.01-0.08%, 075-0.01-0.08%, 0.025-0.075%,0.03-0.075%,0.04-0.075%,0.05-0.075%,0.06-0.075%,0.07-0.075%,0.01-0.06%,0.02-0.06%,0.025-0.06%,0.03-0.06%,0.04-0.06%,0.05-0.06%,0.01-0.06%,0.02-0.06%,0.025-0.06%,0.03-0.06%,0.04-0.06%,0.05-0.06%,0.01-0.05%,0.02-0.05%,0.025-0.05%, 0.02-0.05%, 0.05-0.05%,0.01-0.05%,0.02-0.05%,0.025-0.05%, 0.03-0.04%, 0.03-0.03%, 0.01-0.02%.
Xanthan gum
Xanthan gum is a primary structure consisting of regular repeating units, each containing five sugars: two glucose, two mannose and one glucuronic acid. The backbone is built up from β -D-glucose units linked through the 1-and 4-positions, i.e. the chemical structure is identical to that of cellulose. Trisaccharide side chains are attached to the 3-position of every other glucose residue in the backbone. About half of the terminal D-mannose residues contain pyruvate residues linked to positions 4 and 6.
In certain embodiments, the xanthan gum comprises, by mass, 0.01-0.1%, such as, but not limited to, 0.02-0.1%,0.025-0.1%,0.03-0.1%,0.04-0.1%,0.05-0.1%,0.06-0.1%,0.07-0.1%,0.075-0.1%,0.08-0.1%,0.09-0.1%,0.01-0.09%,0.02-0.09%,0.025-0.09%,0.03-0.09%,0.04-0.09%,0.05-0.09%,0.06-0.09%,0.07-0.09%,0.075-0.09%,0.01-0.08%, 0.025-0.08%,0.03-0.08%,0.04-0.08%,0.05-0.08%, 0.03-0.08%, 0.01-0.08%, 0.025-0.075%,0.03-0.075%,0.04-0.075%,0.05-0.075%,0.06-0.075%,0.07-0.075%,0.01-0.06%,0.02-0.06%,0.025-0.06%,0.03-0.06%,0.04-0.06%,0.05-0.06%,0.01-0.06%,0.02-0.06%,0.025-0.06%,0.03-0.06%,0.04-0.06%,0.05-0.06%,0.01-0.05%,0.02-0.05%,0.025-0.05%, 0.02-0.05%, 0.05-0.05%,0.01-0.05%,0.02-0.05%,0.025-0.05%, 0.03-0.04%, 0.03-0.03%, 0.01-0.02%.
Sodium chloride
In the composition of the present application, the sodium chloride accounts for 0.2 to 0.8% by mass of the composition, such as, but not limited to, 0.2 to 0.7%,0.2 to 0.6%,0.2 to 0.5%,0.2 to 0.4%,0.2 to 0.3%,0.3 to 0.8%,0.3 to 0.7%,0.3 to 0.6%,0.3 to 0.5%,0.3 to 0.4%,0.4 to 0.8%,0.4 to 0.7%,0.4 to 0.6%,0.4 to 0.5%,0.5 to 0.8%,0.5 to 0.7%,0.5 to 0.6%,0.6 to 0.8%,0.6 to 0.7%.
Methyl vinyl ether maleic anhydride copolymer (Gantrez for short)
Methyl vinyl ether maleic anhydride copolymers are copolymers of maleic acid or anhydride and methyl vinyl ether, which are commonly used as bioadhesives in oral care products, as film formers, and to extend the residence time of the active on the oral mucosa or enamel. The present inventors have unexpectedly found that by adding Gantrez to the suspension system, stable suspension of high density solid particles in an oral care liquid composition having a viscosity of less than or equal to 3000 Pa.s can be more effectively achieved at high temperature (40 ℃).
In certain embodiments, the methyl vinyl ether maleic anhydride copolymer is present in the composition at a mass ratio of 0.3 to 2%, such as, but not limited to, 0.5 to 2%,0.75 to 2%,1 to 2%,1.25 to 2%,1.5 to 2%,1.75 to 2%,0.3 to 1.75%,0.5 to 1.75%,0.75 to 1.75%,1.25 to 1.75%,1.5 to 1.75%,0.3 to 1.5%,0.5 to 1.5%,0.75 to 1.5%,1 to 1.5%,1.25 to 1.5%,0.3 to 1.25%,0.5 to 1.25%,0.75 to 1.25%,1 to 1.25%,0.3 to 1%,0.5 to 1%,0.75 to 1%,0.3 to 0.75%,0.5 to 0.75%,0.3 to 0.5%.
Viscosity of oral Care compositions
The viscosity of the oral care liquid composition of the present application is less than or equal to 3000mpa.s, such as, but not limited to, 5-3000mpa.s,5-2800mpa.s,5-2500mpa.s,5-2000mpa.s,5-1500mpa.s,5-1000mpa.s,10-3000mpa.s,10-2800mpa.s,10-2500mpa.s,10-2000mpa.s,10-1500mpa.s,10-1000mpa.s,30-3000mpa.s,30-2800mpa.s,30-2500mpa.s,30-2000mpa.s, 50-280 mpa.s,50-2000mpa.s, 50-1000mpa.s,100-300 mpa.s,100-280 mpa.s,100-2000mpa.s, less than or equal to 500 mPas, less than or equal to 300 mPas, less than or equal to 200 mPas, less than or equal to 100 mPas, less than or equal to 80 mPas, less than or equal to 50 mPas, 5-100 mPas, 10-100 mPas, 20-100 mPas, 30-100 mPas, 40-100 mPas, 50-100 mPas, 80-100 mPas, 5-80 mPas, 10-80 mPas, 20-80 mPas, 30-80 mPas, 40-80 mPas, 50-80 mPas, 5-50 mPas, 10-50 mPas, 20-50 mPas, 30-50 mPas, 40-50 mPas, 10-40 mPas, 20-40 mPas, 30-40 mPas, 10-30 mPas.
pH
The present application has unexpectedly found that when the pH is stabilized between 5.5 and 9.5 in an oral care liquid composition, the suspension stability of high density solid particles in the composition formulation can be improved.
In certain embodiments, the oral care liquid composition has a pH of 5.5 to 9.5, such as, but not limited to, 5.9 to 9.5,6.3 to 9.5,7 to 9.5,7.4 to 9.5,8.1 to 9.5,8.6 to 9.5,6.3 to 9.5,9 to 9.5,5.5 to 9,5.9 to 9,6.3 to 9,7 to 9,7.4 to 9,8.1 to 9,8.6 to 9,5.5 to 8.6,5.9 to 8.6,6.3 to 8.6,7 to 8.6,7.4 to 8.6,8.1 to 8.6,5.5 to 8.1,5.9 to 8.1,6.3 to 8.1,7 to 8.1,7.4 to 8.1,5.5 to 7.4,5.9 to 7.4,6.3 to 7.4,7 to 7.4,5.5 to 7,5.9 to 7,6.3 to 7,5.5 to 6.3,5.9 to 6.3,5.5 to 5.9.
In certain embodiments, the oral care liquid composition comprises a pH adjustor for adjusting the pH of the composition formulation to between 5.5 and 9.5.
In certain embodiments, the pH adjustor comprises one or more of sodium hydroxide, hydrochloric acid, sulfuric acid, citric acid and salts thereof, lactic acid and salts thereof, phosphoric acid and salts thereof, phthalic acid and salts thereof, pyrophosphoric acid and salts thereof, triphosphoric acid and salts thereof, polyphosphoric acid and salts thereof, citric acid and salts thereof, acetic acid and salts thereof.
Other orally acceptable carriers
In the present application, the "orally acceptable carrier" refers to any vehicle suitable for formulating the disclosed oral care liquid compositions; an orally acceptable carrier is not harmful to a mammal when retained in the mouth in the amounts disclosed herein without swallowing for a period of time sufficient to allow effective contact with the tooth surfaces as required by the present application; generally, an orally acceptable carrier is not harmful even if inadvertently swallowed; suitable orally acceptable carriers include, for example, one or more of the following: water, thickeners, pH modifiers, humectants, sweeteners, flavoring agents, visual aids (e.g., pigments, dyes, or mixtures thereof), anticaries agents, antibacterial agents, whitening agents, desensitizing agents, vitamins, preservatives, enzymes, mixtures thereof, and the like.
In certain embodiments of the application, the oral care liquid composition is a liquid toothpaste, mouthwash or mouthwash.
Method for detecting viscosity of oral care liquid composition
1. Selecting a model DV2TRV type viscometer;
2. adjusting the viscometer bracket to keep the viscometer horizontal;
3. turning on a power supply of the viscometer, prompting to perform zero calibration operation (a rotor cannot be connected in the zero calibration process) on a display screen of the viscometer, and performing zero calibration according to the next step; setting the rotating speed of the rotor to 2000 revolutions per second;
4. and (3) adjusting the position of the sample so that the rotor is opposite to the center of the sample. Pressing down a lifting needle on the lifting support, turning on a power supply of the lifting support, and starting the lifting support to automatically descend; clicking an operation button when the rotor contacts the surface of the toothpaste sample, and starting the test; and after the test is completed, turning off the power supply of the lifting bracket, and clicking for storage.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
In the present application, the formulations of examples and comparative examples each includeBasic formula、Suspending agent systemAnddeionized water。
Basic formula 1
Base formulation 1 contained the ingredients described in table 1:
TABLE 1
Suspending agent system 1
The suspension system comprises the ingredients described in table 2:
TABLE 2
| Additive amount (weight percentage) | |
| Acrylic ester copolymer | 2 |
Comparative examples 1-1 to 1-4
Comparative examples 1-1 to 1-4 included base formulation 1, suspension system 1, 0.1wt% solids, and deionized water was added to 100%.
Solid particles were added to the comparative example according to table 3:
table 3:
| comparative examples 1 to 1 | Comparative examples 1 to 2 | Comparative examples 1 to 3 | Comparative examples 1 to 4 | |
| Solid particles 1 | 0.1 | / | / | / |
| Solid particles 2 | / | 0.1 | / | / |
| Solid particles 3 | / | / | 0.1 | / |
| Solid particles 4 | / | / | / | 0.1 |
| Observation of | Suspending | Suspending | Suspending | Suspending |
And (3) injection:
the solid particles 1 had a density of 3.5g/cm 3 Mica powder particles of (a);
the solid particles 2 had a density of 1.2g/cm 3 Polymer particles of (2);
the solid particles 3 had a density of 0.20g/cm 3 Is a plant petal granule;
the solid particles 4 had a density of 0.25g/cm 3 Longjing tea granules.
Comparative examples 1-1 to 1-4 had pH values of 7.9, and comparative examples 1-1 to 1-4 were left at normal temperature for 12 hours, and the appearance was as follows:
table 4:
| comparative examples 1 to 1 | Comparative examples 1 to 2 | Comparative examples 1 to 3 | Comparative examples 1 to 4 | |
| Particulate state | Suspending | Suspending | Suspending | Suspending |
As can be seen from tables 2-4, comparative examples 1-1 to 1-4 refer to the corolline cherry bath cream, the acrylate copolymer is used as a suspending agent system, the addition amount of the acrylate copolymer is 2%, the viscosity of the composition is 27400mPa.s, and after the composition is placed for 12 hours at normal temperature, solid particles in four groups of formulas of comparative examples 1-1 to 1-4 are in a suspending state. That is, in a colloidal composition of high viscosity, almost all solid particles can be stably suspended therein.
Suspending agent System 2
Suspending agent system 2 comprises the ingredients described in table 5 below:
TABLE 5
| Additive amount (weight percentage) | |
| Acrylic ester copolymer | 0.05 |
Comparative examples 2-1 to 2-4
Comparative examples 2-1 to 2-4 included base formulation 1, suspending agent system 2, 0.1% solids, and deionized water to 100%.
Solid particles were added to the comparative examples according to table 6 below.
TABLE 6
| Comparative example 2-1 | Comparative examples 2 to 2 | Comparative examples 2 to 3 | Comparative examples 2 to 4 | |
| Solid particles 1 | 0.1 | / | / | / |
| Solid particles 2 | / | 0.1 | / | / |
| Solid particles 3 | / | / | 0.1 | / |
| Solid particles 4 | / | / | / | 0.1 |
Comparative examples 2-1 to 2-4 had a viscosity of 31mPa.s and a pH of 7.9, and were left at normal temperature for 12 hours, and the appearance was as shown in Table 7 below:
TABLE 7
| Comparative example 2-1 | Comparative examples 2 to 2 | Comparative examples 2 to 3 | Comparative examples 2 to 4 | |
| Particulate state | Precipitation | Precipitation | Suspending | Suspending |
It can be seen from tables 5 to 7:
comparative examples 2-1 to 2-4 also used the acrylate copolymer as the suspending agent system, but the acrylate copolymer was added in an amount of 0.05%, at which time the viscosity of the composition was only 31mpa.s, consistent with the viscosity of conventional oral care compositions.
After comparative examples 2-1 to 2-4 were left at normal temperature for 12 hours, the solid particles of the formulations of comparative examples 2-3 and 2-4 were still in suspension, but the solid particles of the formulations of comparative examples 2-1 and 2-2 were precipitated.
That is, in low viscosity liquid formulations, high density solid particles settle more easily than low density solid particles.
Suspending agent system 3
Suspending agent system 3 contains the ingredients described in table 8 below,
table 8:
| additive amount (weight percentage) | |
| Xanthan gum | 0.5 |
Comparative examples 3-1 to 3-4
Comparative examples 3-1 to 3-4 included base formulation 1, suspending agent system 3, 0.1% solids, and deionized water to 100%.
Solid particles were added in the comparative examples according to table 9 below.
TABLE 9
| Comparative example 3-1 | Comparative example 3-2 | Comparative examples 3 to 3 | Comparative examples 3 to 4 | |
| Solid particles 1 | 0.1 | / | / | / |
| Solid particles 2 | / | 0.1 | / | / |
| Solid particles 3 | / | / | 0.1 | / |
| Solid particles 4 | / | / | / | 0.1 |
Comparative examples 3-1 to 3-4 had a viscosity of 2832mPa.s and a pH of 7.9, and were left at normal temperature for 12 hours, and the appearance was as follows:
table 10
| Comparative example 2-1 | Comparative examples 2 to 2 | Comparative examples 2 to 3 | Comparative examples 2 to 4 | |
| Particulate state | Precipitation | Precipitation | Suspending | Suspending |
As can be seen from tables 8-10:
comparative examples 3-1 to 3-4 use 0.5% xanthan gum as the suspending agent system, at which time the viscosity of the composition was 2832mpa.s, consistent with the viscosity of conventional oral care compositions.
After comparative examples 3-1 to 3-4 were left at room temperature for 12 hours, the solid particles of the formulations of comparative examples 3-3 and 3-4 were still in suspension, but the solid particles of the formulations of comparative examples 3-1 and 3-2 were precipitated.
That is, in low viscosity liquid formulations with 0.5wt% xanthan gum as the suspending agent system, the high density solid particles cannot remain stably suspended.
Suspending agent System 4
The suspension system contained the ingredients described in table 11,
TABLE 11
| Additive amount (weight percentage) | |
| Gellan gum | 0.05 |
| Potassium nitrate | 0.5 |
Comparative examples 4-1 to 4-4
Comparative examples 4-1 to 4-4 included base formulation 1, suspending agent system 4, 0.1% solids, and deionized water to 100%.
Solid particles were added to the comparative example according to table 12 below:
table 12
| Comparative example 4-1 | Comparative example 4-2 | Comparative examples 4 to 3 | Comparative examples 4 to 4 | |
| Solid particles 1 | 0.1 | / | / | / |
| Solid particles 2 | / | 0.1 | / | / |
| Solid particles 3 | / | / | 0.1 | / |
| Solid particles 4 | / | / | / | 0.1 |
Comparative examples 4-1 to 3-4 had a viscosity of 32.6mPa.s and a pH of 7.9, and were left at normal temperature for 12 hours in the following appearance states:
TABLE 13
| Comparative example 4-1 | Comparative example 4-2 | Comparative examples 4 to 3 | Comparative examples 4 to 4 | |
| Particulate state | Precipitation | Precipitation | Suspending | Suspending |
It can be seen from tables 11 to 13:
comparative examples 4-1 to 4-4 used 0.05% gellan gum and 0.5% potassium nitrate as suspending agent systems, where the viscosity of the compositions was only 32.6mpa.s, consistent with the viscosity of conventional oral care compositions.
After comparative examples 4-1 to 4-4 were left at room temperature for 12 hours, the solid particles of the formulations of comparative examples 4-3 and 4-4 were still in suspension, but the solid particles of the formulations of comparative examples 4-1 and 4-2 were precipitated.
That is, in low viscosity liquid formulations with 0.05% gellan gum and 0.5% potassium nitrate as suspending agent systems, the high density solid particles cannot remain stably suspended.
Comparative examples 5 to 6, comparative examples 7 to 1 to 7 to 3, examples 1 to 2
Comparative examples 5-6, comparative examples 7-1 to 7-3, and examples 1-2 were prepared as in table 14 below; the components in table 14 below are all in weight percent.
TABLE 14
From table 14, it can be seen that:
the suspension system of comparative example 5 contained 0.05% gellan gum and 0.5% sodium chloride;
the suspension system of comparative example 6 contained 0.05% xanthan gum and 0.5% sodium chloride;
the suspension system of example 1 contained 0.025% gellan gum, 0.025% xanthan gum, and 0.5% sodium chloride;
the suspension system of example 2 contained 0.025% gellan gum, 0.025% xanthan gum, 0.5% sodium chloride, and 0.5% Gantrez;
the suspension system of comparative example 7-1 contained a suspension system comprising 0.025% gellan gum, 0.025% xanthan gum, 0.5% potassium nitrate, and 0.5% gantrez;
the suspension system of comparative example 7-2 contained a suspension system comprising 0.025% gellan gum, 0.025% xanthan gum, 0.5% sodium nitrate, and 0.5% gantrez;
the suspension system of comparative examples 7-3 contained a suspension system comprising 0.025% gellan gum, 0.025% xanthan gum, 0.5% potassium chloride, and 0.5% gantrez.
Comparative examples 5 to 6, comparative examples 7 to 1 to 7 to 3 and examples 1 to 2 were each observed and left at normal temperature for 12 hours, at normal temperature for 90 days, and at 40℃for 90 days, and the appearance was as shown in Table 15:
TABLE 15
From table 15, it can be seen that:
comparative example 5 with 0.05% gellan gum and 0.5% sodium chloride as suspending agent system, after 12 hours of standing, the solid particles were in suspension, but after 90 days of standing at room temperature, the particles began to settle;
comparative example 6 with 0.05% xanthan gum and 0.5% sodium chloride as suspending agent system, settling had started after 12 hours of standing;
example 1 with 0.025% gellan gum, 0.025% xanthan gum and 0.5% sodium chloride as suspending agent system was left at ambient temperature for 90 days, the solid particles remained suspended, but after 90 days at 40 ℃, the solid particles began to settle;
example 2 with 0.025% gellan gum, 0.025% xanthan gum, 0.5% sodium chloride and 0.5% gantrez as suspending agent system remained in suspension after 90 days at 40 ℃;
comparative example 7-1 with 0.025% gellan gum, 0.025% xanthan gum, 0.5% potassium nitrate and 0.5% gantrez as suspending agent system was left at ambient temperature for 12 hours, the solid particles had begun to settle;
comparative example 7-2 with 0.025% gellan gum, 0.025% xanthan gum, 0.5% sodium nitrate and 0.5% gantrez as suspending agent system was left at ambient temperature for 12 hours, the solid particles also started to settle;
comparative examples 7-3, which used 0.025% gellan gum, 0.025% xanthan gum, 0.5% potassium chloride and 0.5% gantrez as suspending agent systems, were left at ambient temperature for 12 hours and the solid particles also began to settle.
In summary, a suspension system comprising gellan gum, xanthan gum, and sodium chloride allows high density solid particles to remain suspended at room temperature for a long period of time; and the Gantrez is added on the basis of taking gellan gum, xanthan gum and sodium chloride as suspending agent systems, so that high-density particles can be kept in suspension for a long time under the high-temperature condition (40 ℃). However, the use of monovalent inorganic salts such as potassium nitrate, sodium nitrate, and potassium chloride in place of sodium chloride does not allow the high density solid particles to remain stably suspended in the oral care liquid composition for long periods of time.
Examples 3 to 5
Examples 3-5 were prepared as in table 16 below; the components in table 16 below are all in weight percent.
Table 16
As can be seen from table 16:
examples 3-5 all used gellan gum, xanthan gum, sodium chloride and Gantrez as suspending agents, with gellan gum added at 0.025%, xanthan gum added at 0.025%, gantrez added at 0.5%, sodium chloride added at 0.2% in example 3, sodium chloride added at 0.6% in example 4, and sodium chloride added at 0.8% in example 5.
The appearance state of each of examples 3 to 5 after being left at normal temperature for 12 hours, at normal temperature for 90 days, and at 40℃for 90 days was observed, and the results are shown in Table 17:
TABLE 17
| Example 3 | Example 4 | Example 5 | |
| For 12 hours | Suspending | Suspending | Suspending |
| Normal temperature for 90 days | Suspending | Suspending | Suspending |
| At 40 ℃ for 90 days | Suspending | Suspending | Sedimentation |
As can be seen from table 17:
when the addition amount of sodium chloride is 0.2% or 0.6%, the solid particles still remain suspended after being placed for 90 days at 40 ℃; however, when the concentration of sodium chloride was increased to 0.8%, the solid particles were left to stand at 40℃for 90 days, and instead, there was a phenomenon of sedimentation.
Example 6
Example 6 was prepared as in table 18, and example 2 is listed in table 18 for comparison purposes:
TABLE 18
As can be seen from table 18:
example 6 was formulated with 0.03% gellan gum, 0.025% xanthan gum, and 0.5% sodium chloride as suspending agent systems, with a viscosity comparable to that of example 2.
The appearance state of example 6 after being left at room temperature for 12 hours and at room temperature for 90 days and at 40 ℃ for 90 days was observed, and the results are shown in Table 19:
TABLE 19
| Example 6 | Example 2 | |
| For 12 hours | Suspending | Suspending |
| Normal temperature for 90 days | Suspending | Suspending |
| At 40 ℃ for 90 days | Sedimentation | Suspending |
As can be seen from table 19:
although the viscosities of example 6 and example 2 were comparable, the solid particles of example 6 without Gantrez added settled after 90 days of standing at 40 ℃.
Examples 7 to 8
Examples 7-8 were prepared as in table 20 below.
Table 20
As can be seen from table 20:
example 7 a suspension system of 0.01% gellan gum, 0.01% xanthan gum and 0.5% sodium chloride having a formulation viscosity of 5mpa.s; example 8 formulation viscosity was 52mpa.s with 0.1% gellan gum, 0.1% xanthan gum, and 0.5% sodium chloride as suspending agent system.
The appearance of each of examples 7 to 8 after being left at room temperature for 12 hours, at room temperature for 90 days, and at 40℃for 90 days was observed, and the results are shown in Table 21:
table 21
| Example 7 | Example 8 | |
| For 12 hours | Suspending | Suspending |
| Normal temperature for 90 days | Suspending | Suspending |
| At 40 ℃ for 90 days | Suspending | Suspending |
As can be seen from table 21: both examples 7 and 8 exhibited a suspended state of the solid particles after being left at 40℃for 90 days.
Basic formulation 2
Base formulation 2 contained the ingredients described in table 2,
table 22
Comparative example 8, examples 9 to 16
Comparative example 8 and examples 9-16 included base formulation 2, pH adjustor, 0.3% solids 5, and deionized water to 100%, wherein the solids density was 3.9g/cm 3 。
The formulation pH values for comparative example 8 and examples 9-16 are shown in table 23 below:
table 23:
the appearance of comparative example 8 and examples 9 to 16, each left at normal temperature for 12 hours, at normal temperature for 90 days, and at 40℃for 90 days was observed, and the results are shown in Table 24 below:
table 24
As can be seen from table 24:
comparative example 8 and examples 7 to 16 were left at normal temperature for 12 hours, and the solid particles were all in a suspended state; however, after 90 days of standing at normal temperature, the solid particles in the formulation of comparative example 8 having a pH of 5.5 had settled; after 90 days of standing at 40 ℃, only the solid particles in the formulations of examples 12 to 14 were still in suspension.
That is to say: the pH in the oral care liquid composition also has some effect on the suspension stability of the solid particles using the same suspending agent system.
It is to be understood that the above examples of the present application are provided by way of illustration only and not by way of limitation of the embodiments of the present application. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. Not all embodiments are exhaustive. All obvious changes or modifications which come within the spirit of the application are desired to be protected.
Claims (16)
1. An oral care liquid composition comprising high density solid particles, comprising:
1) The high-density solid particles are used as a material,
2) The suspension agent system is used for preparing the suspension agent,
3) An orally acceptable carrier;
wherein,,
the density of the solid particles is 1.2-3.9g/cm 3 ；
The viscosity of the oral care liquid composition is less than or equal to 3000mpa.s;
the suspension system comprises xanthan gum, gellan gum and sodium chloride.
2. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the suspension system further comprises a methyl vinyl ether maleic anhydride copolymer.
3. The oral care liquid composition comprising high density solid particles according to claim 2, wherein: the weight ratio of the methyl vinyl ether maleic anhydride copolymer in the composition is 0.3-2%.
4. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the oral care liquid composition has a pH in the range of 5.9 to 9.5.
5. The oral care liquid composition comprising high density solid particles according to claim 4, wherein: the oral care liquid composition has a pH in the range of 7.4 to 8.6.
6. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the oral care liquid composition comprises a pH adjustor for adjusting the pH of the composition formulation to between 5.5 and 9.5; the pH regulator includes, but is not limited to, one or more of sodium hydroxide, hydrochloric acid, sulfuric acid, citric acid and salts thereof, lactic acid and salts thereof, phosphoric acid and salts thereof, phthalic acid and salts thereof, pyrophosphoric acid and salts thereof, triphosphoric acid and salts thereof, polyphosphoric acid and salts thereof, citric acid and salts thereof, acetic acid and salts thereof.
7. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the weight ratio of the gellan gum in the composition is 0.01-0.1%.
8. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the weight ratio of the xanthan gum in the composition is 0.01-0.1%.
9. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the weight ratio of the sodium chloride in the composition is 0.2-0.8%.
10. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the weight ratio of the sodium chloride in the composition is 0.2-0.6%.
11. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the high-density solid particles are one or more of solid pearling agent particles, solid pigment particles, solid opacifier particles and organic polymer particles.
12. The oral care liquid composition comprising high density solid particles according to claim 11, wherein: the solid pearling agent or the solid pigment is one or more of mica, silicon dioxide, carbon powder, titanium dioxide, zinc oxide and hydroxyapatite.
13. The oral care liquid composition comprising high density solid particles according to claim 11, wherein: the organic polymer is one or more of polylactic acid, corn starch, microcrystalline cellulose, hydroxyethyl methyl cellulose, polymethyl methacrylate, polyglutamic acid, sodium hyaluronate, polyacrylate, fish gelatin, gum arabic and paraffin oil.
14. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the weight ratio of the high-density solid particles in the composition is 0.05-0.5%.
15. The oral care liquid composition comprising high density solid particles according to claim 1, wherein: the oral care liquid composition is a liquid toothpaste, mouthwash or mouthwash.
16. A method of suspending high density solid particles in an oral care liquid composition, comprising: xanthan gum, gellan gum and sodium chloride were used as suspending agent systems.
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