CN113384471A - Oral care product comprising a film - Google Patents

Oral care product comprising a film Download PDF

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Publication number
CN113384471A
CN113384471A CN202110650175.7A CN202110650175A CN113384471A CN 113384471 A CN113384471 A CN 113384471A CN 202110650175 A CN202110650175 A CN 202110650175A CN 113384471 A CN113384471 A CN 113384471A
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Prior art keywords
film
oral care
care composition
corn starch
composition
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Granted
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CN202110650175.7A
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Chinese (zh)
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CN113384471B (en
Inventor
陈晓斌
高琳
林志东
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Hawley & Hazel Bvi Co ltd
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Hawley & Hazel Bvi Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/0254Platelets; Flakes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/732Starch; Amylose; Amylopectin; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)

Abstract

The present invention provides an oral care composition comprising a film comprising: 1) a film, 2) an orally acceptable carrier; wherein the film comprises hydroxypropyl methylcellulose, corn starch, a plasticizer, and a nonionic surfactant; the oral care composition has a pH of 6 to 8. According to the oral care composition provided by the invention, the film in the oral care composition is kept stable in the preparation and storage processes, and the retention rate is more than or equal to 90%; the film in the composition has a rupture rate of more than or equal to 75 percent within 15s of brushing teeth and can be rapidly ruptured to release the components needing to be delivered in the film.

Description

Oral care product comprising a film
Technical Field
The invention relates to the technical field of oral care, in particular to an oral care product containing a film.
Background
In oral care compositions, the film can deliver different ingredients such as toners, flavors, actives, and the like. For example, chinese patent CN104837476A discloses a colored film fragment for delivering toner, the film fragment comprising a polymer matrix (e.g., polyvinyl alcohol, hydroxypropyl methylcellulose), a plasticizer (e.g., propylene glycol), optionally a non-ionic surfactant (e.g., polysorbate), and a pigment. The film is stable during preparation and placement of the composition and does not dissolve for a short period of time upon application to the oral cavity or brushing, but after a period of use (e.g., 30-180 seconds), the film begins to disintegrate and release its toner, providing a color signal to the consumer of adequate brushing. Whereas when a film in an oral care composition is used to deliver an active or a flavour, it begins to disintegrate and release if it takes, for example, 30-180 seconds, for a fast-acting consumer, it has been used within 30 seconds, and therefore, when a film is used to deliver an active or flavour, it is required that the film breaks rapidly in the oral cavity to release the flavour or active rapidly, increasing its onset time in the oral cavity.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide an oral care composition comprising a film. The film in the oral care composition is kept stable in the preparation and storage processes, and the retention rate is more than or equal to 90 percent; the film in the composition has a rupture rate of more than or equal to 75 percent within 15s of brushing teeth and can be rapidly ruptured to release the components needing to be delivered in the film.
In order to solve the technical problems, the invention adopts the following technical scheme:
an oral care composition comprising a film, comprising:
1) a film;
2) an orally acceptable carrier;
wherein the film comprises hydroxypropyl methylcellulose, corn starch, a plasticizer, and a nonionic surfactant;
the oral care composition has a pH of 6 to 8.
In certain preferred embodiments, the plasticizer is propylene glycol.
In certain preferred embodiments, the nonionic surfactant is a polysorbate.
In certain preferred embodiments, the film is present in the composition in an amount of 0.1 to 0.5% by weight.
In certain preferred embodiments, the film is in regular or irregular fragments of a five-pointed star, a diamond, a square, a circle, a crescent, a heart, a smiley face, a flower, a sea star, a pine, a leaf, a ghost, a butterfly, a bow tie, a bar, a ligament, a candy, a lip, and the like.
In certain preferred embodiments, the hydroxypropyl methylcellulose is present in the film in an amount of from 40 to 65% by weight.
In certain preferred embodiments, the hydroxypropyl methylcellulose is 45-60% by weight of the film.
In certain preferred embodiments, the corn starch is present in the film in an amount of 10 to 30% by weight.
In certain preferred embodiments, the corn starch is present in the film in an amount of 15 to 25% by weight.
In certain preferred embodiments, the oral care composition has a pH of 6.5 to 7.5.
In certain preferred embodiments, the film further comprises one or a combination of more than one of a toner, a fragrance, or an active.
In certain preferred embodiments, the film has an average thickness of 1.1 to 2.3 mils.
In certain preferred embodiments, the oral care product is a toothpaste.
The starting materials of the present invention are commercially available, unless otherwise specified, and the equipment used in the present invention may be any equipment conventionally used in the art or may be any equipment known in the art.
The invention has the advantages of
Compared with the prior art, the oral care composition containing the film has the advantages that the film in the oral care composition is stable in the preparation and storage processes, and the retention rate is more than or equal to 90 percent; the film in the composition has a rupture rate of more than or equal to 75 percent within 15s of brushing teeth and can be rapidly ruptured to release the components needing to be delivered in the film.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
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 amount of the ingredient, and do not include solvents, fillers, or other materials found in commercially available products with which the ingredient may be combined.
The term "comprising" as used herein means that other steps and ingredients which do not affect the end result can be added.
The term "preferably" and its variants herein refer to embodiments of the invention that are capable of providing specific benefits under specific circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the detailed description of one or more preferred embodiments does not indicate that other embodiments are not useful, and is not intended to exclude other embodiments from the scope of the invention.
The method is carried out according to conventional conditions or conditions recommended by manufacturers if specific conditions are not indicated in the examples of the invention; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
As one aspect of the present invention, an oral care composition comprising a film, comprises:
1) a film.
2) An orally acceptable carrier;
wherein the film comprises hydroxypropyl methylcellulose, corn starch, a plasticizer, and a nonionic surfactant.
The oral care composition has a pH of 6 to 8.
In certain embodiments of the invention, the film is present in the composition at a weight percent of 0.1 to 3%, such as, but not limited to, 0.1 to 2.8%, 0.1 to 2.6%, 0.1 to 2.5%, 0.1 to 2.2%, 0.1 to 2.0%, 0.1 to 1.8%, 0.1 to 1.5%, 0.1 to 1.2%, 0.1 to 1.0%, 0.1 to 0.8%, 0.1 to 0.5%, 0.1 to 0.45%, 0.1 to 0.4%, 0.1 to 0.35%, 0.1 to 0.3%, 0.1 to 0.25%, 0.1 to 0.2%, 0.1 to 0.15%, 0.2 to 2.8%, 0.2 to 2.6%, 0.2 to 2.5%, 0.2 to 2.2%, 0.2 to 2.0%, 0.8%, 0.1 to 1.2.5%, 0.1 to 2.5%, 0.0.45%, 0.1 to 2%, 0.4%, 0.2-0.35%, 0.2-0.3%, 0.2-0.25%, 0.2-0.2%, 0.2-0.25%, 0.25-2.8%, 0.25-2.6%, 0.25-2.5%, 0.25-2.2%, 0.25-2.0%, 0.25-1.8%, 0.25-1.5%, 0.25-1.2%, 0.25-1.0%, 0.25-0.8%, 0.25-0.5%, 0.25-0.45%, 0.25-0.4%, 0.25-0.35%, 0.25-0.3%, 0.3-2.8%, 0.3-2.6%, 0.3-2.5%, 0.3-2.2%, 0.3-2.0%, 0.3-1.8%, 0.3-1.5%, 0.3-2.0.0%, 0.3-1.8%, 0.3-1.5%, 0.3-0.5%, 0.3-0.45%.
In some preferred embodiments, the shape of the film is regular or irregular fragments such as five-pointed star, diamond, square, circle, crescent, heart, smile, flower, sea star, pine, leaf, ghost, butterfly, bow, strip, ligament, candy, lip, etc.
In certain embodiments of the invention, the hydroxypropyl methylcellulose is present in the film in an amount of 40-65% by weight, such as, but not limited to, 42-65%, 44-65%, 45-65%, 48-65%, 50-65%, 52-65%, 55-65%, 58-65%, 60-65%, 62-65%, 42-60%, 44-60%, 45-60%, 48-60%, 50-60%, 52-60%, 55-60%, 58-60%, 42-58%, 44-58%, 45-58%, 48-58%, 50-58%, 52-58%, 55-58%, 42-55%, 44-55%, 45-55%, 48-55%, 50-55%, 52-55%, 42-58%, 44-58%, 45-58%, 48-58%, 50-58%, 52-58%, 55-58%, 42-50%, 44-50%, 45-50%, 48-50%.
In certain embodiments of the invention, the corn starch is present in the film in an amount of 10-30% by weight, such as, but not limited to, 10-25%, 12-25%, 13-25%, 15-25%, 16-25%, 18-25%, 20-25%, 22-25%, 10-24%, 12-24%, 13-24%, 15-24%, 16-24%, 18-24%, 20-24%, 22-24%, 10-22%, 12-22%, 13-22%, 15-22%, 16-22%, 18-22%, 20-22%, 10-20%, 12-20%, 13-20%, 15-20%, 16-20%, 18-20%, 10-18%, 12-18%, 13-18%, 15-18%, 16-18%, 10-16%, 12-16%, 13-16%, 15-16%.
In certain embodiments of the invention, the corn starch is a modified corn starch.
In certain embodiments of the present invention, the film further comprises one or a combination of more than one of a toner, a fragrance, or an active.
In certain embodiments of the present invention, the flavor comprises menthol.
In certain embodiments of the invention, the film has an average thickness of 1.1 to 2.3 mils, such as, but not limited to, 1.1 to 2.2, 1.1 to 2.1, 1.1 to 2.0, 1.1 to 1.9, 1.1 to 1.8, 1.1 to 1.7, 1.1 to 1.6, 1.1 to 1.5, 1.1 to 1.4, 1.1 to 1.3, 1.1 to 1.2, 1.2 to 2.2, 1.2 to 2.1, 1.2 to 2.0, 1.2 to 1.9, 1.2 to 1.8, 1.2 to 1.7, 1.2 to 1.6, 1.2 to 1.5, 1.2 to 1.4, 1.2 to 1.3, 1.3 to 2.2, 1.3 to 2.1, 1.3 to 2.0, 1.3 to 1.1.1.1.1, 1.1.1.4, 1.3 to 1.1.4, 1.3 to 1.4, 1.3, 1.4, 1.3 to 1.4, 1.3, 1.4, 1.3, 1.4, 1.8, 1.4-1.5,1.5-2.2,1.5-2.1,1.5-2.0,1.5-1.9,1.5-1.8,1.5-1.7,1.5-1.6,1.6-2.2,1.6-2.1,1.6-2.0,1.6-1.9,1.6-1.8,1.6-1.7,1.7-2.2,1.7-2.1,1.7-2.0,1.7-1.9,1.7-1.8,1.8-2.2,1.8-2.1,1.8-2.0,1.8-1.9,1.9-2.2,1.9-2.1,1.9-2.0,2.0-2.1.
In certain embodiments of the invention, the oral care composition has a pH of 6 to 8, such as, but not limited to, 6.1 to 7.9, 6.2 to 7.8, 6.3 to 7.7, 6.4 to 7.6, 6.5 to 7.5, 6.6 to 7.4, 6.7 to 7.3, 6.8 to 7.2, 6.9 to 7.1, 6.6 to 7.5, 6.7 to 7.5, 6.8 to 7.5, 6.9 to 7.5, 7 to 7.5, 7.1 to 7.5, 7.2 to 7.5, 7.3 to 7.5, 7.4 to 7.5, 6.6 to 7.4, 6.7 to 7.4, 6.8 to 7.4, 6.9 to 7.4, 7 to 7.4, 7.1 to 7.4, 7.2 to 7.4, 7.6 to 7.7, 6.7 to 7.4, 6.7 to 7.7.4, 6.7.7 to 7.7, 6.7.7 to 7.4, 6.7.7, 6.7 to 7.3.3, 6.7.7 to 7.3.3, 6 to 7.7.5, 6.7.7, 6.1 to 7.5, 6.7.7.7.7.4, 6.7.7.7.7.7, 6.7.7.7.3 to 7.7, 6.7.7.7.7.3.3.7, 6.7.7.7.3 to 7, 6.7.3 to 7, 6 to 7.7.3.3.3.7, 6.3.3.3.3.3 to 7.7.3.5, 7-7.2,7.1-7.2,6.6-7.1,6.7-7.1,6.8-7.1,6.9-7.1,7-7.1,6.6-7.0,6.7-7,6.8-7,6.9-7,6.6-6.9,6.7-6.9,6.8-6.9,6.6-6.8,6.7-6.8.
In certain embodiments of the present invention, the oral care composition pH is measured by the following method:
weighing 10g of toothpaste, accurately weighing to 0.01g, placing in a 50ml beaker, adding 40ml of pure water, stirring well, measuring with a pH meter at room temperature, and reading the pH value within 10 Min.
In certain embodiments of the invention, the plasticizer is one or a combination of more than one of propylene glycol, glycerin, and triacetin.
In certain embodiments of the invention, the plasticizer is present in the film at 1-20% by weight, such as, but not limited to, 2-20%, 5-20%, 8-20%, 10-20%, 12-20%, 15-20%, 18-20%, 2-18%, 5-18%, 8-18%, 10-18%, 12-18%, 15-18%, 2-15%, 5-15%, 8-15%, 10-15%, 12-15%, 2-13%, 5-13%, 8-13%, 10-13%, 12-13%, 2-12%, 5-12%, 8-12%, 10-12%, 2-10%, 5-10%, 8-10%.
In certain embodiments of the invention, the nonionic surfactant is a polysorbate, for example, polysorbate 80 (trade name: polysorbate 80)
Figure BDA0003110879970000051
80, commercially available).
In certain embodiments of the invention, the nonionic surfactant is present in the film in an amount of 1 to 20% by weight, such as but not limited to 2-20%, 5-20%, 8-20%, 10-20%, 12-20%, 15-20%, 18-20%, 2-18%, 5-18%, 8-18%, 10-18%, 12-18%, 15-18%, 2-15%, 5-15%, 8-15%, 10-15%, 12-15%, 2-13%, 5-13%, 8-13%, 10-13%, 12-13%, 2-12%, 5-12%, 8-12%, 10-12%, 2-10%, 5-10%, 8-10%.
Other orally acceptable carriers
In certain embodiments of the present invention, the oral care composition comprises a liquid toothpaste, a mouthwash.
In the present invention, the "orally acceptable carrier" refers to any vehicle suitable for formulating the oral care compositions disclosed herein. The orally acceptable carrier is not harmful to the 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 surface as required by the present invention. In general, an orally acceptable carrier is not harmful if not intentionally swallowed. Suitable orally acceptable carriers include, for example, one or more of the following: water, thickeners, pH adjusters, humectants, sweeteners, flavorants, visual aids (e.g., colors, dyes, or mixtures thereof), anti-caries agents, antibacterial agents, whitening agents, desensitizing agents, vitamins, preservatives, enzymes, mixtures thereof, and the like.
In certain preferred embodiments of the present invention, adjuvants such as humectants and/or thickeners are included in the oral care composition.
"humectants" are ingredients that prevent the oral care composition from becoming dehydrated and hardened. Exemplary humectants include, but are not limited to, glycerin, sorbitol, and the like. The humectant is typically present in the oral care composition in an amount of 10 to 80% by mass.
"pH modifying agents" can substantially modify the pH value of an oral care product formulation. Exemplary pH adjusters include, but are 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, tripolyphosphoric acid and salts thereof, polyphosphoric acid and salts thereof, and acetic acid and salts thereof.
According to certain embodiments of the present application, active ingredients such as antibacterial agents, anticaries agents, anti-sensitivity agents, and/or whitening agents may be further included in the oral care compositions.
By "antibacterial agent" is meant a chemical substance that is capable of maintaining the growth or reproduction of certain microorganisms in an oral care composition below a necessary level over a period of time. Exemplary antimicrobial agents include, but are not limited to: tetrahydrocurcumin, cetylpyridinium chloride, triclosan, and the like.
"anticaries agent" means a substance having an inhibitory effect on caries, for example, a substance which enhances the anticaries ability of teeth by decreasing the solubility of enamel hydroxyapatite, or a substance which controls plaque, inhibiting bacterial growth. Exemplary anticaries agents include, but are not limited to, phosphorus-containing agents (calcium phosphate, magnesium glycerophosphate, calcium lactate phosphate, sodium caseinate, etc.), or arginine and its derivatives. Preferably, in certain embodiments, the anticaries agent comprises a fluoride ion source.
An "anti-sensitivity agent" refers to a substance that prevents or treats dentinal hypersensitivity by inhibiting nerve impulses or being capable of closing or decreasing the permeability of dentinal tubules. Exemplary anti-sensitivity agents include, but are not limited to: potassium ion sources such as dipotassium glycyrrhizinate, potassium fluoride, potassium nitrate, potassium chloride and the like.
The "whitening agent" refers to a substance having a whitening effect on teeth. Exemplary whitening agents include, but are not limited to: a peroxide bleaching agent.
Method for evaluating film stability
This experiment evaluates film stability by the percentage of film remaining in the composition as follows:
1. taking 10g of pentagonal film sheets with uniform size, thickness and weight, counting the number of films corresponding to the 10g of film sheets, and calculating the average number of films per gram as a theoretical value;
2. formulating an oral care composition comprising the film;
3. aging the oral care composition at 40 deg.C for 3 months;
4. taking 10g of the aged oral care composition, flattening the composition on a flat plate, and counting the number of films in the composition;
5. the above procedure was repeated 5 times and the actual number of films in an average worth of 10g of oral care composition was calculated.
6. Calculating the theoretical value of the number of the films in 10g of oral care products according to the addition amount of the films in the oral care products;
7. the leave-on rate of the film in the oral care composition after aging was calculated according to the following formula, the higher the leave-on rate, the more stable the film.
Figure BDA0003110879970000071
The evaluation method for the rapid rupture of the film comprises the following steps:
1. taking a pentagonal film with uniform size, thickness and weight;
2. preparing toothpaste containing the film;
3. taking 2g of the toothpaste, flattening the toothpaste on a flat plate, and counting the number of films in the composition;
5. repeating the operation for 5 times, and calculating the initial number of the films in each gram of toothpaste;
3. taking 2g of the composition to a toothbrush head, and simulating tooth brushing for 15s by a tooth brushing machine;
4. repeating the experiment for 10 times, and collecting the tooth brushing paste;
5. counting the number of films in the toothpaste slurry, and calculating the number of the unbroken films in each gram of the composition;
6. the film's breaking rate was calculated according to the following formula, the higher the breaking rate, the better the delivery of the ingredients in the film.
Figure BDA0003110879970000072
The term "rapidly rupture" in this application means that the film in the composition ruptures at a rate of 75% or more within 15 seconds of brushing.
# #1 to 7 thin film arrangement
Table 1 shows the thickness of 7 films of different compositions or different mass ratios of the compositions, which are all 1.5 mils.
Table 1:
Figure BDA0003110879970000073
as can be seen from table 1:
the polymer matrix of film 1 comprises 10% hydroxypropyl cellulose and 45% polyvinyl alcohol, and does not comprise corn starch;
the polymer matrix of film 2 comprises 40% hydroxypropyl methylcellulose and 15% corn starch;
the polymer matrix of film 3 comprises 65% hydroxypropyl cellulose and 15% corn starch;
the polymer matrix of film 4 comprises 45% hydroxypropyl cellulose and the content of corn starch is 30%;
the polymer matrix of film 5 comprises 45% hydroxypropyl cellulose and 15% corn starch;
the polymer matrix of film 6 comprises 45% hydroxypropyl cellulose and 25% corn starch;
the polymer matrix of film 7 comprises 60% hydroxypropyl cellulose and 15% corn starch.
Examples 1 to 3, comparative examples 1 to 4
Examples 1 to 3 and comparative examples 1 to 4 were prepared according to Table 2, and toothpaste was prepared according to a conventional preparation method.
TABLE 2
Figure BDA0003110879970000081
In Table 2, comparative examples 1 to 4 and examples 1 to 3 each contained tetrasodium pyrophosphate in an amount of 0.9% by mass and disodium dihydrogen pyrophosphate in an amount of 0.6% as a buffer system, and the formulation pH was 7.
Film stability investigation
Comparative examples 1 to 4 and examples 1 to 3 were aged at 40 ℃ for 3 months, and the retention rate was calculated to examine the stability.
TABLE 3
Comparative example1 Comparative example 2 Comparative example 3 Comparative example 4 Example 1 Example 2 Example 3
Retention rate 93.6% 61.5% 47.6% 66.7% 97.6% 94.2% 90.9%
As can be seen from table 3:
the compositions of comparative examples 1-4 and examples 1-3 each had 0.3% film added thereto, wherein,
the film added to the formulation of comparative example 1, which had hydroxypropyl methylcellulose and polyvinyl alcohol as the polymer matrix, had a retention of up to 93.6% after 3 months of aging at 40 ℃.
While the films formulated in comparative examples 2-4 and examples 1-3 all used hydroxypropyl methylcellulose and corn starch as the polymer matrix, wherein,
comparative example 2 the mass ratio of hydroxypropyl methylcellulose added to the film in the formulation was 40% and the mass ratio of corn starch in the film was 15%, at which time the retention of the film in the formulation was 61.5%.
Comparative example 3 the mass ratio of hydroxypropyl methylcellulose added to the film in the formulation was 65% and the mass ratio of corn starch in the film was 15%, at which time the retention of the film in the formulation was 47.6%.
Comparative example 4 the mass ratio of hydroxypropyl methylcellulose added to the film in the formulation was 45% and the mass ratio of corn starch in the film was 30%, at which time the retention of the film in the formulation was 66.7%.
In the formula of example 1, the mass ratio of hydroxypropyl methyl cellulose added into the film in the film is 45%, the mass ratio of corn starch in the film is 15%, and the retention rate of the film in the formula is as high as 97.6%.
In example 2, the mass ratio of hydroxypropyl methylcellulose added to the film in the formula is 45% in the film, the mass ratio of corn starch in the film is 25%, and the retention rate of the film in the formula is 94.2%.
In example 3, the mass ratio of hydroxypropyl methylcellulose added to the film in the formula is 60% in the film, the mass ratio of corn starch in the film is 15%, and the retention rate of the film in the formula is 90.9%.
Film rupture Rate investigation
2g of each of comparative examples 1 to 4 and examples 1 to 3 was taken, and the film breakage rate in each formulation was examined by simulating brushing for 15 seconds with a tooth brushing machine.
TABLE 4
Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Example 1 Example 2 Example 3
Rate of rupture 10.7% 70.3% 75.8% 73.4% 79.50% 81.2% 80.9%
As can be seen from Table 4, the film broke rate was only 10.7% for comparative example 1, and comparable for comparative examples 2-4 and examples 1-3 formulations, after the brusher simulated brushing for 15 seconds.
Combining tables 3 and 4, it can be seen that: in comparative examples 1 to 4 and examples 1 to 3, only examples 1 to 3 satisfied the characteristics that the film was stable during preparation and storage, the leave-on rate was not less than 90%, and the film breakage rate was not less than 75% at 15s of brushing; namely, when the film in the composition takes hydroxypropyl methylcellulose and corn starch as polymer matrixes, the breakage rate of the film is remarkably improved compared with that of the film taking hydroxypropyl methylcellulose and polyethylene glycol as matrixes, the mass percentage of the hydroxypropyl methylcellulose in the film is 45-60%, and when the mass percentage of the corn starch in the film is 15-25%, the breakage rate of the film is not less than 75%, the film is stable in the preparation and storage processes, and the retention rate is not less than 90%.
Examples 4 to 7, comparative examples 5 to 6
Examples 4 to 7 and comparative examples 5 to 6 were prepared according to Table 5, and toothpaste was prepared according to a conventional preparation method. For ease of comparison, example 1 is listed in table 5:
table 5:
Figure BDA0003110879970000101
as can be seen from table 5:
comparative example 5 a formulation pH of 5.5 was used with 0.18 mass percent tetrasodium pyrophosphate and 1% disodium dihydrogen pyrophosphate as the buffer system.
Comparative example 6 was prepared with 0.68 mass percent tetrasodium pyrophosphate and 0.18 mass percent disodium dihydrogen pyrophosphate as buffer system, and a formulation pH of 8.5.
Example 4 the formulation pH was 6 using 0.9 mass percent tetrasodium pyrophosphate and 2.5 mass percent disodium dihydrogen pyrophosphate as buffer systems.
Example 5 the formulation pH was 8 using 2.35% by mass tetrasodium pyrophosphate and 0.6% disodium dihydrogen pyrophosphate as buffer systems.
Example 1 the formulation pH was 7 using 0.9 mass% tetrasodium pyrophosphate and 0.6 mass% disodium dihydrogen pyrophosphate as buffer systems.
Example 6 the formulation pH was 6.5 using 0.9 mass% tetrasodium pyrophosphate and 1.2 mass% disodium dihydrogen pyrophosphate as buffer systems.
Example 7 the formulation pH was 7.5 using 1.36 mass percent tetrasodium pyrophosphate and 0.6 mass percent disodium dihydrogen pyrophosphate as buffer systems.
Film stability investigation
The retention rate was calculated for examples 4-7 and comparative examples 5-6 after aging at 40 ℃ for 3 months, and the stability was examined, the results are shown in Table 6 below.
TABLE 6
Comparative example 5 Comparative example 6 Example 4 Example 5 Example 1 Example 6 Example 7
Retention rate 59.3% 52.9% 70.5% 65.9% 97.6% 97.9% 94.5%
As can be seen from table 6:
comparative example 5 the retention of the film in the formulation was 59.3%;
the retention of the film in the formulation of comparative example 6 was 52.9%;
the retention rate of the film in the formula of example 4 is improved to 70.5 percent;
the retention rate of the film in the formula of example 5 is improved to 65.9 percent;
the leave-on rate of the film in the formulation of example 1 was 97.6%;
the film retention in the formulation of example 6 was 97.9%;
the film retention in the formulation of example 7 was 94.5%.
Namely, when the pH value of the formula is 5.5, the retention rate of the film is only 59.3%; when the pH value of the formula is 6, the retention rate of the film is improved to 70.5 percent; when the pH value of the formula is increased to 6.5, the retention rate of the film is remarkably improved to 97.9%, and when the pH value is further increased to 7.0, the retention rate of the film is kept at 97.9%; when the pH value is increased to 7.5%, the retention rate of the film is 94.5%, and when the pH value of the formula is increased to 8.0, the retention rate of the film is obviously reduced to only 65.9%; when the pH value of the formula is further increased to 8.5, the retention rate of the film is further reduced to only 52.9%.
Film rupture Rate investigation
The results of examining the film breakage rate in each formulation by simulating brushing for 15s with a toothbrushing machine using 2g each of examples 4 to 5 and comparative examples 5 to 6 are shown in Table 7 below.
TABLE 7
Comparative example 5 Comparative example 6 Example 4 Example 5 Example 1 Example 6 Example 7
Rate of rupture 82.5% 78.7% 80.5% 78.5% 79.50% 81.5% 82.3%
The film failure rates were comparable for the formulations of comparative examples 5-6 and examples 4-7.
# #8-11 thin film arrangement
TABLE 8 is 8#-11#Films, film 5 is listed in table 8 for comparison.
Table 8:
Figure BDA0003110879970000121
as can be seen from table 8: 5#Film and 8-11#The films are of the same composition, but of different thickness, wherein,
5#the thickness of the film was 1.5 mils,
8#the thickness of the film was 0.9 mils,
9#the thickness of the film was 1.1 mils,
10#the thickness of the film was 2.3 mils,
11#the thickness of the film was 2.5 mils.
Examples 8 to 9, comparative examples 7 to 8
Examples 8-9, comparative examples 7-8 were configured according to table 9 below, and example 1 is listed below in table 9 for ease of comparison.
TABLE 9
Figure BDA0003110879970000131
Examples 5 to 9 and comparative examples 7 to 5 all used 0.9 mass percent tetrasodium pyrophosphate and 0.6 mass percent disodium dihydrogen pyrophosphate as buffer systems, and the formulation pH was 7.
Film stability investigation
The examples 5 to 9 and the comparative examples 7 to 5 were aged at 40 ℃ for 3 months, the retention rate was calculated, and the stability was examined, and the results are shown in Table 10 below.
Watch 10
Comparative example 7 Comparative example 5 Example 1 Example 5 Example 9
Retention rate 65.3% 75.6% 97.6% 96.4% 97.5%
As can be seen from table 10:
when the thickness of the film in the formulation was 0.9 mils (comparative example 7), the retention was 65.3%, respectively;
when the thickness of the film in the formulation was 2.5 mils (comparative example 5), the retention rates were 75.6%, respectively;
when the film thickness in the formula is 1.5 (example 1), 1.1 (example 5) and 2.3 (example 9) mil, the retention rate of the film is respectively improved to 97.6%, 96.4% and 97.5%, and is remarkably increased compared with the film thickness of 2.5 mil and 0.9 mil.
Film rupture Rate investigation
The results of examining the film breakage rate in each formulation by simulating brushing for 15s with a toothbrushing machine using 2g each of examples 5 to 9 and comparative examples 7 to 5 are shown in Table 11 below.
TABLE 11
Comparative example 7 Comparative example 5 Example 1 Example 5 Example 9
Rate of rupture 65.3% 62.1% 79.50% 75.2% 75.3%
As can be seen from table 11:
comparative example 7 the film thickness in the formulation was 0.9 mils, at which time the film broke 65.3% for 15 seconds with the brusher,
when the film thickness in the formulation is increased to 1.1 mil, i.e., the formulation of example 5 is brushed for 15s using a brushing machine, the film breakage rate is increased to 75.2%,
when the film thickness in the formulation was 1.5 mil, i.e., the formulation of example 1 was brushed for 15 seconds using a toothbrushing machine, the film breakage rate was 79.5%,
when the film thickness in the formulation was 2.3 mils, i.e., the formulation of example 9 was brushed for 15 seconds using a toothbrushing machine, the film breakage rate was 75.3%,
however, when the film thickness in the formulation was further increased to 2.3 mils, i.e., the comparative formulation was brushed for 15 seconds using a toothbrushing machine, the film breakage rate did not increase or remain, but rather decreased significantly, only 62.1%.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.

Claims (13)

1. An oral care composition comprising a film, comprising:
1) a film;
2) an orally acceptable carrier;
wherein the film comprises hydroxypropyl methylcellulose, corn starch, a plasticizer, and a nonionic surfactant;
the oral care composition has a pH of 6 to 8.
2. The oral care composition of claim 1, wherein: the plasticizer is propylene glycol.
3. The oral care composition of claim 1, wherein: the nonionic surfactant is polysorbate.
4. The oral care composition of claim 1, wherein: the mass percentage of the film in the composition is 0.1-0.5%.
5. The oral care composition of claim 1, wherein: the film is in the shape of five-pointed star, diamond, square, circle, crescent, heart, flower, sea star, pine, tree leaf, ghost, butterfly, bow, strip, ligament, candy, lip or smile face.
6. The oral care composition of claim 1, wherein: the mass percentage of the hydroxypropyl methyl cellulose in the film is 40-65%.
7. The oral care composition of claim 6, wherein: the mass percentage of the hydroxypropyl methyl cellulose in the film is 45-60%.
8. The oral care composition of claim 1, wherein: the mass percentage of the corn starch in the film is 10-30%.
9. The oral care composition of claim 8, wherein: the mass percentage of the corn starch in the film is 15-25%.
10. The oral care composition of claim 1, wherein: the method is characterized in that: the oral care composition has a pH of 6.5 to 7.5.
11. The oral care composition of claim 1, wherein: the film further comprises one or a combination of more than one of a toner, a fragrance, or an active.
12. The oral care composition of claim 1, wherein: the film has an average thickness of 1.1 to 2.3 mils.
13. The oral care composition of claim 1, wherein: the oral care product is a toothpaste.
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CN102958567A (en) * 2010-06-30 2013-03-06 高露洁-棕榄公司 Multilayer films for delivery of flavor
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CN101677935A (en) * 2007-04-18 2010-03-24 高露洁-棕榄公司 films comprising a plurality of polymers
US20120121669A1 (en) * 2008-08-11 2012-05-17 Colgate-Palmolive Company Oral care composition comprising capsules
CN102958567A (en) * 2010-06-30 2013-03-06 高露洁-棕榄公司 Multilayer films for delivery of flavor
CN102920683A (en) * 2012-06-11 2013-02-13 江苏豪森药业股份有限公司 Olanzapine oral instant membrane
CN104837476A (en) * 2012-12-14 2015-08-12 高露洁-棕榄公司 Abradable films for use in oral care
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