CN110585062B - Hyaluronic acid oral care composition and preparation method and application thereof - Google Patents
Hyaluronic acid oral care composition and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
Abstract
A hyaluronic acid oral care composition, a preparation method and an application thereof, wherein the composition comprises the following components: 30-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, 35-45% of hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and 20-30% of hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa. The oral care composition is prepared from pure hyaluronic acid or salt thereof, is not added with other functional components, fully excavates and utilizes various nursing effects of HA with different molecular weight segments on oral cavity and oral cavity cells, HAs obvious effects of moisturizing the oral cavity, resisting inflammation of gingival cells, repairing damaged oral cavity cells and the like, can comprehensively care the oral health, and provides more basis for expanding the application field of hyaluronic acid and developing other oral care products.
Description
Technical Field
The invention relates to a hyaluronic acid oral care composition for oral care, a preparation method of the composition and application of the composition in oral care products.
Background
Hyaluronic Acid (HA) is an acidic mucopolysaccharide, an unbranched macromolecular glycosaminoglycan composed of repeating units of N-acetylglucosamine and D-glucuronosyl, present in the stroma of animal tissues and in the capsule of certain bacteria. Hyaluronic acid is widely used in the fields of medicine, cosmetics, food and the like, and has a molecular weight of generally 10 5 ～10 7 Da (Dalton). Hyaluronic acid has various physiological functions such as anti-inflammation and anti-inflammation besides the functions of retaining water and lubricating and regulating osmotic pressureInfection, edema resistance, tissue reconstruction promotion, and wound healing. With the intensive research and the accumulation of clinical experience, HA HAs many new application fields, wherein the application of HA in the oral cavity field HAs been gradually noticed.
A plurality of studies at home and abroad show that HA HAs the functions of resisting inflammation and infection, and promoting the repair and reconstruction of periodontal tissues and the healing of wounds. The high-concentration medium-molecular-weight HA (757kDa) HAs better inhibiting effect on actinobacillus actinomycetemcomitans, prevotella intermedia, staphylococcus aureus and propionibacterium acnes, and the 1.0mg/ml high-molecular-weight hyaluronic acid HAs better inhibiting effect on the six bacteria. HA (Mr) of high relative molecular mass>10 6 Da) can inhibit proliferation of gingival epithelial cell fibroblast and lymphocyte, shorten inflammation process of periodontitis, and improve lesion status (SUNSHUNYANG, etc., hyaluronic acid and its application in stomatology field, journal of stomatology, 2013, 6(1), 56-59). Currently, only HA with medium and high molecular weight HAs been reported to have inhibitory effect on oral inflammation or pathogenic bacteria, HA with other molecular weight HAs not been reported, and detailed research on specific effect of HA with different molecular weight on oral cells is lacked.
There are also a number of oral care products containing hyaluronic acid in the prior art, as follows: CN 106176690A discloses an oral care film containing hyaluronic acid, which is obtained by adding two molecular weight hyaluronate, zinc hyaluronate and other auxiliary materials, drying and forming a film; CN 103405470 a discloses a hyaluronic acid composition in a solution dosage form for treating and relieving xerostomia; CN 105056219 a discloses an artificial saliva containing 0.5mg/ml hyaluronic acid; CN 103462847 a discloses a gargle for oral care. Firstly, the products in the prior art are all finished products of liquid dosage forms and film agents, belong to terminal products, cannot be added into other oral care products, and have narrow application range; secondly, the product mainly aims at the problem of xerostomia, the moisturizing effect of hyaluronic acid is mainly applied, other effects of hyaluronic acid are not fully developed, and other ingredients or auxiliary materials which are not hyaluronic acid and have oral care effects (such as bacteriostasis, repair promotion and the like) are still required to be added into the product to meet the care requirements of other oral problems.
At present, an oral care composition which comprehensively cares the oral cavity, has wide application and convenient use, takes hyaluronic acid as a main body or simply contains hyaluronic acid is urgently needed to fully develop and expand the performance and the application range of the hyaluronic acid and provide a basis for the further development of the hyaluronic acid industry.
Disclosure of Invention
In order to solve the problem that the performance of hyaluronic acid in oral care products is not sufficiently exerted at present, the invention provides the hyaluronic acid oral care composition, which takes hyaluronic acid or salt thereof with different molecular weights as components, can be used for oral moisture preservation through the synergistic collocation of the hyaluronic acid or the salt, can also be used for resisting inflammation and repairing oral problems such as oral inflammation, ulcer and the like, has various effects, meets different requirements, and is convenient to use.
Aiming at the defect that the performance of hyaluronic acid in oral care is not fully researched at present, the inventor carries out detailed research on the safety and the action efficacy of hyaluronic acid or salt thereof with different molecular weights on oral cells. The method specifically comprises the following steps: the inhibition effect and cytotoxicity of HA (2-5 kDa, 30-50 kDa, 200-600 kDa, 1300-1500 kDa and 2000-3000 kDa) with five molecular weight segments on the release of inflammatory factors (IL-6 and IL-1 beta) are examined by taking human gingival cells (HGF-1) as model cells, and the results show that: in the concentration range of 0.05-0.5% (w/v), HA with different molecular weight HAs no obvious cytotoxicity to HGF-1 of gingival fibroblast. Along with the reduction of the molecular weight, the inhibition rate of the compound on IL-6 and IL-1 beta is higher, especially HA (2-5 kDa), and the inhibition rate on two proinflammatory factors is more than 50%; while the high molecular HA (1300-1500 kDa and 2000-3000 kDa) HAs almost no inhibitory effect on inflammatory factors. In addition, the cell scratching method is used for investigating the effect of the HA with the five molecular weight sections on repairing the gingival wound cells, and the result shows that the hydrolyzed HA (2-5 kDa), the low molecular HA (200-600 kDa) and the high molecular HA (1300-1500 kDa) have obvious effects on promoting healing of a scratched area of the gingival cells under the same concentration condition, wherein the low molecular HA (200-600 kDa) HAs the best effect, and the low molecular HA (30-50 kDa) and the high molecular HA (2000-3000 kDa) have poor effects. It can be seen that the efficacy of HA of different molecular weights on oral cells is slightly different from the function of HA of different molecular weights reported in the literature.
With the support of the research results, according to the effects of the HA with each molecular weight section on oral cells, the inventor selects the HA with good effects and moisturizing, anti-inflammatory and repairing effects, and combines the HA with different molecular weight sections in specific content to obtain the oral care composition consisting of the pure hyaluronic acid or the salt thereof.
Furthermore, the invention selects hydrolyzed hyaluronic acid or salt thereof with molecular weight of 2-5 kDa, hyaluronic acid or salt thereof with molecular weight of 200-600 kDa and hyaluronic acid or salt thereof with molecular weight of 1300-1500 kDa as effective components, and the weight percentage of each component is as follows: 30-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, 35-45% of hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and 20-30% of hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa.
Preferably, the hyaluronic acid oral care composition comprises the following components in percentage by weight: 35-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, 38-43% of hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and 22-27% of hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa.
More preferably, the hyaluronic acid oral care composition of the invention comprises the following components in percentage by weight: 35-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-3 kDa, 38-43% of hyaluronic acid or salt thereof with the molecular weight of 400-500 kDa and 22-27% of hyaluronic acid or salt thereof with the molecular weight of 1300-1400 kDa.
Further, in the hyaluronic acid oral care composition, the hydrolyzed hyaluronic acid or salt thereof is oligomeric hyaluronic acid or salt thereof, and is obtained by digesting oligomeric hyaluronic acid or salt thereof with bacillus hyaluronidase obtained by fermentation culture of bacillus a50CGMCC No.5744, and the hydrolyzed hyaluronic acid or salt thereof can be obtained by the method disclosed in patent nos. CN 102876748A and CN 108220364 a. The enzyme-digested oligomeric hyaluronic acid or salt thereof obtained by using the bacillus hyaluronidase has a complete structure, and has the advantages of good transdermal absorbability, high purity, no cytotoxicity, strong oxidation resistance and the like compared with other oligomeric hyaluronic acids. In addition, the enzyme-cleaved oligomeric hyaluronic acid has the activity of removing free radicals, repairing after-sun cells, protecting against sunlight, promoting angiogenesis and the like, which is the characteristic that general hyaluronic acid does not have.
Furthermore, the hyaluronic acid salt or the hydrolyzed hyaluronic acid salt is sodium salt, potassium salt, magnesium salt, calcium salt or zinc salt of hyaluronic acid or hydrolyzed hyaluronic acid.
Furthermore, the invention also provides a preparation method of the hyaluronic acid oral care composition, which is simple to operate, and the hyaluronic acid oral care composition can be obtained by respectively crushing and sieving hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa, and then uniformly mixing the crushed materials.
Furthermore, in the preparation method, the aperture of the screen mesh used when the components are crushed and sieved is kept consistent, so that the three powders can be fully and uniformly mixed, and the obtained hyaluronic acid oral care composition can achieve the best effect.
Furthermore, the hyaluronic acid oral care composition has the effects of moisturizing the oral cavity, resisting inflammation of the gums, repairing damaged oral cells and the like, can keep the oral cavity moist, can resist inflammation of the gums and repair the injured gingival cells, has single component and no cytotoxicity, and is urgently needed for comprehensively caring the oral health. The product of the present invention can be used as an effective ingredient in various oral care products, and therefore, the application of the hyaluronic acid oral care composition of the present invention in the oral care products is also within the protection scope of the present invention.
Further, the oral care product may be various types of oral care products such as mouthwashes, toothpastes, mouth repair gels, mouth sprays, mouth fresheners, mouth ulcer strips, and the like.
Through comprehensive oral efficacy experiments, the formula of the hyaluronic acid oral care composition with remarkable effects of moisturizing the oral cavity, resisting inflammation of gums, repairing damaged oral cells and the like is finally determined. For oral health, there is an urgent need for an oral care composition which can maintain the oral cavity moist, resist gingival inflammation, repair wounded gingival cells, has no cytotoxicity, has a single component, and can comprehensively care the oral health.
The invention has the following beneficial effects:
1) the hyaluronic acid oral care composition combines hyaluronic acid or salts thereof with different molecular weights, has good safety and no cytotoxicity, has remarkable functions of moisturizing the oral cavity, resisting inflammation of gingival cells, repairing damaged oral cells and the like, and can comprehensively care the oral health.
2) The hyaluronic acid oral care composition disclosed by the invention is prepared from pure hyaluronic acid or salt thereof, is not added with other functional components, fully excavates and utilizes various care effects of HA with different molecular weight segments on oral cavities and oral cavity cells, finally determines the optimal proportion of the composition with comprehensive oral care effects through a plurality of oral care efficacy tests, and provides more bases for expanding the application field of hyaluronic acid and developing other oral care products.
3) The hyaluronic acid oral care composition is white powder in shape, is in a solid state, has the advantages of convenience in storage and transportation, is compatible with a formula system of various oral articles (such as mouthwash, toothpaste, oral repair gel, oral spray, an oral freshener, an oral ulcer patch and the like), is easy to add and is convenient to use.
Detailed Description
The present invention is described in further detail below with reference to specific examples, but it should be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
In the following examples, unless otherwise specified, the percentages are by mass.
Test example 1: effect of HA of different molecular weights on HGF-1 cell proliferation
1. Experimental Material
Hydrolyzed sodium hyaluronate (molecular weight 2-5 kDa), sodium hyaluronate 30-50 kDa, sodium hyaluronate 200-600 kDa, sodium hyaluronate 1200-1500 kDa and sodium hyaluronate 2000-3000 kDa, all from Huaxi Biotechnology Ltd.
2. The experimental method comprises the following steps:
recovering, culturing 3-4 generations of HGF-1 cells, digesting the cells with pancreatin when reaching 60% -80% fusion, adjusting cell density to 2 × 10 4 One cell/mL, inoculated into 96-well cell culture plate, each well of 100 u L cell suspension, placed in carbon dioxide incubator at 37 deg.C, 5% CO 2 The culture was routinely carried out overnight. Preparing HA solutions with different molecular weights of 0.5%, 0.2%, 0.1% and 0.05% (w/v) by using serum-free DMEM high-glucose culture solution, filtering and sterilizing by using a 0.22 mu m filter membrane, sucking and removing the old culture solution, adding 100 mu L of the HA solution into each hole of a test group, adding the same amount of serum-free DMEM high-glucose culture solution into a negative control group, adding the same amount of cell culture solution into a blank control group without cells, and continuously culturing for 48 hours. Add 10. mu.L of WST-1 solution to each well and continue incubation in the cell incubator for 4 h. The absorbance was measured at a wavelength of 450nm with a microplate reader. The relative proliferation rate was calculated according to the following formula:
RGR＝A/A 0 ×100％
in the formula:
RGR-relative proliferation rate,%;
a-test absorbance-blank control absorbance;
A 0 -absorbance of negative control-absorbance of blank control.
3. Results of the experiment
TABLE 1 Effect of HA of different molecular weights on HGF-1 cell proliferation
Note: the molecular weight of HA-2000-3000 kDa is too high, and a sample solution prepared with the concentration of 0.5% is too viscous, so that the experiment cannot be carried out.
4. Conclusion of the experiment
As can be seen from the data in Table 1, HA with different molecular weights HAs no obvious cytotoxicity to the gingival fibroblast HGF-1 in the concentration range of 0.05-0.5% (w/v).
Test example 2: comparison of wound repair Effect of HA's of different molecular weights
1. Experimental Material
Hydrolyzed sodium hyaluronate (molecular weight 2-5 kDa), sodium hyaluronate 30-50 kDa, sodium hyaluronate 200-600 kDa, sodium hyaluronate 1200-1500 kDa and sodium hyaluronate 2000-3000 kDa, all from Huaxi Biotechnology Ltd.
2. Experimental methods
At 5X 10 5 HGF-1 cells were seeded in 24-well plates at a density of 1000. mu.L/well in 5% CO at 37 ℃ 2 Culturing for 24h under the condition, drawing a straight line on a single-layer cell in a culture hole along the vertical direction by using a 10-mu-L gun head to form a damaged area, scratching the single-layer cell, discarding all liquid in the hole, adding a sample solution (HA with different molecular weights is prepared into a solution with the concentration of 0.1% (w/v) by using a serum-free DMEM high-sugar culture solution, filtering and sterilizing the sample solution by 0.22 mu m), replacing 1000 mu-L of each hole by using a negative control group by using the serum-free DMEM high-sugar culture solution, continuously culturing for 24h, photographing and observing, analyzing the area ratio of the healed damaged area by using Image J software, and calculating the healing rate according to the following formula:
rate of healing ═ S 0 –S r )/S 0 ×100％
In the formula:
S 0 -initial scratch area, pixel;
S r -detecting the remaining scratch area, pixels, at the time point.
3. The experimental results are as follows:
TABLE 2 24-hour healing rate of scratches on cells treated with HA of different molecular weights
| Group of | 24h healing Rate (%) |
| Negative control | 43.16 |
| HA-2～5kDa | 88.34 |
| HA-30～50kDa | 74.43 |
| HA-200～600kDa | 93.67 |
| HA-1300～1500kDa | 87.23 |
| HA-2000～3000kDa | 80.66 |
4. Conclusion of the experiment
As shown in table 2, according to the calculation result (n ═ 3) of the scratch area by the software, under the same 0.1% (w/v) concentration condition, HA-2 to 5kDa, HA-200 to 600kDa and HA-1300 to 1500kDa showed significant effects on promoting healing of the scratch area, while HA-30 to 50kDa and HA-2000 to 3000kDa showed some effects on promoting healing of damaged gingival cells, but the effects were weaker than those of other molecular weight ranges. Therefore, aiming at the repair promoting effect of the damaged gingival cells, the oligomeric HA and the low molecular HA have obvious effects, and the high molecular HA (with the molecular weight of 1300-1500 kDa) also HAs the effect of promoting the repair of the damaged gingival cells.
According to the conclusion, HA with three molecular weight sections of HA-2-5 kDa, HA-200-600 kDa and HA-1300-1500 kDa which have good repairing effect on damaged gingival cells is selected as the raw material of the oral care composition.
Examples 1 to 10
Respectively crushing hydrolyzed sodium hyaluronate, sodium hyaluronate I and sodium hyaluronate II, sieving with a 60-mesh sieve, accurately weighing according to a formula, respectively putting into a double-cone rotary vacuum dryer, starting the dryer, and rotationally mixing for 1 hour. And (3) filling the uniformly mixed product into a sterilized packaging material (such as bottles, bags, aluminum plastic packages and the like) to obtain the hyaluronic acid oral care composition. The above operations are all carried out in a clean workshop.
The molecular weight and mass ratio of each sodium hyaluronate are shown in table 3 below:
TABLE 3 summary of the molecular weights and mass ratios of the raw materials used in the examples
Comparative examples 1 to 8
Respectively crushing hydrolyzed sodium hyaluronate, sodium hyaluronate I and sodium hyaluronate II, sieving with a 60-mesh sieve, accurately weighing according to a formula, respectively putting into a double-cone rotary vacuum dryer, starting the dryer, and rotationally mixing for 1 hour. And (3) filling the uniformly mixed product into a sterilized packaging material (such as bottles, bags, aluminum plastic packages and the like) to obtain the hyaluronic acid oral care composition. The above operations are all carried out in a clean workshop.
The molecular weight and mass ratio of each sodium hyaluronate are shown in table 4 below:
TABLE 4 summary of the molecular weights and mass ratios of the raw materials used in each proportion
Note: the formula of the comparative example 9 is the optimal formula of the hyaluronic acid moisturizing composition for moisturizing the skin in the patent CN106109265A, and the formula of the comparative example 10 is the optimal formula of the hyaluronic acid anti-aging composition for resisting the skin aging in the patent CN 106137786A.
Test example 3: anti-inflammatory study of hyaluronic acid oral care compositions
Anti-inflammatory experiments, human gingival fibroblast (HGF-1) is taken as a model cell, inflammatory factors are secreted by the model cell through LPS stimulation, different hyaluronic acid oral care composition samples are used for processing, and the inhibition effect of the different hyaluronic acid oral care composition samples on the release of the inflammatory factors is investigated through quantitatively detecting the expression of the inflammatory factors in culture supernatants.
1. Experimental methods
Preparation of sample solution: the products of examples 1-10 and comparative examples 1-10 were prepared in a 0.2 wt% concentration DMEM medium without serum, containing 10000IU of LPS, and sterilized by 0.22 μm filtration.
The cells were cultured at 5X 10 5 Perml inoculated in 24-well plates at 37 ℃ with 5% CO 2 Culturing for 24h under the condition, adding 1000 μ L of each sample solution, replacing the negative control group with a culture solution containing no LPS and no HA, replacing the model group with a culture solution containing LPS and no HA, continuously culturing for 24h, quantitatively detecting the secretion of inflammatory factor IL-6 in the culture supernatant by using an ELISA kit, and carrying out the operation process according to the kit instructions. The inflammatory factor inhibition was calculated according to the following formula:
the inflammatory factor inhibition rate Is (Im-Is)/(Im-In). times.100%
In the formula:
im-model group inflammatory factor secretion, pg/mL;
is-amount of inflammatory factor secretion in sample group, pg/mL;
in-inflammatory factor secretion In negative control group, pg/mL.
2. Test results
TABLE 5 inhibition of human gingiva inflammatory factor by each of the examples and comparative examples
According to the data in the table, the inhibition rates of examples 1-10 to the gingival cell inflammatory factor IL-6 can reach more than 60%, while the inhibition rates of comparative examples 2-10 to the inflammatory factor are lower, and only comparative example 1 has a more obvious inhibition effect on the inflammatory factor. Therefore, within the molecular weight and content ranges defined in the present invention, the hyaluronic acid oral care composition has a significant inhibitory effect on gingival cell inflammatory factors, thereby having a soothing inhibitory effect on inflammation present in the oral cavity or other discomfort caused by inflammation.
In addition, it can be seen from the data of comparative examples 7-10 that the formula developed for skin moisturizing and skin anti-aging has poor effects on oral anti-inflammation.
Test example 4: effect of hyaluronic acid oral Care compositions on oral wound repair
The cell scratching method for simulating wound healing in vitro is a simple method for measuring cell migration movement and repair capacity. On the monolayer adherent human gingival fibroblast HGF-1 cultured in a culture dish, a trace gun head is used for scribing in the central area of cell growth, cells in the central part are removed, then the cells are contacted with a sample with a repairing effect, the cells are continuously cultured for the time set by an experiment, and whether peripheral cells grow and migrate to a central scratching area is observed by photographing so as to judge the growth and migration capacity of the cells.
1. Experimental methods
Preparation of sample solution: the products of examples 1 to 10 and comparative examples 1 to 10 were prepared in a 0.2 wt% concentration DMEM medium without serum, and sterilized by filtration.
At 5X 10 5 Per mL density human gingival fibroblast HGF-1 cells were seeded in 24-well plates at 1000. mu.L cell suspension per well, 37 ℃ with 5% CO 2 Culturing for 24h under the condition, drawing a straight line on a monolayer cell in a culture hole along the vertical direction by using a 10-mu-L gun head to form a damaged area, scratching, discarding all liquid in the hole, adding each sample solution, adding 1000 mu L of each hole, simultaneously replacing a negative control group by serum-free DMEM high-sugar culture solution, continuously culturing for 48h, photographing and observing, analyzing the area ratio of the healed damaged area by using Image J software, and calculating the healing rate according to the following formula:
rate of healing ═ S 0 –S r )/S 0 ×100％
In the formula:
S 0 -initial scratch area, pixel;
S r -detecting the remaining scratch area, pixels, at the time point.
2. Test results
Table 6 healing rates of the examples and comparative examples on damaged human gingival cells
From the above data, it can be seen that within the molecular weight and content ranges defined in the present invention, the oral care composition has a wound healing rate of oral gingival cells of more than 80%, which is significantly higher than that of the control group and each proportion, and the synergistic effect is significant. Therefore, the oral care composition of the present invention has a good repairing effect on injured gingival cells in the oral cavity, and can solve various oral problems due to trauma.
In addition, it can be seen from the data of comparative examples 7-10 that the oral cell repair effect is not good when the formula developed for skin moisturizing and skin anti-aging is applied.
Test example 4: effect of hyaluronic acid oral Care compositions on oral moisturizing
Sensory tests were conducted to compare the oral wettability and comfort before and after use using a mouth rinse base formulation as a control and a sample of the mouth rinse base formulation with 0.2 wt% hyaluronic acid oral care composition (example 10) as an experimental group.
1. Preparation of Experimental samples
The basic formula of the mouthwash is as follows:
propylene glycol 5%
10 percent of glycerin
Polysorbate-202%
0.5 percent of essence
0.3 percent of saccharin sodium
Purifying water to 100%
The base mouthwash is numbered mouthwash 1. A mouthwash to which 0.2 wt% oral care composition was added was numbered mouthwash 2.
2. Sensory test method
The number of the tested persons in the sensory test is 1-9, the age is 18-40 years old, 5 men and 4 women. Mouthwash 1 and mouthwash 2 were used after breakfast and lunch, respectively. The specific use method is as follows: before using the mouthwash, the user rinses with clear water, and the method comprises the following steps: the clear water is contained in the mouth, the two cheeks are shaken, the clear water can be fully contacted with teeth and gum in the mouth, and each part of the mouth is repeatedly flushed by utilizing the water power, so that food residues remained in the mouth are removed as much as possible. The method for using the mouthwash is as follows: the mouth wash containing about 12 ml of mouth wash water is used for rinsing for 1 minute by the method, and the mouth wash is finished without rinsing.
3. Sensory evaluation and results:
the evaluation method mainly evaluates the mouth feel comfort (whether taste exists or not and irritation exists) during mouth rinsing, the oral wettability and the lubricity after mouth rinsing and whether the oral water is rich or not, and fills the evaluation table with the mouth feel comfort, the oral wettability and the lubricity. Evaluation reference: for sensory evaluation score, the full score is 5, the score of 5 is the best effect, the mouth feel is comfortable, the wettability and the lubricity are good, the oral liquid amount is rich, the sequential effect weakening is 4, 3, 2, 1, the effect of 1 is the worst, the mouth feel is poor, irritation is generated, the mouth is dry after gargling, the mouth is dry, and the lubricity is poor. Each score is 1-5.
TABLE 7 sensory evaluation Table
As can be seen from the comparison of the data in the table, the mouthwash 2 containing the hyaluronic acid oral care composition is generally evaluated to be higher than the mouthwash 1, and particularly has obvious advantages in oral wettability and lubricity, only has a weak advantage in mouth feel comfort, and has a small difference in effect in terms of the amount of the mouthwash. Therefore, the product of the invention has obvious oral moisturizing effect.
Therefore, the combination of the above experimental data can show that the hyaluronic acid oral care composition of the invention makes full use of different effects of different molecular weight fragments of HA on oral cells, can repair wounded gingival cells, can perform anti-inflammatory treatment on inflamed gingival cells, and HAs excellent moisturizing effect of HA, so as to nurse and improve the oral cavity, thereby showing a significant oral care effect. The hyaluronic acid oral care composition is solid powder, has good compatibility when being added into oral care cosmetics, can be added into various oral care cosmetics, and has wide application range.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the embodiments, and any other changes, modifications, combinations, substitutions and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (8)
1. The hyaluronic acid oral care composition is characterized by comprising the following components in percentage by weight: 30-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, 35-45% of hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and 20-30% of hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa.
2. The hyaluronic acid oral care composition according to claim 1, characterized by consisting of the following components in percentage by weight: 35-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, 38-43% of hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and 22-27% of hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa.
3. The hyaluronic acid oral care composition according to claim 1, which is composed of the following components in percentage by weight: 35-40% of hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-3 kDa, 38-43% of hyaluronic acid or salt thereof with the molecular weight of 400-500 kDa and 22-27% of hyaluronic acid or salt thereof with the molecular weight of 1300-1400 kDa.
4. The hyaluronic acid oral care composition of any of claims 1-3, characterized by: the hydrolyzed hyaluronic acid or the salt thereof is enzyme-digested oligomeric hyaluronic acid or the salt thereof which is obtained by degrading hyaluronic acid or the salt thereof by bacillus hyaluronidase which is obtained by fermenting and culturing bacillus A50CGMCC NO. 5744.
5. The hyaluronic acid oral care composition of any of claims 1-3, characterized by: the hyaluronic acid salt or the hydrolyzed hyaluronic acid salt is sodium salt, potassium salt, magnesium salt, calcium salt or zinc salt of hyaluronic acid or hydrolyzed hyaluronic acid.
6. A method of preparing a hyaluronic acid oral care composition of claim 1, 2, 4 or 5, characterized by: respectively crushing and sieving hydrolyzed hyaluronic acid or salt thereof with the molecular weight of 2-5 kDa, hyaluronic acid or salt thereof with the molecular weight of 200-600 kDa and hyaluronic acid or salt thereof with the molecular weight of 1300-1500 kDa, and then uniformly mixing to obtain the hyaluronic acid oral care composition.
7. Use of a hyaluronic acid oral care composition according to any of claims 1-5 in the manufacture of an oral care product.
8. Use according to claim 7, characterized in that: the oral care product comprises mouthwash, toothpaste, mouth repair gel, mouth spray, mouth freshener, and mouth ulcer patch.
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| CN112007006B (en) * | 2020-08-07 | 2022-12-30 | 山东省药学科学院 | A pharmaceutical composition for treating oral ulcer, and its preparation method |
| CN112022738B (en) * | 2020-09-11 | 2022-09-13 | 华熙生物科技股份有限公司 | Oral mucosa protection plasma-explosion capsule containing hyaluronic acid, preparation method and application thereof |
| CN112168739A (en) * | 2020-09-25 | 2021-01-05 | 山东华熙海御生物医药有限公司 | Composition containing hyaluronic acid and application of composition in oral care product |
| CN112618413A (en) * | 2020-12-30 | 2021-04-09 | 重庆登康口腔护理用品股份有限公司 | Oral product containing hyaluronic acid and preparation method thereof |
| CN112618389A (en) * | 2021-02-04 | 2021-04-09 | 山东华熙海御生物医药有限公司 | Sodium bicarbonate whitening toothpaste containing hyaluronic acid and preparation method thereof |
| CN114159500A (en) * | 2021-11-25 | 2022-03-11 | 上海利康生物高科技有限公司 | Hyaluronic acid essential oil composition for nourishing and repairing oral cavity and application thereof |
| CN114344194B (en) * | 2021-12-28 | 2023-10-20 | 华熙生物科技股份有限公司 | Oral care composition containing hyaluronic acid or salt thereof, application and product thereof |
| CN115518004B (en) * | 2022-01-13 | 2024-01-16 | 海尼达(江苏)医疗科技有限公司 | Composition for assisting in improving oral health and application thereof |
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