CN113730440A - Antibacterial composition and oral care product containing same - Google Patents
Antibacterial composition and oral care product containing same Download PDFInfo
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- CN113730440A CN113730440A CN202111073349.4A CN202111073349A CN113730440A CN 113730440 A CN113730440 A CN 113730440A CN 202111073349 A CN202111073349 A CN 202111073349A CN 113730440 A CN113730440 A CN 113730440A
- Authority
- CN
- China
- Prior art keywords
- oral care
- parts
- paeonol
- magnolol
- toothpaste
- Prior art date
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- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/12—Ketones
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/045—Hydroxy compounds, e.g. alcohols; Salts thereof, e.g. alcoholates
- A61K31/05—Phenols
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/63—Arthropods
- A61K35/64—Insects, e.g. bees, wasps or fleas
- A61K35/644—Beeswax; Propolis; Royal jelly; Honey
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/347—Phenols
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/35—Ketones, e.g. benzophenone
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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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
- A61K8/988—Honey; Royal jelly, Propolis
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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
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A—HUMAN NECESSITIES
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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
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
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- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
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- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a bacteriostatic composition and an oral care product containing the same. The bacteriostatic composition comprises the following components in parts by weight: 1-4 parts of paeonol, 1-4 parts of magnolol, 1-4 parts of propolis extract, and 6 parts of paeonol, magnolol and propolis extract. The paeonol, the magnolol and the propolis extract are reasonably compounded, and the paeonol, the magnolol and the propolis extract have good comprehensive antibacterial effect on escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like by utilizing the effects of complementation and mutual synergism of the paeonol, the magnolol and the propolis extract, have positive significance for applying the traditional natural medicine to oral care products, and meet the requirement of contemporary social development.
Description
Technical Field
The invention belongs to the field of daily chemicals, and relates to a bacteriostatic composition and an oral care product containing the same.
Background
In recent years, toothpaste manufacturers have gradually moved from using chemical bacteriostats (such as triclosan, cetylpyridinium chloride, chlorhexidine, etc.) to natural plant bacteriostats. Because the chemical bacteriostatic agent has some defects, such as objection to the safety of human bodies, influence on the stability of the formula, poor use taste and the like, the natural plant bacteriostatic agent can avoid the problems, and although the single natural plant bacteriostatic agent has slightly weak bacteriostatic ability, the defect of the bacteriostatic ability of the natural plant bacteriostatic agent can be solved as much as possible through purposeful compound research.
The application of paeonol, magnolol and propolis in oral care products such as toothpaste has been partially studied, and the oral care products have certain curative effect on relieving gingival inflammation, but have more or less shortcomings, such as failure to effectively inhibit most strains, and instability problems of discoloration and the like of toothpaste bodies caused by partial application in the toothpaste. How to utilize paeonol, magnolol and propolis to improve the comprehensive antibacterial ability of the oral care product, and make the oral care product have good stability, become the difficult problem to be solved urgently.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a bacteriostatic composition and an oral care product containing the same.
In order to achieve the above object, in a first aspect, the present invention provides a bacteriostatic composition, which comprises the following components in parts by weight: 1-4 parts of paeonol, 1-4 parts of magnolol, 1-4 parts of propolis extract, and 6 parts of paeonol, magnolol and propolis extract.
Paeonol is colorless, white or yellowish needle-shaped crystal with luster, is an effective component extracted from dried root bark of Paeonia suffruticosa of Ranunculaceae, has strong antibacterial effect on Staphylococcus aureus, Streptococcus faecalis, Escherichia coli, etc., and has tranquilizing, antiinflammatory, antipyretic, antiallergic, and other pharmacological effects. Modern researches have shown that paeonol can be rapidly absorbed, metabolized and excreted in human body with little toxic and side effects.
Magnolol is brown or white powder, is derived from natural plant cortex Magnolia officinalis, has broad-spectrum antibacterial effect, and good effect in killing cariogenic bacteria, and can be used for preparing toothpaste for preventing and treating dental caries.
Propolis is in the form of block or irregular fragment, is in the form of greenish blue, brown yellow, red, brown or dark brown, is a colloidal substance prepared by mixing resin substance collected by bee from new branch bud or flower bud of collagen plant with secretion of palate gland, and repeatedly processing by bee. Propolis is a traditional natural medicine, is recorded in pharmacopoeia of the people's republic of China, and defines ' tonifying deficiency, dissolving turbid fat and relieving thirst '; it is used externally to relieve swelling, astringe and promote granulation. Can be used for treating asthenia, senilism, hyperlipidemia, and diabetes; the external treatment of chapped skin, burn and scald has wide pharmacological activity, and a large number of studies prove that the external treatment of chapped skin, burn and scald has obvious bacteriostatic and anti-inflammatory effects when applied to the oral care aspect, and has the effects of inhibiting and killing staphylococcus aureus, escherichia coli, candida albicans and other germs.
The antibacterial composition utilizes the synergistic effect of the paeonol, the magnolol and the propolis extract, has good inhibition effect on escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like, and has better comprehensive antibacterial effect compared with the antibacterial composition using only one or two of the paeonol, the magnolol and the propolis extract. The antibacterial composition is applied to toothpaste, so that the toothpaste has obvious antibacterial and anti-inflammatory effects, dental plaque can be effectively inhibited, gingival inflammation can be effectively relieved, and the obtained toothpaste can still keep stable after being placed at 45 ℃ for 3 months.
Preferably, the bacteriostatic composition comprises the following components in parts by weight: 1-3 parts of paeonol, 1-3 parts of magnolol and 2-4 parts of propolis extract. When the paeonol, magnolol and propolis extracts are in the specific content, the obtained antibacterial composition has a better comprehensive antibacterial effect on escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like, the antibacterial rate can reach more than 50%, and the toothpaste has better effects of inhibiting dental plaque and relieving gingival inflammation when the composition is added into toothpaste.
Preferably, the paeonol is obtained by extracting root bark of peony with supercritical carbon dioxide, the magnolol is obtained by extracting bark of magnolia with supercritical carbon dioxide, and the propolis extract is obtained by extracting propolis with supercritical carbon dioxide.
The natural plant extract has complex components, and has ineffective components besides required effective components, and most of the traditional plant extraction processes are high temperature and high pressure, so that the effective components are easily damaged to a certain extent, and the obtained extract possibly has solvent residues, so that the extract has certain harmfulness to human bodies and the environment and is very unfavorable for developing new products.
The paeonol is extracted from the peony root bark by using a supercritical carbon dioxide extraction method, the extraction rate is high, the paeonol components are not easy to lose and damage, the obtained paeonol has high purity, light color and stable quality, the production process is simple and convenient to operate, and the toothpaste has strong inhibiting effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus and the like when being applied to toothpaste.
The effective component magnolol (containing honokiol) can be selectively extracted from the magnolia bark by using a supercritical carbon dioxide extraction method, 80 percent of the effective component in the magnolia bark can be extracted by the process, the production process is simple to operate, the process period is short, the obtained magnolol is used in toothpaste, and the toothpaste has good bacteria inhibiting (killing) effect on main cariogenic bacteria such as streptococcus mutans, lactobacillus acidophilus, lactobacillus and the like.
The supercritical carbon dioxide extraction method is adopted to extract the propolis, is nontoxic, residue-free and safe, and can effectively avoid the high-temperature decomposition and oxidation of effective components, so that the effective components can be effectively retained.
Preferably, the process parameters of the supercritical carbon dioxide extraction are as follows: adding an entrainer during extraction, wherein the entrainer is ethanol, the flow rate of the entrainer is 0.2-0.6 mL/min, the extraction temperature is 40-60 ℃, the extraction time is 80-120 min, and CO is added2The flow rate is 12-18 kg/(h.kg), and then secondary separation is carried out, wherein the pressure of the primary separation is 10-15 MPa, the temperature of the primary separation is 40-45 ℃, the pressure of the secondary separation is 6-10 MPa, and the temperature of the secondary separation is 38-42 ℃.
More preferably, the process parameters of the supercritical carbon dioxide extraction are as follows: entrainer flow rate of 0.4mL/min, extraction temperature of 50 deg.C, extraction time of 100min, and CO2The flow rate is 15 kg/(h.kg), and then the two-stage separation is carried out, wherein the pressure of the first-stage separation is 12MPa, the temperature of the first-stage separation is 42 ℃, the pressure of the second-stage separation is 8MPa, and the temperature of the second-stage separation is 40 ℃.
In a second aspect, the invention also provides an oral care product, which comprises the bacteriostatic composition.
Preferably, the antibacterial composition accounts for 0.3-0.6% of the weight of the oral care product. When the addition amount of the antibacterial composition in the oral care product is 0.3-0.6 wt%, the obtained oral care product has a good comprehensive antibacterial effect, dental plaque can be effectively inhibited, gingival inflammation can be relieved, and the obtained oral care product, such as toothpaste, can still be kept stable after being placed at 45 ℃ for 3 months.
Preferably, the antibacterial composition is contained in the oral care product in an amount of 0.5% by weight.
Preferably, the oral care implement is a toothpaste.
Preferably, the oral care implement further comprises a humectant, a taste modifier, a preservative, a colorant, a thickener, a foaming agent, an abrasive, a fragrance, and water.
Preferably, the toothpaste comprises the following components in parts by weight: 45-55% of humectant, 0.20-0.25% of taste modifier, 0.2-0.3% of preservative, 0.3-0.6% of colorant, 0.8-1.2% of thickener, 2.0-3.0% of foaming agent, 20-25% of abrasive, 1.0-1.5% of aromatic and the balance of water.
Preferably, the humectant is PEG-400 and sorbitol, the taste modifier is saccharin sodium, the preservative is sodium benzoate, the colorant is titanium dioxide, the thickener is sodium carboxymethylcellulose and xanthan gum, the foaming agent is sodium lauryl sulfate, the abrasive is silicon dioxide, and the aromatic is edible essence.
Humectant: the toothpaste has the main effects that the toothpaste body is kept moist and certain moisture is kept, when the toothpaste body is exposed in the air, the moisture in the toothpaste body can be effectively prevented from being evaporated and lost, so that the toothpaste at the pipe orifice is not easy to dry and agglomerate during the storage period, is easy to extrude and is convenient for consumers to use; meanwhile, the rheological property of the paste is improved and maintained, and the filling is convenient in production; lowering the freezing point; the stability of the toothpaste is improved. PEG-400 is compounded with sorbitol, and the PEG-400 has a good moisturizing function, a lower freezing point than glycerol, an antifreezing property and an effect of dissolving tooth stains; sorbitol is a common toothpaste humectant, and researches show that the moisturizing effect is more stable than that of glycerin, the loss moisture of sorbitol is lower than that of glycerin at lower humidity, and the absorption moisture of sorbitol is lower than that of glycerin at higher humidity, so that the toothpaste humectant has very good freezing resistance and good taste. The mass ratio of PEG-400 to sorbitol is usually 10: 1.
taste modifier: is used for improving the mouthfeel of the toothpaste and covering the bad taste of certain ingredients of the toothpaste. Saccharin sodium is an artificial sweetener, has a long history and stable application, and is widely used as a taste modifier in toothpaste.
Preservative: preventing and inhibiting the growth of toothpaste microorganisms, and avoiding the decay and deterioration of toothpaste. Sodium benzoate is used as a preservative, and when the formula system uses silicon dioxide as an abrasive and has a high proportion of alcohol humectant, the sodium benzoate can completely deal with the preservative of the formula.
Colorant: for altering the appearance of toothpaste. The titanium dioxide is extremely stable in chemical property, has excellent whiteness, tinting strength, covering power, weather resistance, heat resistance and chemical stability compared with other white pigments, has no toxicity, can weaken the transparent feeling of a formula silicon dioxide system, and can also properly lighten the yellowing of the paste caused by functional substances.
Thickening agent: the toothpaste is a key and leading raw material for ensuring the stability of the toothpaste, can ensure that the toothpaste has proper viscosity and consistency and good flowing and strip forming performance, and ensures that the toothpaste body is easy to disperse when a consumer brushes the teeth, the powder in the toothpaste system can be stably dispersed in a liquid phase, and the toothpaste body is ensured to be in a stable state. Sodium carboxymethylcellulose is a toothpaste thickener commonly used at home and abroad at present, is low in price, has the functions of thickening and stabilizing paste, but has large influence on viscosity due to soluble electrolytes, particularly sodium salt and heavy metals, and is easy to biodegrade under the action of enzyme, so that xanthan gum is compounded in the formula, the salt resistance and enzyme resistance of the paste are improved, the dispersibility, the appearance, the taste and the filling performance of the paste are also improved, and the mass ratio of the sodium carboxymethylcellulose to the xanthan gum is 3: 1.
foaming agent: the toothpaste generates rich foam when brushing teeth and rubbing, gives certain sensory experience to consumers, simultaneously plays the roles of removing tartar and cleaning oral cavity, has certain emulsification effect, and can be beneficial to the formation of a stable system of oil-soluble substances such as essence and the like and other components in the toothpaste. Sodium dodecyl sulfate is the most commonly used toothpaste foaming agent at present, has good cost performance in price and foaming power, and also has excellent decontamination, emulsification and foaming power compared with other foaming agents.
Aromatic agent: endows the toothpaste with fragrance and mouthfeel, covers the peculiar smell of certain ingredients, and gives the product with label cognition of specific style.
Compared with the prior art, the invention has the beneficial effects that: the paeonol, the magnolol and the propolis extract are reasonably compounded, and the effects of supplementing each other and mutual synergy of the paeonol, the magnolol and the propolis extract are utilized, so that the greatest respective effects of the paeonol, the magnolol and the propolis extract can be exerted, the defects of single improvement or double improvement are overcome, a good comprehensive antibacterial effect is generated on escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like, the oral care product has positive significance on the application of the traditional natural medicine to the oral care product, and the oral care product meets the requirement of contemporary social development.
Drawings
FIG. 1 is a graph of the bacteriostatic results in example 2.
Figure 2 is a process flow for the preparation of toothpaste according to example 3.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
Extracting cortex moutan, cortex Magnolia officinalis and propolis respectively by supercritical carbon dioxide extraction method to obtain paeonol, magnolol and propolis extract. The three extraction processes are the same, and specifically comprise the following steps: adding a certain amount of raw materials into extraction kettle, heating the extraction kettle, the analysis kettle I, the analysis kettle II, the separation column and the storage tank respectively, and starting CO when the selected temperature is reached2A bottle, pressurizing the system by a high pressure pump, and closing CO when the pressure of the extraction kettle, the pressure of the analysis kettle I, the pressure of the analysis kettle II and the pressure of the separation column reach the set pressure respectively2Bottle, beginning to circularly extract, adding a certain amount of entrainer and regulating CO2The flow rate of the water reaches a certain amount, and the constant temperature and the constant pressure are kept. And when the selected extraction time is reached, separating the extract by the resolving kettle I and the resolving kettle II in sequence, discharging from a discharge hole of the resolving kettle II to obtain a crude product of the active substances, and performing suction filtration or centrifugation, washing, refining and drying to obtain an ideal extract product.
The specific process parameters of the supercritical carbon dioxide extraction are as follows: entrainer is ethanol, entrainer flow rate is 0.4mL/min, extraction temperature is 50 deg.C, extraction time is 100min, and CO2The flow rate is 15 kg/(h.kg), and then the two-stage separation is carried out, wherein the separation pressure of the resolving kettle I is 12MPa, the separation temperature of the resolving kettle I is 42 ℃, the separation pressure of the resolving kettle II is 8MPa, and the separation temperature of the resolving kettle II is 40 ℃.
Example 2
(1) Preparation of test sample solution
The paeonol, magnolol and propolis extracts obtained in example 1 were subjected to in vitro antibacterial tests, and the specific test protocol is shown in table 1.
TABLE 1
Scheme(s) | Paeonol/g | Magnolol/g | Propolis extract/ |
1 | 0.6 | 0 | 0 |
2 | 0.4 | 0.2 | 0 |
3 | 0.4 | 0.1 | 0.1 |
4 | 0.4 | 0 | 0.2 |
5 | 0.3 | 0.2 | 0.1 |
6 | 0.3 | 0.1 | 0.2 |
7 | 0.2 | 0.4 | 0 |
8 | 0.2 | 0.3 | 0.1 |
9 | 0.2 | 0.2 | 0.2 |
10 | 0.2 | 0.1 | 0.3 |
11 | 0.2 | 0 | 0.4 |
12 | 0.1 | 0.4 | 0.1 |
13 | 0.1 | 0.3 | 0.2 |
14 | 0.1 | 0.2 | 0.3 |
15 | 0.1 | 0.1 | 0.4 |
16 | 0 | 0.6 | 0 |
17 | 0 | 0.4 | 0.2 |
18 | 0 | 0.2 | 0.4 |
19 | 0 | 0 | 0.6 |
Preparing a test sample solution: taking samples in the scheme by aseptic operation, firstly adding a small amount of absolute ethyl alcohol, then adding Tween 20 and distilled water (the content of Tween and ethanol is not more than 0.5%), carrying out ultrasonic emulsification, then adding 94mL of sterilized 0.03mol/L phosphate buffer (pH value is 7.2), and fully shaking and dissolving to prepare 1 wt% of uniformly dispersed suspension.
(2) Bacteriostatic test method
According to QB/T2738-.
The experimental procedure refers to part 7.3.3 of standard QB/T2738-:
in the formula: i-average number of colonies in control samples,
II-average colony number of test sample.
The results of the experiment are shown in FIG. 1.
According to the results of the bacteriostatic experiments shown in fig. 1, under the same total addition amount of the efficacy substances, the bacteriostatic rates of the schemes 6, 9, 10, 13, 14 and 15 on staphylococcus aureus, escherichia coli, candida albicans and streptococcus mutans are all over 50%, the bacteriostatic effect on four bacteria is proved according to the 7.3.6 bacteriostatic effect evaluation standard in QB/T2738-, the three components are compounded to play the role of mutual synergy, and the compound of the scheme can be applied to toothpaste.
Example 3
According to the schemes 6, 9, 10, 13, 14 and 15, respectively, paeonol, magnolol and propolis extract are added into the toothpaste according to the total adding amount of 0.5 wt%, and the mixture ratio of the other components in the toothpaste is shown in table 2.
TABLE 2
The preparation process of the toothpaste comprises the following steps:
1. accurately weighing saccharin sodium, sodium benzoate and deionized water, dissolving uniformly in advance, and pumping the uniformly dissolved solution into a paste making pot when the vacuum degree of the paste making pot is controlled to be-0.04 MPa-0.06 MPa;
2. accurately weighing PEG-400 and sorbitol, and pumping the PEG-400 and sorbitol into a paste making pot when the vacuum degree of the paste making pot is controlled between-0.04 MPa and 0.06 MPa;
3. stirring by a scraper and a double stirrer of a paste preparing pot;
4. accurately weighing silicon dioxide, titanium dioxide, sodium carboxymethylcellulose, xanthan gum and sodium lauryl sulfate, and controlling the vacuum degree of a paste preparation pot to be-0.06 MPa-0.08 MPa to pump powder of the silicon dioxide, the titanium dioxide, the sodium carboxymethylcellulose, the xanthan gum and the sodium lauryl sulfate into the paste preparation pot;
5. timing for 15-25 minutes by double stirring;
6. accurately weighing edible essence, paeonol, magnolol and propolis, dissolving in advance, adding into paste making pot, and stirring for 10 min;
7. stopping stirring, keeping the scraper on, and keeping the vacuum degree above-0.094 MPa for 5 minutes;
8. stopping stirring, inspecting, discharging, filling, inspecting, and warehousing.
The obtained toothpaste is respectively placed in an electric heating constant-temperature drying box at 45 ℃, is taken out after being placed for 3 months and is compared with a sample stored at normal temperature, and the changes of the appearance, the fragrance, the pH value and the like of the high-temperature sample are observed, so that the stability of the toothpaste within the shelf life of 3 years is deduced, and the result is shown in table 3.
TABLE 3
As can be seen from table 3, the composition of the above scheme was added to toothpaste in a total amount of 0.5 wt%, and the resulting toothpaste was left at 45 ℃ for 3 months with good stability and 3-year shelf life.
Example 4
The toothpaste obtained in example 3 (the total addition amount of the composition formed by paeonol, magnolol and propolis extracts in each scheme is 0.5 wt%, except for the composition and water, the types and the contents of other components are the same, and the balance is water) is tested according to a QB/T2738-2012 evaluation method for antibacterial and bacteriostatic effects of daily chemical products 7.3 suspension quantitative method on the inhibitory effects of staphylococcus aureus, escherichia coli, candida albicans and streptococcus mutans.
The experimental procedure refers to part 7.3.3 of standard QB/T2738-.
The results of the toothpaste bacteriostasis tests are shown in table 4.
TABLE 4
According to the evaluation standard of the 7.3.6 antibacterial effect in QB/T2738-2012 (namely that the product has an antibacterial effect when the antibacterial rate is 50-90%), the obtained toothpaste has an antibacterial effect on four kinds of bacteria and meets the national standard requirements of the toothpaste.
Example 5
(1) Test method and object
Using the toothpaste obtained in example 3 (scheme 9) as a test group and a toothpaste group without active ingredients (except the composition and water in scheme 9, the types and contents of the other ingredients are the same, and the balance of water) as a control group, the method of a random, double-blind and parallel control clinical test is adopted, and whether the effects of inhibiting dental plaque and relieving gingival inflammation exist after the product to be tested is used at least twice a day by a daily household under an unsupervised condition is evaluated for three months. The subjects were 72 healthy adult males and females meeting inclusion and exclusion criteria in guangzhou city.
(2) Procedure of the test
Gingivitis was assessed using the Gingival Index (GI), percent of bleeding on probation (BOP%), plaque was assessed using the Plaque Index (PI), clinical examinations were performed on the whole mouth at the start of the trial, 1 half month, 3 months, 6 sites per tooth were examined, and the normality of soft and hard tissues of the mouth was recorded. Subjects brushed their teeth twice a day for at least 1 minute using a uniformly dispensed toothbrush and toothpaste. Group A is experimental group, and toothpaste A (toothpaste containing supercritical extraction of paeonol, magnolol and propolis) is dispensed; group B was a control group and toothpaste B (toothpaste with no efficacy substance added) was dispensed.
(3) Test results
Of the 72 volunteers enrolled in the trial, 69 completed all (3 months) of the trial, and a total of 3 subjects were withdrawn halfway, with data not included in the statistical analysis.
The mean age and gender of the test and control groups are shown in table 5.
TABLE 5
The indexes of the test group and the control group are shown in table 6.
TABLE 6
Note: 1) comparing the P value of each index of the test group and the control group; 2) improvement rate (control mean-test mean)/control mean 100%.
The results of comparing the end of the test with the baseline indexes of the test group and the control group are shown in Table 7.
TABLE 7
Note: end compare P values to baseline indicators.
(4) Analysis and discussion
As shown in the statistical table, the mean age and gender distribution of the test group and the control group have no significant difference, and the indexes of the baseline examination have no significant difference. The test results of 3 months show that the plaque amount, the gingivitis degree and the probing bleeding percentage value of the test group show a gradually descending trend; the control group showed a downward trend in gingivitis, while the values of plaque and percentage of bleeding detected at the end of the test were slightly higher than those at the middle of the test. At the end of the test, the examination indexes of the test group and the control group are reduced to different degrees compared with the baseline examination, the examination indexes of the gingivitis and the plaque of the test group are all reduced by the control group, the difference degree is significant, wherein the plaque improvement rate is 23.50%, the gingivitis improvement rate is 21.2%, the probing bleeding percentage improvement rate is 23.0%, and no side effect of soft and hard tissues in the oral cavity is observed.
The clinical research result proves that compared with the common control group toothpaste without functional substances, the toothpaste containing paeonol, magnolol and propolis extracted by supercritical extraction can effectively inhibit dental plaque and relieve gingival inflammation, and is the toothpaste capable of inhibiting bacteria and diminishing inflammation.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The bacteriostatic composition is characterized by comprising the following components in parts by weight: 1-4 parts of paeonol, 1-4 parts of magnolol, 1-4 parts of propolis extract, and 6 parts of paeonol, magnolol and propolis extract.
2. The bacteriostatic composition according to claim 1, which comprises the following components in parts by weight: 1-3 parts of paeonol, 1-3 parts of magnolol and 2-4 parts of propolis extract.
3. The bacteriostatic composition according to claim 1 or 2, wherein the paeonol is obtained by extracting root bark of peony with supercritical carbon dioxide, the magnolol is obtained by extracting bark of magnolia with supercritical carbon dioxide, and the propolis extract is obtained by extracting propolis with supercritical carbon dioxide; the technological parameters of the supercritical carbon dioxide extraction are as follows: adding an entrainer during extraction, wherein the entrainer is ethanol, the flow rate of the entrainer is 0.2-0.6 mL/min, the extraction temperature is 40-60 ℃, the extraction time is 80-120 min, and CO is added2The flow rate is 12-18 kg/(h.kg), and then secondary separation is carried out, wherein the pressure of the primary separation is 10-15 MPa, the temperature of the primary separation is 40-45 ℃, the pressure of the secondary separation is 6-10 MPa, and the temperature of the secondary separation is 38-42 ℃.
4. The bacteriostatic composition according to claim 3, wherein the bacteriostatic composition is a bacteriostatic composition,the method is characterized in that the technological parameters of the supercritical carbon dioxide extraction are as follows: entrainer flow rate of 0.4mL/min, extraction temperature of 50 deg.C, extraction time of 100min, and CO2The flow rate is 15 kg/(h.kg), and then the two-stage separation is carried out, wherein the pressure of the first-stage separation is 12MPa, the temperature of the first-stage separation is 42 ℃, the pressure of the second-stage separation is 8MPa, and the temperature of the second-stage separation is 40 ℃.
5. An oral care product comprising the bacteriostatic composition according to any one of claims 1 to 4.
6. The oral care implement of claim 5, wherein the bacteriostatic composition is present in the oral care implement in an amount of 0.3 to 0.6% by weight.
7. The oral care implement of claim 6, wherein the bacteriostatic composition is present in the oral care implement at 0.5% by weight.
8. The oral care implement of any one of claims 5 to 7, wherein the oral care implement is a toothpaste.
9. The oral care implement of claim 8, wherein the toothpaste further comprises the following components in amounts by weight: 45-55% of humectant, 0.20-0.25% of taste modifier, 0.2-0.3% of preservative, 0.3-0.6% of colorant, 0.8-1.2% of thickener, 2.0-3.0% of foaming agent, 20-25% of abrasive, 1.0-1.5% of aromatic and the balance of water.
10. The oral care implement of claim 9, wherein the humectants are PEG-400 and sorbitol, the taste modifier is sodium saccharin, the preservative is sodium benzoate, the colorant is titanium dioxide, the thickening agents are sodium carboxymethylcellulose and xanthan gum, the foaming agent is sodium lauryl sulfate, the abrasive is silicon dioxide, and the flavoring agent is a flavorant.
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