CN116270336A - Composition with antibacterial and anti-inflammatory effects and application thereof in oral care products - Google Patents
Composition with antibacterial and anti-inflammatory effects and application thereof in oral care products Download PDFInfo
- Publication number
- CN116270336A CN116270336A CN202211575593.5A CN202211575593A CN116270336A CN 116270336 A CN116270336 A CN 116270336A CN 202211575593 A CN202211575593 A CN 202211575593A CN 116270336 A CN116270336 A CN 116270336A
- Authority
- CN
- China
- Prior art keywords
- seed oil
- antibacterial
- percent
- oral care
- bidens pilosa
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 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
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- 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
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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
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- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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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
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Abstract
The invention discloses a composition with antibacterial and anti-inflammatory effects and application thereof in oral care products, and belongs to the technical field of oral care products; the mass ratio of the bidens pilosa extract to the black seed oil is that the bidens pilosa extract is as follows: black seed oil= (0.25-2): (0.25-2). The composition has a strong inhibition effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like, has effects on inhibiting dental plaque and reducing gingivitis, has a remarkable synergistic effect on antibiosis of the bidens pilosa extract and the black seed grass seed oil, and has an antibiosis effect obviously superior to that of using only one of the bidens pilosa extract and the black seed grass seed oil.
Description
Technical Field
The invention relates to the technical field of oral care products, in particular to a composition with antibacterial and anti-inflammatory effects and application thereof in the oral care products.
Background
Chinese herbal medicine resources in China are rich, the application of the Chinese herbal medicine has a long history, most of Chinese herbal medicines have antibacterial and anti-inflammatory effects, but the antibacterial property of a single plant source bactericide in the nature is poor, and the development can cause cost waste. Therefore, the research on the compound plant source bactericide not only can effectively utilize the existing Chinese herbal medicine resources, but also can reduce the cost, expand the broad-spectrum antibacterial property of the bactericide and improve the antibacterial performance. Has positive significance for the application of the traditional natural medicines to the oral care products, and meets the development needs of the modern society.
CN103830355a discloses a nigella sativa seed oil nose drop and a preparation method thereof, wherein the nose drop is prepared from the following raw materials in parts by weight: 25-35 parts of black grass seed oil, 20-30 parts of ephedra herb, 20-30 parts of mosla chinensis, 15-25 parts of magnolia flower, 15-25 parts of angelica dahurica, 30-40 parts of centipeda minima, 20-30 parts of schizonepeta herb and 20-30 parts of divaricate saposhnikovia root; the preparation method of the nigella sativa seed oil comprises the following steps: adding 10 times of petroleum ether into nigella sativa seeds, extracting for 1h for 2 times, mixing oil and fat, and recovering solvent to obtain nigella sativa seed oil. The nigella sativa seed is extracted by petroleum ether to obtain nigella sativa seed oil, the nigella sativa seed oil nose drops have good anti-inflammatory effect, the content of antibacterial active components is low due to the petroleum ether extraction, and the antibacterial effect of the nigella sativa seed oil is not verified.
CN107889461a discloses an immunocompetent plant mixture and its use in a method of preventing and treating rash, which claims that the ethanol extract of bidens pilosa has a certain antibacterial and anti-inflammatory effect, but its effect is partially not verified, and the actual use of bidens pilosa verifies that the ethanol extract of bidens pilosa has a certain antibacterial and anti-inflammatory performance.
Although the technology has been partially studied on the anti-inflammatory activity of nigella sativa seed oil and the antibacterial activity of bidens pilosa, no prior art has used the nigella sativa seed oil and the bidens pilosa extract in oral care products, and the combined effect is verified.
Disclosure of Invention
The present invention aims to overcome the deficiencies of the prior art and to provide a composition with antibacterial and anti-inflammatory properties and its use in oral care products, said composition having good antibacterial and anti-inflammatory properties.
In order to achieve the above object, in a first aspect of the present invention, there is provided a composition having antibacterial and anti-inflammatory effects, comprising Bidens pilosa extract, nigella sativa seed oil;
the mass ratio of the bidens pilosa extract to the black seed oil is that the bidens pilosa extract is as follows: black seed oil= (0.25-2): (0.25-2).
As a preferred embodiment of the present invention, the mass ratio of the bidens pilosa extract and the nigella sativa seed oil is that of the bidens pilosa extract: black seed oil= (1-2): (1-2).
As a preferred embodiment of the invention, the bidens pilosa extract is obtained by ultrasonic extraction with 60-95% ethanol solution as a solvent.
As a preferred embodiment of the present invention, the nigella sativa seed oil is obtained by cold pressing by a screw press.
In a second aspect of the invention, the present invention provides an oral care product comprising a composition as described above having antibacterial and anti-inflammatory effects.
As a preferred embodiment of the present invention, the composition having antibacterial and anti-inflammatory effects is contained in an amount of 1 to 4% by mass in the oral care product.
As a preferred embodiment of the invention, the invention further comprises the following components in percentage by mass: 12 to 50 percent of friction agent, 27 to 71 percent of humectant, 2 to 3 percent of foaming agent, 0.6 to 1.3 percent of thickening agent, 0.2 to 0.3 percent of sweetener and the balance of water.
As a preferred embodiment of the present invention, the friction agent includes at least one of dibasic calcium phosphate dihydrate, silica, hydroxyapatite, sodium metaphosphate, potassium metaphosphate, tribasic calcium phosphate, calcium pyrophosphate, magnesium orthophosphate, tribasic magnesium phosphate, calcium carbonate and sodium bicarbonate.
As a preferred embodiment of the present invention, the humectant comprises at least one of glycerin, sorbitol, propylene glycol, polyethylene glycol, sorbitol, xylitol, maltitol, mannitol; and/or
The foaming agent comprises at least one of sodium dodecyl sulfate and sodium dodecyl sarcosinate; and/or
The thickener comprises at least one of xanthan gum, sodium carboxymethyl cellulose, starch, hydroxyethyl propyl cellulose, hydroxybutyl methyl cellulose, hydroxyethyl cellulose, carrageenan, gellan gum and locust bean gum; and/or
The sweetener comprises at least one of saccharin sodium, glucose, dextrose, invert sugar, fructose, sucrose and glycyrrhizin.
As a preferred embodiment of the invention, the invention further comprises the following components in percentage by mass: 0.15 to 0.25 percent of preservative, 0 to 0.7 percent of buffer and 0.6 to 1 percent of essence.
The invention has the beneficial effects that: (1) The composition has a strong inhibition effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like, has effects on inhibiting dental plaque and reducing gingivitis, has a remarkable synergistic effect on antibiosis, and has an antibiosis effect obviously superior to that of only one of the two (under the condition of the same dosage). (2) Toothpaste prepared from herba Bidentis Bipinnatae extract and semen Nigellae oil has excellent antibacterial and antiinflammatory effects, and good stability.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the invention, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present invention, the numerical ranges are referred to as continuous, and include the minimum and maximum values of the ranges, and each value between the minimum and maximum values, unless otherwise specified. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
In the present invention, the specific dispersing and stirring treatment method is not particularly limited.
In the present invention, the parts are parts by mass unless specifically stated otherwise.
The reagents or apparatus used in the present invention are conventional products commercially available without the manufacturer's knowledge.
The embodiment of the invention provides a composition with antibacterial and anti-inflammatory effects, which comprises a bidens pilosa extract and black seed oil;
the mass ratio of the bidens pilosa extract to the black seed oil is that the bidens pilosa extract is as follows: black seed oil= (0.25-2): (0.25-2).
Nigella plants are mainly distributed in asia, africa and europe, and their seeds are mainly nigella sativa (nigella glandulifera), nigella sativa (nigella sativa) and nigella sativa (nigella damascana) as medicinal resources. The nigella sativa seeds are dry mature seeds of nigella sativa of Ranunculaceae, are plant resources special for Xinjiang and Yunnan of China and are used as the conventional medicinal materials of Uyghur and Dai nationality, and the nigella sativa seeds have remarkable effects on protecting liver and kidney, resisting cancer, resisting oxidation, resisting inflammation, relieving cough, eliminating phlegm, resisting virus, regulating immunity and the like.
Bidens pilosa L is a plant of the genus Bidens (Bidens L.) of the family Compositae, also known as herba Bidens pilosae. The whole herb can be used as medicine, has the functions of clearing heat and detoxicating, removing blood stasis and detumescence, and can be used for treating malaria, diarrhea, dysentery, hepatitis, acute nephritis, stomach ache, dysphagia, acute appendicitis, sore throat, traumatic injury, snake and insect bite, etc. The extract mainly comprises flavonoids, eneyne, coumarin, organic acid and its esters, triterpene, sterol, volatile oil, etc. by ultrasonic extraction method, wherein the content of flavonoids is high.
The invention creatively combines the bidens pilosa extract and the black seed oil, discovers that the bidens pilosa extract and the black seed oil have stronger inhibition effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus, streptococcus mutans, candida albicans and the like, and has effects on inhibiting dental plaque and relieving gingivitis, and the inventor discovers that the bidens pilosa extract and the black seed oil have obvious synergistic effect on antibiosis through a large number of experiments, and the combined antibiosis effect of the bidens pilosa extract and the black seed oil is obviously superior to that of the bidens pilosa extract and the black seed oil which are only used in one (under the condition of the same dosage).
In some embodiments, the mass ratio of the bidens pilosa extract to the nigella sativa seed oil is the bidens pilosa extract: black seed oil= (1-2): (1-2). Particularly, the effect is better at this ratio.
In some embodiments, the bidens pilosa extract is obtained by ultrasonic extraction with 60-95% ethanol solution as a solvent. At present, the sticktight is usually extracted by adopting a reflux extraction method, and the extraction time is long. The invention adopts the ultrasonic extraction method and has the advantages of high extraction efficiency, short extraction time, low extraction temperature, simple and easy operation, convenient equipment maintenance and the like.
More specifically, the preparation method of the bidens pilosa extract comprises the following steps: pulverizing herba Bidentis Bipinnatae, sieving with No. four sieve (pharmacopoeia grade), adding into 60-95% ethanol solution (feed-liquid ratio is 1g: 8-20 ml), performing ultrasonic extraction for 1-3 times with ultrasonic power of 150-300W for 45min each time, mixing extractive solutions, and filtering to obtain herba Bidentis Bipinnatae extract.
In some embodiments, the nigella sativa seed oil is cold pressed by a screw press.
More specifically, the preparation method of the nigella sativa seed oil comprises the following steps: selecting nigella sativa seeds, removing impurities, peeling, cleaning with clear water, peeling, drying at 30-40 ℃ for 1-3 days, putting into a screw press, extruding and flowing out grease from gaps of a pressing cage, deforming solid into solid bran pieces (cake rings) and discharging the solid bran pieces (cake rings) from the tail end of a pressing chamber, adjusting the cake rings to 8mm, adjusting the pressing temperature to 50 ℃, pressing for 5 times, controlling the rotation speed of a pressing shaft of an oil press to be 30r/min, precipitating and standing nigella sativa seed oil crude oil obtained by cold pressing, and removing impurities such as nigella sativa seed kernel chips in the crude oil by combining a filter cloth and a centrifugal machine to obtain the nigella sativa seed oil product.
The existing extraction method of the volatile oil of the nigella plant seeds mainly comprises a steam distillation method, a supercritical fluid extraction method and the like. The most common extraction method is a steam distillation method, but the method has the advantages of longer extraction time, lower extraction efficiency, higher temperature, larger loss of volatile substances and adverse extraction of thermally unstable substances. The supercritical fluid extraction method has a great improvement in extraction efficiency, but the required equipment is complex, a high-pressure device is required, and the production cost is high. The nigella sativa seed oil adopted by the invention adopts a standardized cold pressing high-efficiency clean separation technology, so that the content of the obtained effective matters is high, the quality is stable, the process is simple, the period is short, and the nigella sativa seed oil is suitable for large-scale industrial production.
The extracted nigella seed oil has strong activity, and contains 3 to 3.4 percent of thymoquinone, 0.1 to 0.2 percent of thymoquinone, 1.0 percent of p-cymene, 0.1 to 0.2 percent of carvacrol, 0.1 to 0.2 percent of longifolene and 0.01 to 0.02 percent of Nigellone by weight percent; the main active ingredients of the bidens pilosa extracted by ultrasonic comprise flavonoids, eneyne, coumarin, organic acid and esters thereof, triterpenes, sterols, volatile oil and the like, wherein the flavone content is higher. The black seed oil and the bidens pilosa extract have synergistic effect and exert anti-inflammatory and antibacterial effects to the greatest extent.
An embodiment of the present invention provides an oral care product comprising the above-described composition having antibacterial and anti-inflammatory effects.
In some embodiments, the antibacterial and anti-inflammatory composition is present in the oral care product in an amount of 1 to 4% by mass.
In some embodiments, the composition further comprises the following components in percentage by mass: 12 to 50 percent of friction agent, 27 to 71 percent of humectant, 2 to 3 percent of foaming agent, 0.6 to 1.3 percent of thickening agent, 0.2 to 0.3 percent of sweetener and the balance of water.
The oral care product containing the composition with antibacterial and anti-inflammatory effects has good inhibition effect on enterobacteria, staphylococcus aureus, streptococcus mutans and candida albicans, and the anti-inflammatory effect experiment proves that the oral care product containing the nigella sativa seed oil and the bidens pilosa extract has excellent anti-inflammatory effect and good stability.
In some embodiments, the friction agent comprises at least one of dibasic calcium phosphate dihydrate, silica, hydroxyapatite, sodium metaphosphate, potassium metaphosphate, tribasic calcium phosphate, calcium pyrophosphate, magnesium orthophosphate, tribasic magnesium phosphate, calcium carbonate, sodium bicarbonate.
In some embodiments, the humectant comprises at least one of glycerin, sorbitol, propylene glycol, polyethylene glycol, sorbitol, xylitol, maltitol, mannitol.
In some embodiments, the foaming agent comprises at least one of sodium dodecyl sulfate, sodium dodecyl sarcosinate.
In some embodiments, the thickener comprises at least one of xanthan gum, sodium carboxymethyl cellulose, starch, hydroxyethyl propyl cellulose, hydroxybutyl methyl cellulose, hydroxyethyl cellulose, carrageenan, gellan gum, locust bean gum.
In some embodiments, the sweetener comprises at least one of saccharin sodium, glucose, dextrose, invert sugar, fructose, sucrose, glycyrrhizin.
In some embodiments, the composition further comprises the following components in percentage by mass: 0.15 to 0.25 percent of preservative, 0 to 0.7 percent of buffer and 0.6 to 1 percent of essence.
Illustratively, the preservative includes at least one of sodium benzoate, butyl hydroxy anisole, butyl hydroxy toluene, methyl parahydroxybenzoate, propyl parahydroxybenzoate.
Illustratively, the buffering agent includes at least one of sodium dihydrogen phosphate, sodium pyrophosphate, disodium hydrogen phosphate, sodium carbonate, sodium bicarbonate, sodium silicate.
The following examples are provided to facilitate an understanding of the present invention. These examples are not provided to limit the scope of the claims.
Example 1
1. Preparation of Bidens pilosa extract and black seed oil.
1.1 preparation method of Bidens pilosa extract comprises the following steps: pulverizing herba Bidentis Bipinnatae, sieving with No. four sieve (pharmacopoeia grade), adding into 80% ethanol solution (feed-liquid ratio of 1g:12 ml), performing ultrasonic extraction for 2 times with ultrasonic power of 200W and ultrasonic time of 45min each time, mixing extractive solutions, and filtering to obtain herba Bidentis Bipinnatae extract.
The obtained Bidens pilosa extract mainly contains flavonoids, eneyne, coumarin, organic acid and esters thereof, triterpenes, sterols, volatile oil, etc.
1.2 preparation method of nigella sativa seed oil comprises the following steps: selecting nigella sativa seeds, removing impurities, peeling, cleaning with clear water, drying at 40deg.C for 2 days, putting dried nigella sativa seeds into a screw press, squeezing oil out of the gap of a squeezing cage, deforming solid into solid bran pieces (cake rings), discharging from the end of the squeezing chamber, adjusting the cake rings to 8mm, adjusting the squeezing temperature to 50deg.C, squeezing for 5 times, setting the rotation speed of the squeezing shaft of an oil press to 30r/min, settling the crude oil of the nigella sativa seed obtained by cold squeezing, filtering with filter cloth, and centrifuging to obtain nigella sativa seed oil.
The active ingredient content of the prepared black seed oil is in the following range: 3 to 3.4 percent of thymoquinone, 0.1 to 0.2 percent of thymoquinone, 1.0 percent of p-cymene, 0.1 percent of carvacrol, 0.1 to 0.2 percent of longifolene and 0.01 to 0.02 percent of Nigellone.
2. Verification of synergistic antibacterial effect of Bidens pilosa extract and black seed oil
2.1 preparation of Bidens pilosa extract and nigella sativa seed oil was performed according to the following table protocol.
TABLE 1
| Scheme for the production of a semiconductor device | Nigella seed oil/g | Bidens pilosa extract/g |
| 1 | 1 | 0 |
| 2 | 2 | 0 |
| 3 | 0 | 1 |
| 4 | 0 | 2 |
| 5 | 1 | 1 |
| 6 | 1 | 2 |
| 7 | 2 | 1 |
| 8 | 2 | 2 |
2.2 preparation of experimental protocol: taking the scheme by aseptic operation, adding the Bidens pilosa extract and the black seed oil in the scheme, 0.15g of absolute ethyl alcohol, 0.35g of Tween 20, 0.5g of 0.03mol/L phosphate buffer (pH=7.2) and water to 100g, and fully oscillating and dissolving to prepare the uniformly dispersed suspension with corresponding concentration.
2.3 antibacterial test method
According to the QB/T2738-2012 (evaluation method of antibacterial and bacteriostatic effects of daily chemical products) 7.3 suspension quantification method, test samples of different schemes are tested for antibacterial rates of staphylococcus aureus, escherichia coli, candida albicans and streptococcus mutans to evaluate antibacterial effects of different combination ratios.
The experimental steps are referred to standard QB/T2738-2020-7.3.3, the experimental strains are staphylococcus aureus ATCC 6538, escherichia coli 8099, candida albicans ATCC 10231 and streptococcus mutans ATCC 25175, the action time is 3min, and the calculation formula of the bacteriostasis rate is as follows:
wherein: i-average colony count for control protocol, II-average colony count for test protocol.
The test results are shown in Table 2.
TABLE 2
According to QB/T2738-2012-7.3.6 antibacterial effect evaluation criteria, the antibacterial effect is 50% -90%, and the antibacterial experiment results show that the antibacterial effect of the scheme 5-8 on staphylococcus aureus, escherichia coli, candida albicans and streptococcus mutans is 50%, wherein the scheme 8 (namely 2% of each of the black seed oil and the sticktight extract) has the best comprehensive antibacterial ability on staphylococcus aureus, escherichia coli, candida albicans and streptococcus mutans, and under the condition of the same addition amount of the same efficacy, the antibacterial effect of the single efficacy extract is poorer than that of the other efficacy extract, and the two efficacy extracts are compounded, so that the synergistic effect can be exerted, and the antibacterial effect is remarkably improved.
Example 2
1 toothpaste containing the composition with antibacterial and anti-inflammatory effects, the formulation is shown in table 3.
TABLE 3 Table 3
1.1 preparation method of toothpaste containing semen Nigellae oil and herba Bidentis Bipinnatae extract of calcium hydrophosphate system
Accurately weighing various raw materials according to the formula proportion for standby, adding deionized water into saccharin sodium and sodium pyrophosphate water-soluble raw materials for dissolving, adding propylene glycol and sorbitol (pre-mixing 1), dissolving herba Bidentis Bipinnatae extract with glycerol (pre-mixing 2), adding calcium hydrophosphate dihydrate, sodium dodecyl sulfate, sodium carboxymethyl cellulose and xanthan gum into a powder pot, starting a disperser for 20 minutes, uniformly dispersing for standby (pre-mixing 3), and dissolving nigella sativa seed oil and methyl hydroxybenzoate in essence (pre-mixing 4).
Starting the paste making machine, stopping the vacuum pump when the vacuum is increased to-0.08 MPa, opening the feeding valve, sucking the pre-mixing materials 1 and 2, keeping the vacuum degree at-0.08 MPa, starting the high-speed stirrer and the slow-speed scraping plate, sucking the pre-mixing materials 3, after the vacuum is increased to-0.095 MPa and dispersed for 30 minutes, adjusting the vacuum degree to-0.06 MPa after timing, stopping the vacuum pump, slowly opening the valve of the essence feeding port to the pre-mixing materials 4, and preferably preventing air from entering and affecting the vacuum degree. After premixing 4, closing the fragrance inlet valve, and continuously starting the fast and slow stirring machine and degassing for 15 minutes when the vacuum degree in the paste making pot reaches more than-0.09 MPa to obtain the finished paste.
1.2 preparation method of toothpaste containing semen Nigellae oil and herba Bidentis Bipinnatae extract in silica system
Accurately weighing various raw materials according to the formula proportion for standby, adding saccharin sodium raw material into a dispersing pot, dissolving with deionized water, adding polyethylene glycol 400 and sorbitol (pre-mixing 1), and dissolving herba Bidentis Bipinnatae extract with glycerol (pre-mixing 2). Adding silicon dioxide, sodium dodecyl sulfate, sodium carboxymethyl cellulose and xanthan gum into a powder pot, starting a disperser for 20 minutes, and uniformly dispersing for later use (premixing 3). Dissolving nigella sativa seed oil and methyl hydroxybenzoate in essence (premixing 4), starting a paste making machine, stopping a vacuum pump when vacuum is increased to-0.08 MPa, opening a feeding valve, sucking premixing 1 and 2, keeping the vacuum degree at-0.09 MPa, starting a high-speed stirrer and a slow scraping plate, sucking mixing 3, carrying out vacuum increasing to more than-0.095 MPa, dispersing for 30 minutes, regulating the vacuum degree to-0.06 MPa after timing, stopping the vacuum pump, slowly opening a valve of an essence adding port, and premixing 4 until air cannot enter, so as to prevent air from entering and influence the vacuum degree. After premixing 4, closing the fragrance inlet valve, and continuously starting the fast and slow stirring machine and degassing for 15 minutes when the vacuum degree in the paste making pot reaches more than-0.09 MPa to obtain the finished paste.
2. Performance testing
2.1 stability test
The prepared toothpaste finished product is placed in an electric heating constant temperature drying oven at 45 ℃, after the placing is carried out for 3 months, the sample is taken out to be compared with a sample stored at normal temperature, and the changes of appearance, fragrance, 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 can be deduced, and the test result is shown in Table 4.
TABLE 4 Table 4
As can be seen from Table 4, the toothpaste of the present invention has good stability and can pass the stability test.
2.2 antibacterial Property test
The inhibition effect of finished toothpaste with different additive amounts of functional substances on staphylococcus aureus, escherichia coli, candida albicans and streptococcus mutans is tested according to a QB/T2738-2012 (evaluation method of antibacterial and bacteriostatic effect of daily chemical products) 7.3 suspension quantification method.
The experimental steps are referred to standard QB/T2738-2020-7.3.3, the experimental strains are staphylococcus aureus ATCC 6538, escherichia coli 8099, candida albicans ATCC 10231 and streptococcus mutans ATCC 25175, the action time is 3min, and the calculation formula of the bacteriostasis rate is as follows:
wherein: i-average colony count for control protocol, II-average colony count for test protocol.
The test results are shown in Table 5.
TABLE 5
According to QB/T2738-2012-7.3.6 antibacterial effect evaluation standard, the antibacterial rate is 50% -90%, and the product has antibacterial effect, and according to the stability and antibacterial performance test results, the toothpaste containing the black seed oil and the bidens pilosa extract has antibacterial effect, and through the stability test, various indexes also meet the national standard requirements of the toothpaste.
3. Anti-inflammatory action experiment
3.1 test sample: toothpaste # 1 in calcium hydrophosphate system and toothpaste # 3 in silica system.
3.2 experimental animals: SPF KM mice 24, male, 18 g-22 g, supplied by Guangdong medical laboratory animal center, laboratory animal production license number SCXK 2018-0002.
3.3 instruments and reagents
The main instrument is METTLER TOLEDO AG electronic balance and 8mm puncher.
Reagent, xylene.
3.4 test methods
3.4.1 randomly dividing 36 SPF-grade KM mice subjected to quarantine into 3 groups, wherein each group comprises 12 mice, namely a test object group 1, a test group 2 and a model control group.
3.4.2 after quarantine grouping of mice, the left ear is not treated to serve as a background value, 30 mu L of xylene solution is coated on the inner side and the outer side of the right ear, after 30 min, a model control group is not treated, 0.1g of corresponding paste is coated on the two sides of the right ear of the mice in a test object group, after 1h of sample coating, the mice are killed by dislocation of cervical vertebra, the test object is wiped off, two ears are cut off, and the weighing record is carried out on the ears (the same parts of the left ear and the right ear) with the diameter of 8 mm. The difference in weight of the left and right ears of the same animal is the swelling degree.
Swelling degree = right ear weight-left ear weight
Swelling inhibition = (average swelling degree of model control group-average swelling degree of test substance group)/average swelling degree of model control group x100%.
3.5 statistical analysis, experimental data are expressed as mean.+ -. Standard deviation
The independent sample T-test was performed using SPSS software.
3.6 test results: the inhibitory effect of ear swelling in mice is shown in table 6 below.
TABLE 6
| Group of | Ear swelling degree (mg) | Ear swelling inhibition (%) |
| Model control group | 22.33±2.78 | - |
| Calcium hydrogen phosphate System 1# | 15.03±3.75* | 32.69* |
| Silica System 3# | 14.93±3.65* | 33.14* |
Note that P <0.05 compared to model control.
The mice in the subject group had a reduced ear swelling compared to the model control group, and the differences were statistically significant (P < 0.05).
As can be seen from table 6, under the test conditions, the ear swelling degree of the toothpaste 1# containing the black seed oil and the bidens pilosa extract calcium hydrophosphate system and the toothpaste 3# containing the black seed oil and the bidens pilosa extract silicon dioxide system is obviously reduced (P < 0.05) compared with the model control group, and the toothpaste samples containing the black seed oil and the bidens pilosa extract have certain anti-inflammatory effect.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been 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 to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. A composition with antibacterial and anti-inflammatory effects is characterized by comprising Bidens pilosa extract and black seed oil;
the mass ratio of the bidens pilosa extract to the black seed oil is that the bidens pilosa extract is as follows: black seed oil= (0.25-2): (0.25-2).
2. The composition with antibacterial and anti-inflammatory effects according to claim 1, wherein the mass ratio of the bidens pilosa extract to the black seed oil is bidens pilosa extract: black seed oil= (1-2): (1-2).
3. The composition with antibacterial and anti-inflammatory effects according to claim 1, wherein the bidens pilosa extract is obtained by ultrasonic extraction using 60-95% ethanol solution as a solvent.
4. The composition having antibacterial and anti-inflammatory effects according to claim 1, wherein the nigella sativa seed oil is obtained by cold pressing with a screw press.
5. An oral care product comprising the antibacterial and anti-inflammatory composition according to any one of claims 1 to 4.
6. The oral care product according to claim 5, wherein the composition having antibacterial and anti-inflammatory effects is present in the oral care product in an amount of 1 to 4% by mass.
7. The oral care product of claim 5, further comprising the following components in mass percent: 12 to 50 percent of friction agent, 27 to 71 percent of humectant, 2 to 3 percent of foaming agent, 0.6 to 1.3 percent of thickening agent, 0.2 to 0.3 percent of sweetener and the balance of water.
8. The oral care product of claim 7, wherein the abrasive comprises at least one of dibasic calcium phosphate dihydrate, silica, hydroxyapatite, sodium metaphosphate, potassium metaphosphate, tricalcium phosphate, calcium pyrophosphate, magnesium orthophosphate, tribasic magnesium phosphate, calcium carbonate, sodium bicarbonate.
9. The oral care product of claim 7 wherein the humectant comprises at least one of glycerin, sorbitol, propylene glycol, polyethylene glycol, sorbitol, xylitol, maltitol, mannitol; and/or
The foaming agent comprises at least one of sodium dodecyl sulfate and sodium dodecyl sarcosinate; and/or
The thickener comprises at least one of xanthan gum, sodium carboxymethyl cellulose, starch, hydroxyethyl propyl cellulose, hydroxybutyl methyl cellulose, hydroxyethyl cellulose, carrageenan, gellan gum and locust bean gum; and/or
The sweetener comprises at least one of saccharin sodium, glucose, dextrose, invert sugar, fructose, sucrose and glycyrrhizin.
10. The oral care product of claim 7, further comprising the following components in mass percent: 0.15 to 0.25 percent of preservative, 0 to 0.7 percent of buffer and 0.6 to 1 percent of essence.
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