CN111317708A - Soothing and refreshing toothpaste and preparation method thereof - Google Patents
Soothing and refreshing toothpaste and preparation method thereof Download PDFInfo
- Publication number
- CN111317708A CN111317708A CN202010130751.0A CN202010130751A CN111317708A CN 111317708 A CN111317708 A CN 111317708A CN 202010130751 A CN202010130751 A CN 202010130751A CN 111317708 A CN111317708 A CN 111317708A
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- China
- Prior art keywords
- toothpaste
- parts
- soothing
- stirring
- refreshing
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Abstract
The invention discloses a soothing fresh toothpaste which comprises the following components in parts by weight: 0-90 parts of solvent, 1-90 parts of humectant, 0-90 parts of abrasive, 0.1-30 parts of thickening agent, 0-20 parts of foaming agent, 0-10 parts of sweetening agent, 1-20 parts of plant compound extract, 0.1-50 parts of efficacy agent and 0.001-0.02 part of probiotics. The invention also discloses a preparation method of the moistening refreshing toothpaste. The invention has the beneficial effects that: the efficacy agent and the original abrasive of the toothpaste take effect synergistically, so that the toothpaste has good cleaning and whitening effects and also has very good repairing and whitening effects; the plant composite extract and the probiotics are added, so that the oral disease treatment bacteria such as streptococcus sobrinus, porphyromonas gingivalis, streptococcus mutans and fusobacterium nucleatum and the like can be effectively inhibited for a long time, and meanwhile, the oral disease treatment bacteria have an anti-inflammatory effect, can effectively assist in treating and preventing oral inflammation, keep fresh breath, eliminate halitosis and have good moistening and refreshing feeling; has good repairing effect on the damage of human gingival cells; has very good oral cavity moisturizing and other care effects.
Description
Technical Field
The invention relates to the field of toothpaste, in particular to a moistening and refreshing toothpaste with long-acting antibacterial and anti-inflammatory effects, effects of keeping oral cavity moistening and refreshing, repairing wounds and whitening and a preparation method thereof.
Background
The world health organization proposed that oral health including "chronic pain in the amateur jaw, oropharyngeal cancer, oral ulcers, congenital defects such as cleft lip and palate, periodontal (gum) disease, caries, tooth loss, and other diseases and disorders affecting the oral cavity" was listed as one of ten major criteria for overall health and was an important assessment item for assessing overall health. Oral health is now gaining more and more attention.
Toothpaste is a necessity of daily life for maintaining tooth health, and along with the continuous improvement of living standard, the toothpaste is developed from a common tooth cleaning type to a whitening functional type and the like. Additives used in existing whitening toothpastes generally include peroxide compounds, solvent compounds or high friction compounds. Although the peroxide compound has a relatively obvious whitening effect, the peroxide compound is extremely unstable and has poor matching performance with other components of toothpaste, so that the whitening effect is influenced, and the safety of the peroxide when being used in the oral cavity is controversial. Solvent-type compound additives such as polyethylene glycol and the like have certain effect of dissolving color spots, but the effect is not obvious and the cost is not low. High friction compounds such as anhydrous calcium hydrogen phosphate have the defect of great abrasion to tooth enamel when in use.
In addition, in reality, a large proportion of people have dry mouth and bad breath, which causes a series of psychological and physiological hidden troubles and is difficult to treat. The existing toothpaste aims to solve the problem, but the effect is not ideal.
Disclosure of Invention
The invention aims to provide the moistening and refreshing toothpaste with long-acting antibacterial and anti-inflammatory effects, the effects of keeping the mouth cavity moistening and refreshing, repairing wounds and whitening the skin, aiming at the defects of the prior art.
The second purpose of the invention is to provide a preparation method of the soothing and refreshing toothpaste.
In order to realize the purpose of the invention, the invention adopts the technical scheme that: the soothing and refreshing toothpaste is prepared from the following components in parts by weight:
the efficacy agent is prepared from the following components in parts by weight:
the preparation method of the efficacy agent comprises the following steps: mixing the above components uniformly;
the plant composite extract is prepared from the following traditional Chinese medicine components in parts by weight:
preferably, the soothing and refreshing toothpaste is prepared from the following components in parts by weight:
preferably, the moistening and refreshing toothpaste is prepared from the following components in parts by weight:
the solvent may include, but is not limited to, water, deionized water, purified water, and edible ethanol, among others.
The humectant may include, but is not limited to, polyol analogs such as glycerin, sorbitol, propylene glycol, glycerin, and polyethylene glycol.
The abrasive may include, but is not limited to, silica, titanium dioxide, calcium carbonate, calcium phosphate, sodium bicarbonate, kaolin, and cellulose and the like.
Such thickeners may include, but are not limited to, xanthan gum, sodium carboxymethylcellulose, sodium carboxyethylcellulose, carbomers, silicon dioxide, guar gum, carrageenan, polyvinylpyrrolidone, PVM/MA copolymer, and the like.
The foaming agent may include, but is not limited to, sodium lauryl sulfate, sodium methylcocoyl taurate, sodium cocoyl glutamate, sodium lauroyl glutamate, and cocoamine propyl betaine, and the like.
Such sweeteners may include, but are not limited to, sodium saccharin, sucralose, and erythritol analogs.
The probiotics can be sterilized lactobacillus paracasei LPC-37, can be selected from LPC-37 of DuPont company in America, can effectively inhibit the growth of pathogenic bacteria in the oral cavity, is beneficial to good oral health and protects teeth. Especially, the oral cavity antibacterial composite has a long-term good inhibition effect on streptococcus mutans, streptococcus sobrinus and fusobacterium nucleatum in oral cavity germs, and the antibacterial composite takes effect in a synergistic and composite mode with the plant composite extract, so that the antibacterial effect is more obvious, and the comfort and freshness of the oral cavity can be kept for a long time.
Preferably, the efficacy agent is prepared from the following components in parts by weight:
preferably, the efficacy agent is prepared from the following components in parts by weight:
preferably, the efficacy agent is prepared from the following components in percentage by mass:
preferably, the efficacy agent is prepared from the following components in parts by weight:
the hyaluronic acid is an important component of tissues such as gingiva, periodontal and periodontal ligament, and the like, and the supplement of hyaluronic acid can prevent and relieve inflammatory reaction of periodontal tissues, inhibit bacterial plaque to prevent inflammatory development of gingiva, reduce red and swollen reaction of wound, relieve pain, promote ulcer healing and repair gingival injury; in addition, hyaluronic acid is a natural moisturizing factor, keeps the oral cavity moist and lubricated, and improves the dry mouth symptom. Preferably, the hyaluronic acid may be oral specific hyaluronic acid of Huaxi Furrida biomedical corporation.
The sodium pyrophosphate can loosen and remove compact stains and calculus deposited on the surface of teeth, and can also prevent the deposition of calculus. In addition, sodium pyrophosphate and calcium ions in the formula can form colloid, so that the function of a stable system is achieved, and the deterioration and the invalidation of the toothpaste are avoided.
The Hydroxyapatite (HAP) has excellent biocompatibility and bioactivity, is an induction factor of bones or teeth, and has better remineralization, desensitization, restoration and whitening effects on teeth in the field of oral health care. Experiments prove that the HAP particles have good biocompatibility and high affinity with enamel, and the mineralized liquid can effectively form remineralization deposition, prevent calcium ions from losing, solve the problem of enamel demineralization and fundamentally prevent dental caries. The toothpaste containing HAP material has strong adsorption effect on salivary protein and dextran, can reduce dental plaque in oral cavity of patient, promote gingivitis healing, and has good prevention and treatment effect on dental caries and periodontal disease. Nano hydroxyapatite is preferred.
The particle size range of the perlite is 15-25 microns, the particle size range of the abrasive is 0.5-10 microns, and the perlite and the abrasive can effectively clean the surface of the enamel under the matching of the particle sizes, avoid damage to cracks of the enamel, promote repair and improve scrubbing and whitening effects.
Preferably, the plant composite extract is prepared from the following traditional Chinese medicine components in parts by weight:
the preparation method of the plant composite extract comprises the following steps:
(1) pretreating medicinal materials: weighing the traditional Chinese medicine raw materials of each component according to the formula dosage, crushing the traditional Chinese medicine raw materials into particles of 10-100 meshes, and uniformly mixing the particles to obtain a medicinal material mixture;
(2) extraction: placing the medicinal material mixture into a container, adding an extraction solvent which is 10-30 times of the total weight of the medicinal material mixture, soaking for 8-10 hours, treating for 2-4 times by ultrasonic waves at 60-75 ℃ for 30-50min each time, wherein the ultrasonic power is 700-;
(3) centrifuging: removing dregs of the extract by a centrifugal machine, wherein the speed of the centrifugal machine is 11000-13000 r/min, and the treatment time is 20-40 min;
(4) and (3) purification: filtering and centrifuging the extracting solution obtained in the step (3) by using a ceramic membrane with the aperture of 200-400 nm to obtain a liquid medicine;
(5) concentration: concentrating the liquid medicine until the weight ratio of the liquid medicine to the Chinese medicinal material mixture in the step (1) is 1: 1-3: 1.
Preferably, the extraction solvent in the step (2) is deionized water, pure water, a lower alcohol with carbon chains of C1-C4, and a lower alcohol aqueous solution with carbon chains of C1-C4 at a volume ratio concentration of 10-60%.
Preferably, the extraction solvent which is 15 to 25 times of the total weight of the medicine mixture is added in the step (2), the mixture is soaked for 9 hours, and the mixture is treated by ultrasonic waves with power of 750 and 850W for 2 to 3 times at 65 to 70 ℃, wherein each time lasts for 35 to 45 min. The ultrasonic wave is used for extraction under the specific power, the ultrasonic wave can generate appropriate multistage effects such as strong cavitation effect, disturbance effect, high acceleration, crushing and stirring action and the like, the molecular motion frequency and speed of the substance are increased, and the penetrating power of the solvent is increased, so that the target component is accelerated to enter the solvent, the extraction is promoted, but the required effective active ingredients are not damaged due to the strong cavitation effect, high acceleration and crushing effect, the extraction efficiency is improved, and the activity of the effective ingredients of the extract is ensured.
Preferably, the concentration temperature in the step (5) is 50-60 ℃.
The plant composite extract added into the toothpaste formula has good effects of soothing, removing dental plaque, performing gum physical therapy, inhibiting bacteria, resisting inflammation and refreshing breath.
The soothing and refreshing toothpaste of the present invention also includes, but is not limited to: essence, fluoride, preservative, polypeptide, enzyme, pearl powder and other inorganic salt additives to improve the corresponding performance.
The preparation method of the soothing and refreshing toothpaste comprises the following steps:
(1) preparation of the first aqueous phase: adding sweetener and plant compound extract into solvent 30-60% of the total amount of the solvent, and stirring at 20-25 deg.C to dissolve completely;
(2) preparation of the second aqueous phase: adding foaming agent into the rest solvent, and stirring at 20-25 deg.C until completely dissolved;
(3) preparing colloid: mixing humectant and thickener, and stirring at 20-25 deg.C;
(4) adding the first water phase obtained in the step (1) into a stirring pot, slowly adding the colloid obtained in the step (3) into the stirring pot under a stirring state, and stirring until the mixture forms colloid;
(5) adding a friction agent into the colloid in the step (4), and stirring for 10-30 minutes in vacuum at the temperature of 20-25 ℃ to form paste;
(6) and (3) adding the second water phase obtained in the step (2), the probiotics and the efficacy agent into the paste in the step (5), and stirring for 10-30 minutes at 20-25 ℃ under vacuum.
The preparation method disclosed by the invention is simple in process, good in finished product stability, capable of effectively keeping the activity of various components, and capable of effectively reducing the production cost, and the energy consumption and time consumption are reduced compared with those of the traditional process.
Compared with the prior art, the invention has the beneficial effects that: the efficacy agent and the original abrasive of the toothpaste take effect synergistically, so that the toothpaste has good cleaning and whitening effects and also has very good repairing and whitening effects; the plant composite extract and the probiotics are added, so that the oral disease treatment bacteria such as streptococcus sobrinus, porphyromonas gingivalis, streptococcus mutans and fusobacterium nucleatum and the like can be effectively inhibited for a long time, and meanwhile, the oral disease treatment bacteria have an anti-inflammatory effect, can effectively assist in treating and preventing oral inflammation, keep fresh breath, eliminate halitosis and have good moistening and refreshing feeling; has good repairing effect on the damage of human gingival cells; has very good oral cavity moisturizing and other care effects.
Drawings
FIG. 1 is a graph of IL-1a release of an efficacy agent in skin cell irritation experiments;
FIG. 2 is a graph of experimental IL-1B release of an efficacy agent on human gingival cell stimulation;
FIG. 3 is a graph of experimental IL-6 release of an efficacy agent on human gingival cell stimulation;
fig. 4 is a graph of efficacy agent in human gingival cell repair experiments (PBS VS MH5 (efficacy agent));
fig. 5 is a consumer perception evaluation plot of a soothing fresh dentifrice of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings and the embodiments, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The comfortable and fresh toothpaste comprises a solvent, a humectant, an abrasive, a thickening agent, a foaming agent, a sweetening agent, probiotics and other additives.
Table 1 shows a soothing and refreshing toothpaste of examples 1-7
The preparation method of the soothing and refreshing toothpaste comprises the following steps:
(1) preparation of the first aqueous phase: adding sweetener and plant compound extract into solvent 50% of the total amount of the solvent, and stirring at room temperature to dissolve completely;
(2) preparation of the second aqueous phase: adding a foaming agent into the residual solvent, and stirring at the room temperature at the rotating speed of 100rmp until the foaming agent is completely dissolved;
(3) preparing colloid: mixing the humectant and the thickener, and stirring uniformly at the room temperature at the rotating speed of 100 rmp;
(4) adding the first water phase obtained in the step (1) into a stirring pot, slowly adding the colloid obtained in the step (3) into the stirring pot under the stirring state, and stirring at 100rmp until the mixture forms colloid;
(5) adding a friction agent into the colloid in the step (4), and stirring for 15 minutes at room temperature in vacuum at the rotating speed of 100 rmp;
(6) and (3) adding the second water phase obtained in the step (2), the probiotics and the efficacy agent into the paste in the step (5), and stirring for 15 minutes in vacuum at room temperature.
The preparation method disclosed by the invention is simple in process, good in finished product stability, capable of effectively keeping the activity of various components, and capable of effectively reducing the production cost, and the energy consumption and time consumption are reduced compared with those of the traditional process.
Example 8
The soothing and refreshing toothpaste is prepared from the following components in percentage by mass:
the preparation method of the soothing and refreshing toothpaste comprises the following steps:
1. preparation of the first aqueous phase: adding sodium fluoride, saccharin sodium and plant composite extract into deionized water with the formula amount of 50%, and stirring at room temperature until the sodium fluoride, saccharin sodium and plant composite extract are completely dissolved;
2. preparation of the second aqueous phase: adding sodium cocoyl methyl taurate into the rest 50% of deionized water, and stirring at room temperature until the sodium cocoyl methyl taurate is completely dissolved;
3. preparing colloid: mixing glycerol, sorbitol and polyethylene glycol, stirring, adding xanthan gum and sodium carboxymethylcellulose, and stirring at room temperature until the mixture is uniformly dispersed to form colloid;
4. adding the first water phase obtained in the step (1) into a stirring pot, slowly adding the colloid in the step (3) into the stirring pot under stirring, and stirring until the mixture forms uniform colloid;
5. adding thickening silica, silica and mica powder into the colloid in the step (4), and stirring for 15 minutes at room temperature under vacuum;
6. and (3) adding the efficacy agent, methyl hydroxybenzoate, LPC-37, essence and the second water phase obtained in the step (2) into the paste obtained in the step (5), and stirring for 15 minutes at room temperature under vacuum.
Example 9
The soothing and refreshing toothpaste is prepared from the following components in percentage by mass:
the preparation method of the soothing and refreshing toothpaste comprises the following steps:
1. preparation of the first aqueous phase: adding sodium fluoride, saccharin sodium and plant composite extract into deionized water with the formula amount of 50%, and stirring at room temperature until the sodium fluoride, saccharin sodium and plant composite extract are completely dissolved;
2. preparation of the second aqueous phase: adding sodium cocoyl methyl taurate into the rest 50% of deionized water, and stirring at room temperature until the sodium cocoyl methyl taurate is completely dissolved;
3. preparing colloid: mixing glycerol, sorbitol and polyethylene glycol, stirring, adding xanthan gum and sodium carboxymethylcellulose, and stirring at room temperature until the mixture is uniformly dispersed to form colloid;
4. adding the first water phase obtained in the step (1) into a stirring pot, slowly adding the colloid in the step (3) into the stirring pot under stirring, and stirring until the mixture forms uniform colloid;
5. adding thickening silica, silica and mica powder into the colloid in the step (4), and stirring for 15 minutes at room temperature under vacuum;
6. and (3) adding the efficacy agent, methyl hydroxybenzoate, LPC-37, essence and the second water phase obtained in the step (2) into the paste obtained in the step (5), and stirring for 15 minutes at room temperature under vacuum.
Example 10
The soothing and refreshing toothpaste is prepared from the following components in percentage by mass:
the preparation method of the soothing and refreshing toothpaste comprises the following steps:
1. preparation of the first aqueous phase: adding sodium fluoride and saccharin sodium into deionized water with the formula amount of 50%, and stirring at room temperature until the sodium fluoride and saccharin sodium are completely dissolved;
2. preparation of the second aqueous phase: adding PVM/MA copolymer into deionized water with the formula amount of 25%, and stirring at room temperature until the PVM/MA copolymer is completely dissolved;
3. preparation of the third aqueous phase: adding sodium cocoyl methyl taurate into the rest 25% of deionized water, and stirring at room temperature until the sodium cocoyl methyl taurate is completely dissolved;
4. preparing colloid: adding o-cymene-5-alcohol into polyethylene glycol, and stirring at room temperature until completely dissolved; then adding glycerol and sorbitol, and stirring uniformly; adding xanthan gum and sodium carboxymethylcellulose, and stirring at room temperature until the mixture is uniformly dispersed to form colloid;
5. adding the first water phase into the mixture in the stirring pot, and stirring uniformly at room temperature; then adding a second water phase, and stirring uniformly at room temperature; slowly adding the colloid in the step (3) into the mixture in the stirring pot under stirring, and stirring until the mixture forms colloid;
6. adding an efficacy agent, thickening silica, zinc citrate, silica and mica powder into the colloid in the step (5), and stirring for 15 minutes at room temperature under vacuum;
7. adding probiotics, methyl hydroxybenzoate, essence and a third water phase into the paste obtained in the step (6), and stirring for 15 minutes at room temperature under vacuum;
in the verification experiment of a positive control group of 2% SLS solution and an experimental group of 2% SLS solution added with 5% of efficacy agent, the result is shown in figure 1, and after the efficacy agent is added, the IL-1 α inflammation factor is inhibited by 50%.
Human gingival cells can release IL-1 β and IL-6 inflammatory factors under the stimulation of Lipopolysaccharide (LPS), under the same conditions, after 5% of the efficacy agent is added, as shown in figure 2, the inhibition on IL-1 β reaches 52.8%, as shown in figure 3, the release on the IL-6 inflammatory factors reaches 62.7%, and therefore the efficacy agent can play an anti-inflammatory role in the oral cavity.
The effective agent has repairing effect on injury of human gingival cells. In the human gingival cell experiment, human gingival cells were mechanically scratched, damaged gingival cells were treated with Phosphate Buffered Saline (PBS) and a solution containing 2% of an efficacy agent, respectively, and growth recovery of both groups of cells after 24 hours and 48 hours was observed with a microscope. As shown in fig. 4, after 48h of treatment with the efficacy agent, the damaged part was almost completely recovered, and the cell proliferation rate was much higher than that of the control group, indicating that the efficacy agent can significantly promote the proliferation of gingival cells, which is beneficial to the recovery of the damaged oral tissue to a healthy state. . The efficacy agent is used in toothpaste, and has the beneficial effect that the experimental results are basically consistent. In addition, the components of the efficacy agent are low in price, so that the formula cost can be effectively reduced.
The plant complex extract is shown in Table 2 below for examples 11-15.
The preparation method comprises the following steps:
(1) pretreating medicinal materials: weighing the traditional Chinese medicine raw materials of each component according to the formula dosage, crushing into 80 meshes, and uniformly mixing to obtain a medicinal material mixture;
(2) extraction: placing the mixture in a container, adding an extraction solvent 20 times the total weight of the mixture, soaking at 70 deg.C for 9 hr, treating with ultrasonic wave for 3 times (40 min each time) with the ultrasonic power of 800W, and collecting extractive solution;
(3) centrifuging: respectively removing the residues from the extractive solution by centrifuge at a speed of 12000r/min for 30 min;
(4) and (3) purification: filtering the extracting solution obtained in the step (3) by using a ceramic membrane with the aperture of 300nm to obtain a liquid medicine;
(5) concentration: concentrating the liquid medicine at 55 ℃ until the weight ratio of the liquid medicine to the Chinese medicinal material mixture in the step (1) is 2: 1.
Wherein the extraction solvent in the step (2) is deionized water, pure water, lower alcohol with carbon chains of C1-C4 or aqueous solution of lower alcohol with carbon chains of C1-C4 at a volume ratio concentration of 10-60%.
The preparation method of the plant composite extract has the advantages of simple process, low equipment requirement and low production cost, can effectively keep the activity of the active ingredients of the extract, and can finish extraction only by soaking once, so that the efficiency is greatly improved.
In the formula, the chamomile has the effects of resisting bacteria and diminishing inflammation, relieving gum and preventing decayed teeth; rhizoma Polygoni Cuspidati has effects of relieving inflammation and pain, treating dental caries, and treating oral ulcer; the liquorice has obvious proliferation inhibiting effect on streptococcus mutans and porphyromonas gingivalis; the Salvia officinalis has antibacterial, antiinflammatory and analgesic effects; the rosemary leaf has the effects of resisting bacteria and inflammation, treating dental ulcer and preventing gingivitis and dental plaque accumulation; centella asiatica has the effects of promoting fibroblast proliferation, resisting inflammation, resisting oral ulcer, preventing periodontitis and gingivitis, and repairing oral mucosa; the green tea has effects of inhibiting growth of Streptococcus mutans and Porphyromonas gingivalis in oral cavity, preventing dental caries, and preventing gingival and periodontal diseases; the tea is alkaline substance, and can inhibit calcium decrease and protect teeth; the tea polyphenol has the effects of sterilizing, cleaning tea saponin and removing halitosis; scutellariae radix has effects in resisting dental caries, gingivitis, periodontitis, oral ulcer, tooth sensitivity, and halitosis. The traditional Chinese medicine components adopt the concept of 'monarch, minister, assistant and guide' in traditional Chinese medicine and the specific preparation method of the application, so that the components take effect synergistically, and the traditional Chinese medicine has good effects of soothing and moistening, removing dental plaque, performing gum physiotherapy, inhibiting bacteria and resisting inflammation and refreshing breath. The prepared plant composite extract is used together with probiotics, so that the synergistic effect can be greatly improved, the growth of oral pathogenic bacteria can be effectively inhibited, the oral health is facilitated, and teeth are protected. Especially has long-term good inhibition effect on streptococcus mutans, streptococcus sobrinus and fusobacterium nucleatum in oral pathogens, can keep the oral cavity comfortable and fresh for a long time, and can eliminate halitosis.
Verification example 1 evaluation of moisturizing Effect
The moisturizing efficacy of the toothpaste with the added efficacy agent was evaluated by comparing the soothing and refreshing toothpaste of example 1 of the present invention with a control of a blank toothpaste of the same composition without the added efficacy agent. The experiment was a double blind experiment, 10 volunteers used the soothing and refreshing toothpaste of the present application, and another 10 volunteers used a control group toothpaste containing no efficacy agent, and the volunteers brushed for 2 minutes and then gargled, and after brushing (0Min), questionnaires were evaluated after brushing for 5 minutes (5Min) and 30 minutes (30 Min). The volunteers were rated from the degree of oral lubrication, the feeling of oral moistening and the amount of oral water according to the actual conditions, and 0 to 10 points of the standard, 0 points means dryness and 10 points means wetness. From the blind test results, it can be seen that after using the toothpaste containing the efficacy agent, the volunteers had more than 1-fold higher degree of oral lubrication, degree of wetness and amount of saliva than the control group using the toothpaste containing no efficacy agent, as shown in fig. 5.
Verification example 2 efficacy experiment for preventing dental calculus
The soothing fresh toothpaste is prepared into an aqueous solution with the concentration of 15%, a blank control group is arranged, the purpose of reducing calcium ions is achieved by adding the aqueous solution into a calcium chloride saturated solution in an experiment to form a complex precipitate, the precipitate is centrifuged to obtain a supernatant, 0.6% of ammonium diuranate indicator is used for developing color, then an absorbance value A506 of the supernatant is measured at 506nm by a 721 type spectrophotometer, the content of residual calcium ions in the solution is compared, and the results are shown in the following table:
the results show that the oral cavity moistening and refreshing toothpaste provided by the invention enables the calcium ion concentration to be reduced, and the oral cavity moistening and refreshing toothpaste provided by the invention can effectively prevent dental calculus. Tests have shown that other examples of soothing toothpaste have similar effects.
Experimental example 3 for confirming stain removing and color removing effects
The experimental method comprises the following steps: adding a high-concentration tooth stain source into hydroxyapatite powder, adsorbing under a certain condition, simulating the formation of tooth stains in an oral cavity, adding the soothing fresh toothpaste, and quantitatively evaluating the stain removal effect of the extract by comparing the absorbance values before and after comparison, wherein the results are shown in the following table:
the result shows that the moisturizing refreshing toothpaste has obvious stain removal rate, and the moisturizing refreshing toothpaste can effectively remove the stains. Tests have shown that other embodiments of soothing and refreshing toothpastes also have similar effects.
Verification example 4 bacteriostatic experiment
The antibacterial effect of the soothing fresh toothpaste obtained in example 5 of the invention is determined by referring to the experimental method in the 7.5 antibacterial ring method of the evaluation method of antibacterial and bacteriostatic effects of the QBT 2738-:
the result shows that the moistening and refreshing toothpaste has the antibacterial effect. Tests have shown that other embodiments of soothing and refreshing toothpastes also have similar effects.
Verification example 5 anti-adhesion experiment
Preparing a streptococcus mutans bacterial suspension, adjusting the concentration of viable bacteria contained in the bacterial suspension to about 1 × 108cfu/ml, taking 50 mul of the soothing fresh toothpaste stock solution of example 5 of the invention, adding the fresh toothpaste stock solution into a beef soup culture medium, and gradually diluting the fresh toothpaste stock solution in a duplicate way to be 1: 100, 3: 100 and 5: 100 times.
Adding a certain amount of calf serum and bacterial suspension into the culture medium respectively, placing a glass rod and a glass slide with fixed length and diameter after autoclaving into each test tube, placing the test tubes into a candle jar according to the mark A, B, C when the concentration of the culture medium is high to low, and carrying out anaerobic culture at 37 ℃ for 24 h.
The same amount of liquid culture medium without the soothing and refreshing toothpaste of example 8 was added with calf serum and bacterial suspension and glass rods and slides as the above steps, and cultured for 24h simultaneously as a positive control.
And taking the liquid culture medium which is not added with the soothing fresh toothpaste and the bacteria liquid in the same amount, adding the same calf serum, the glass rod and the glass slide, and culturing for 24 hours as a negative control.
And (3) taking out the glass rod after anaerobic culture for 24h, scraping bacteria attached to the glass rod into a test tube containing 3ml of physiological saline, centrifuging the culture solution, removing supernatant, adding 3ml of physiological saline into sediment at the bottom of the tube, respectively measuring OD600 values, and calculating the attachment percentage according to a formula:
the percentage of attached bacteria OD/(attached bacteria OD + unattached bacteria OD) × 100%
The measurement results are shown below:
the result shows that the addition of the refreshing toothpaste can effectively reduce the adhesion amount of streptococcus mutans on the glass rod, and the refreshing toothpaste is proved to have the anti-adhesion effect. Tests have shown that other examples of soothing toothpaste have similar effects.
Verification example 6 clinical test of the finished product
40 patients with exogenously stained teeth (patients without other dental history and healthy) were taken out of hospital and randomized into two groups, one group was experimental and the other was control, 20 patients each. The patient diet was strictly controlled during the experiment as was the case with the experimental differences due to the exogenous pigment introduction, and the teeth were brushed with the same amount of the soothing fresh toothpaste of example 9 in the morning and evening without using other oral products in addition to this, with an experimental period of 4 months. The patient's tooth stains are detected before and after treatment and are evaluated using the Lobene stain index, which uses numbers from 0 to 3 to evaluate the size of the stained portion and the extent of the stain. The Lobene stain index rating and scoring criteria are shown in the following table:
the tooth surfaces are the anterior labial lips of the mandible, the lingual surfaces and the labial surfaces of the anterior maxillary teeth.
The mean stain score for each patient was the area score mean and the extent score mean. The area scoring average is the color spot area scoring/total number of tooth surfaces to be inspected; the average degree score is the mottle degree score/total number of teeth examined, and the results are shown in the following table:
the results show that the control group and the experimental group have significant difference, and the effect of dissolving the color spots and the dental plaques by using the soothing and refreshing toothpaste disclosed by the invention for tooth brushing is proved to be certain. Tests have shown that other examples of soothing toothpaste have similar effects.
Validation example 7 evaluation of efficacy of removal of exogenous color plates
Basis of examination
GQT/ZY-HJ-A-9 & lt & ltevaluation and examination rules for removing exogenous color spots by toothpaste & gt
Test method
Preparing an enamel sample: the removed incisors are cut into enamel blocks of about 5mm by 5mm in size, embedded in, for example, polymethylmethacrylate resin. And (3) polishing the lip surface of the enamel by using 180-mesh abrasive paper wetted by water, and polishing the enamel surface with an arc structure to be flat. After rinsing the samples with water, the enamel surfaces were polished smooth with water-wet 600 mesh sandpaper and rinsed with deionized water in an ultrasonic bath for 15 minutes.
Acid etching: immersing the enamel block into 1% hydrochloric acid, stirring for 1 minute, taking out, and sucking the residual liquid with a paper towel; then soaking the mixture into a saturated sodium carbonate solution, stirring for 1 minute, taking out the mixture, and then sucking the residual liquid with a paper towel; finally, the mixture was immersed in a 1% phytic acid solution, stirred for 1 minute, and taken out, and the remaining liquid was blotted with a paper towel.
Staining of enamel specimens: (1) the dyeing liquid comprises the following components: 4.0g/L coffee, 4.0g/L black tea, 2.5g/L gastric mucin, 4.0g/L soy sauce, 0.05g/LFeCl3. (2) Preparing a dyeing solution: first, a gastric mucin solution (deionized water is used) is prepared, the components of the staining solution are added, and the mixture is cooled. FeCl of 0.05g/L stored in 4 is added in an amount of 10mL/L before use3And (3) solution. And (4) putting the acid-etched enamel block into a dyeing machine for dyeing, and continuously dyeing for 12d.
Measurement of color of stained tooth enamel specimens: the stained enamel blocks were numbered and marked and the color of the enamel (L x) was measured with a colorimeterBefore brushing teeth) Selecting enamel blocks with L value of 30-50, randomly distributing the enamel blocks to a sample group, a blank control group and a competitive product control group, wherein each group comprises 8 blocks, and performing brushing treatment by using a test object, a blank control object and a competitive product control object respectively. The competitive product control group is one of the most popular similar products in the market at present.
Simulating a tooth brushing process: (1) example 1 preparation of a test toothpaste slurry: weighing a certain weight of toothpaste to be tested and deionized water according to the proportion of 1:16 (toothpaste: water), stirring with a glass rod to disperse the toothpaste, and stirring with a magnetic stirrer to form homogenate for later use. Control toothpaste slurries were prepared as described above. (2) And (3) placing the enamel block into a sample fixing groove of an automatic mechanical tooth brushing machine for fixing, enabling the enamel block to be higher by about 2cm, and screwing down screws to fix the enamel block. The toothbrush head was mounted so that the bristles vertically contacted the enamel surface, the total weight of the toothbrush head and post was 150 g. Weighing about 70g of sample to be tested, homogenizing, adding into a grinding fluid bottle, fixing the grinding fluid bottle on a tooth brushing machine, enabling the toothpaste slurry to bury the enamel sample, and brushing the teeth repeatedly for 800 times. After the tooth brushing is finished, taking out the enamel sample from the tooth brushing machine, washing the enamel sample by water, sucking dry water by a paper towel, and drying the enamel sample.
Determination of enamel color L after tooth brushingAfter brushing teeth
Calculating the difference value △ L between the values before and after brushing
△L*＝L*After brushing teeth-L*Before brushing teeth
The evaluation method is that the SPSS20.0 system software is adopted, independent samples are subjected to t test, and if the value of △ L of a sample group is larger than that of △ L of a control group, and the comparison of the values of △ L of the two groups has statistical significance (P is less than 0.05), the tested substance is considered to have whitening efficacy.
The experimental data and statistical results are shown in the following table:
the test article is considered to be effective in removing extrinsic stains in enamel caused by coffee, black tea, gastric mucin, soy sauce, and the like, because Δ L values significantly differ between the two groups (P < 0.05).
Compared with the competitive product control group toothpaste, the delta L value of the multiple whitening toothpaste is smaller than that of the control group, and the delta L values between the two groups have no significant difference (P is larger than 0.05), so that the effect of the test product is equivalent to that of the competitive product control product.
Verification example 8 evaluation of bacteriostatic Effect
Evaluation basis and method: QB/T2738-2012(7.3)
The sample of example 8 was selected as such.
The results of the bacteriostatic test on Porphyromonas gingivalis are shown in the following table:
the results of the bacteriostatic test on the streptococcus mutans are shown in the following table:
the results of the test for the inhibition of F.nucleatum are shown in the following table:
through the test results, the invention has the advantages that the invention can effectively inhibit the growth of porphyromonas gingivalis, streptococcus mutans and fusobacterium nucleatum, is beneficial to good oral health and protects teeth; can effectively clean the oral cavity, keep the oral cavity fresh and avoid other diseases. Can keep the oral cavity smooth and fresh for a long time and eliminate halitosis. Other embodiments of the present application also have substantially the same effects.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention should not be limited thereby, and all the simple equivalent changes and modifications made in the claims and the description of the present invention are within the scope of the present invention.
Claims (9)
1. The soothing and refreshing toothpaste is characterized by comprising the following components in parts by weight:
the efficacy agent is prepared from the following components in parts by weight:
the plant composite extract is prepared from the following traditional Chinese medicine components in parts by weight:
2. the soothing and refreshing toothpaste as claimed in claim 1, which comprises the following components in parts by weight:
3. the soothing and refreshing toothpaste as claimed in claim 2, wherein the efficacy agent is prepared from the following components in parts by weight:
4. the soothing and refreshing toothpaste according to claim 4, wherein the efficacy agent is prepared from the following components in parts by weight:
5. a soothing and refreshing toothpaste according to claim 1, wherein said solvents include but are not limited to water, deionized water, purified water and edible ethanol; the humectants include, but are not limited to, sorbitol, propylene glycol, glycerin, and polyethylene glycol; the abrasives include, but are not limited to, silica, calcium carbonate, calcium phosphate, sodium bicarbonate, kaolin, and cellulose; such thickeners include, but are not limited to, xanthan gum, sodium carboxymethylcellulose, sodium carboxyethyl cellulose, carbomer, silicon dioxide, guar gum, carrageenan, polyvinylpyrrolidone, and PVM/MA copolymer; such foaming agents include, but are not limited to, sodium lauryl sulfate, sodium methylcocoyl taurate, sodium cocoyl glutamate, sodium lauroyl glutamate, and cocoamidopropyl betaine; such sweeteners include, but are not limited to, saccharin sodium, sucralose, and erythritol.
6. A soothing and refreshing toothpaste as claimed in claim 1, wherein said perlite has a particle size in the range of 15-25 microns and said abrasive has a particle size in the range of 0.5-10 microns.
7. The soothing and refreshing toothpaste according to claim 1, wherein the preparation method of the plant composite extract comprises the following steps:
(1) pretreating medicinal materials: weighing the traditional Chinese medicine raw materials of each component according to the formula dosage, crushing into 10-100 meshes, and mixing uniformly to obtain a medicinal material mixture;
(2) extraction: placing the medicinal material mixture into a container, adding an extraction solvent which is 10-30 times of the total weight of the medicinal material mixture, soaking for 8-10 hours, treating for 2-4 times by ultrasonic waves at 60-75 ℃ for 30-50min each time, wherein the ultrasonic power is 700-;
(3) centrifuging: removing dregs of the extract by a centrifugal machine, wherein the speed of the centrifugal machine is 11000-13000 r/min, and the treatment time is 20-40 min;
(4) and (3) purification: filtering and centrifuging the extracting solution obtained in the step (3) by using a ceramic membrane with the aperture of 200-400 nm to obtain a liquid medicine;
(5) concentration: concentrating the liquid medicine until the weight ratio of the liquid medicine to the Chinese medicinal material mixture in the step (1) is 1: 1-3: 1.
8. The soothing and refreshing toothpaste as claimed in claim 7, wherein the extraction solvent in step (2) is deionized water, pure water, lower alcohol with carbon chain of C1-C4, and aqueous solution of lower alcohol with carbon chain of C1-C4 at a volume concentration of 10-60%; adding an extraction solvent 15-25 times the total weight of the medicinal material mixture, soaking for 9 hours, and treating for 2-3 times with ultrasonic waves of 750 and 850W at 65-70 ℃ for 35-45min each time.
9. A method of making a soothing fresh toothpaste according to claim 1 comprising the steps of:
(1) preparation of the first aqueous phase: adding sweetener and plant compound extract into solvent 30-60% of the total amount of the solvent, and stirring at 20-25 deg.C to dissolve completely;
(2) preparation of the second aqueous phase: adding foaming agent into the rest solvent, and stirring at 20-25 deg.C until completely dissolved;
(3) preparing colloid: mixing humectant and thickener, and stirring at 20-25 deg.C;
(4) adding the first water phase obtained in the step (1) into a stirring pot, slowly adding the colloid obtained in the step (3) into the stirring pot under a stirring state, and stirring until the mixture forms colloid;
(5) adding a friction agent into the colloid in the step (4), and stirring for 10-30 minutes in vacuum at the temperature of 20-25 ℃ to form paste;
(6) and (3) adding the second water phase obtained in the step (2), the probiotics and the efficacy agent into the paste in the step (5), and stirring for 10-30 minutes at 20-25 ℃ under vacuum.
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| CN116898741A (en) * | 2023-08-18 | 2023-10-20 | 广州品硬生物科技有限公司 | Gum restoration toothpaste containing lysozyme and probiotics and preparation method thereof |
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