Gingiva protecting and bleeding stopping toothpaste and preparation method thereof

Abstract

The invention discloses gum-protecting and bleeding-stopping toothpaste and a preparation method thereof. The gingiva-protecting and bleeding-stopping toothpaste comprises the following components in percentage by weight: 0.0001-0.2% of fibronectin, 0.0001-0.2% of sodium alginate, 0.0001- 0.01%-1% of a pseudo-ginseng extract; 0.01%-1% of a rhizoma bletillae extract; 31%-70% of a humectant; 0.1%-3% of a thickening agent; 5%-30% of a friction agent; 0.3 to 5% of a surfactant; and the balance water. According to the gingiva-protecting and bleeding-stopping toothpaste disclosed by the invention, the fibronectin, the rhizoma bletillae extract and the radix notoginseng extract are added and have a synergistic effect, so that the gingiva-protecting and bleeding-stopping toothpaste has a remarkable gingiva-protecting and bleeding-stopping effect, and can be used for effectively improving the problems of gingival bleeding and oral inflammation and achieving the effects of easing pain and diminishing swelling.

Description

Technical Field

[0001] The invention relates to the technical field of oral care, and in particular to a gum protecting and hemostatic toothpaste and a preparation method thereof. Background Art

[0002] Bleeding gums are one of the common symptoms of oral diseases. They refer to a small amount of bleeding gums that occurs spontaneously or due to minor irritation. In mild cases, there will be blood in the saliva only when sucking, brushing teeth, or chewing hard food. In severe cases, the gums will bleed more or even spontaneously when they are slightly stimulated. Generally speaking, gingivitis or periodontitis is the most common cause of bleeding gums. When the gums are acutely or chronically inflamed, the gums will become congested and edematous, and the capillaries in the gums will dilate and proliferate. At this time, when brushing teeth, touching or chewing food, the capillaries are prone to rupture and bleeding gums will occur. According to the data from the "Fourth National Oral Health Epidemiology" survey report, the detection rate of gum bleeding is: 87.4% in the 35-44 age group, with an average of 13.77 teeth with bleeding gums per person; 88.45% in the 55-64 age group, with an average of 13.87 teeth with bleeding gums per person; 72.6% in the 65-74 age group, with an average of 11.25 teeth with bleeding gums per person. Gum bleeding is often accompanied by bad breath, which will affect work and social activities to a certain extent, and may even bring mental burden to patients. Studies have shown that if gum bleeding is not treated in time and bleeding frequently, it may be prone to many complications, such as chronic anemia. Therefore, sufficient attention should be paid to the problem of gum bleeding.

[0003] At present, the most important measure for gum bleeding is prevention. Developing good oral hygiene habits can effectively reduce the risk of gum bleeding. Using oral care products that protect gums and stop bleeding (such as toothpaste) is an important auxiliary means in daily oral care.

[0004] In recent years, the toothpaste industry has developed towards specialization, providing professional solutions for different dental problems, reflecting the continued upgrading of consumers' attention to oral health. At present, there are many gum-protecting and hemostatic toothpaste products on the market, but their gum-protecting and hemostatic effects vary. Some of them have drug resistance problems and are not suitable for long-term use. There are not many options for consumers, and gum protection technology is difficult to upgrade. Therefore, it is urgent to develop an oral care product that can effectively improve gum bleeding and oral inflammation problems to meet consumers' daily oral care needs. Summary of the invention

[0005] In view of this, the purpose of the present invention is to provide a gum protecting and hemostatic toothpaste, which can effectively improve the problems of gum bleeding and oral inflammation and achieve the effect of analgesia and swelling reduction.

[0006] The present invention is achieved through the following technical solutions:

[0007] A gum protecting and hemostatic toothpaste, comprising the following components by weight percentage:

[0008] Fibronectin 0.0001%-0.2%;

[0009] Panax notoginseng extract 0.01%-1%;

[0010] Bletilla striata extract 0.01%-1%;

[0011] Moisturizer 31%-70%;

[0012] Thickener 0.1%-3%;

[0013] Friction agent 5%-30%;

[0014] Surfactant 0.3-5%;

[0015] Water balance.

[0016] The fibronectin described in the present invention, namely fibronectin (Fn), is a high molecular weight glycoprotein in the extracellular matrix.

[0017] The gum protecting and hemostatic toothpaste of the present invention is prepared by adding fibronectin, Bletilla striata extract and Panax notoginseng extract, which have synergistic effects. The Bletilla striata extract and Panax notoginseng extract promote the conversion of fibrinogen into insoluble fibrin by activating platelets and activating thrombin. The fibronectin is effectively cross-linked with the fibrin at the "core" of the hemostatic plaque to promote platelet aggregation, thereby achieving the effect of rapid hemostasis. The toothpaste of the present invention can effectively improve the problems of gum bleeding and oral inflammation when used, and achieve the effects of analgesia and swelling reduction.

[0018] Preferably, the weight ratio of fibronectin, Bletilla striata extract and Panax notoginseng extract is 1:(1-5000):(1-1000); more preferably 1:(2-400):(1-120); and even more preferably 1:(4-200):(1-40). When the ratio of fibronectin or Panax notoginseng extract is too high, while the fibronectin in the "core" of the thrombus is covalently linked to fibrin, the non-fibrin on the periphery of the thrombus will be linked to the fibronectin, inhibiting the further growth of the thrombus, preventing vascular occlusion, and maintaining the blood supply to downstream tissues and organs, which in turn affects the hemostatic effect.

[0019] Preferably, the weight content of Bletilla striata polysaccharide in the Bletilla striata extract of the present invention is 1.94%-2.2%, and the weight average molecular weight of the Bletilla striata polysaccharide is 1000DA-30KDA.

[0020] The Bletilla striata extract of the present invention can be obtained by commercial purchase or homemade. As a preferred embodiment, the present invention provides a preparation method of the Bletilla striata extract, comprising the following steps: soaking the Bletilla striata tuber raw material in 45-55°C water for 4-5h, the solid-liquid ratio is 1: (6-40), after crushing, ultrasonic extraction is performed at a temperature of 55-65°C for 50-80min, wherein the ultrasonic power is 120-450w, and then water and ethanol are added (preferably, based on the mass of the Bletilla striata tuber raw material as 1 part by mass, 6-40 parts by mass of ethanol are added, and the ratio of ethanol to water is 1: 1), reflux extraction at 55-65°C for 120-150min, filtering, collecting the filtrate, and adding 80-90°C hot water to the filter residue for extraction again, the liquid-to-solid ratio is 1: (45-50), ultrasonic extraction for 50-70min, filtering, collecting the filtrate, combining the filtrate, concentrating the obtained filtrate at a temperature of 85-95°C, filtering and collecting the filtrate for high-pressure sterilization, and obtaining the Bletilla striata extract. The filtration may be performed using a 1 μm filter membrane; after the filtrate is sterilized, a preservative and water may be added to prepare a Bletilla striata extract. Preferably, the Bletilla striata tuber raw material is a dried Bletilla striata tuber. More preferably, the Bletilla striata tuber raw material is free of wormholes, mildew, and uniform in size.

[0021] As a preferred embodiment, the drying method of Bletilla striata tubers includes the following steps: after digging up the Bletilla striata tubers, the fibrous roots are removed, washed, boiled or steamed in boiling water until there is no white core, then dried in the sun until half dry, the outer skin is removed, and further dried in the sun to obtain a dry Bletilla striata tuber raw material.

[0022] Preferably, the weight content of total notoginseng saponins in the notoginseng extract of the present invention is not less than 75%.

[0023] The Panax notoginseng extract of the present invention can be obtained by commercial purchase or homemade. As a preferred embodiment, the present invention provides a preparation method of the Panax notoginseng extract, comprising the following steps: after the Panax notoginseng raw material is crushed, 70%-75% ethanol is added, the solid-liquid ratio is 1: (12-15), reflux extraction is performed at a temperature of 60-70°C for 40-60 minutes, concentrated by freeze drying to obtain a concentrated extract, dissolved in water, filtered, 80% ethanol is added to the filtrate, and then concentrated by adsorption resin to obtain a second concentrated extract, then water and 90-95% ethanol are added to dissolve, then activated carbon is added for decolorization, and then a filtrate is obtained by filtering with a titanium rod, refined and concentrated to obtain an extract, the extract is vacuum dried, crushed into fine powder, sieved, and the Panax notoginseng extract is obtained.

[0024] The adsorption resin is preferably D101 macroporous adsorption resin, which is washed with water until the effluent is colorless, then eluted with 50% ethanol, and the elution endpoint is checked by TLC to obtain a second concentrated extract.

[0025] Preferably, the raw material of Panax notoginseng is dried rhizomes of Panax notoginseng, and more preferably, the raw material of Panax notoginseng rhizomes is free of wormholes, mildew and uniform in size.

[0026] As a preferred embodiment, the drying method of Panax notoginseng rhizomes comprises the following steps:

[0027] Take fresh Panax notoginseng roots, wash them, remove the rhizomes and fibrous roots, keep the main root, then cut the main root into two halves, and then freeze-dry (-60-50°C, -0.32-0.36MPa) for 1-4 days until the moisture mass fraction is less than 10%.

[0028] Preferably, the moisturizer is selected from any one or more of sorbitol, glycerol, and PEG-400.

[0029] Preferably, the thickener is selected from any one or more of carrageenan, xanthan gum, and hydroxymethyl cellulose gum.

[0030] Preferably, the friction agent is selected from any one or more of silicon dioxide (hydrated silica) and calcium carbonate.

[0031] Preferably, the surfactant is selected from any one or more of K12, sodium lauroyl sarcosinate, and cocamidopropyl betaine.

[0032] Preferably, the gum protecting and hemostatic toothpaste of the present invention further comprises, by weight percentage: 0.01-1.0% sweetener; 0.1-2% flavor; 0-0.5% preservative; 0.01-0.5% dipotassium glycyrrhizinate; 0.05-0.33% sodium fluoride; 0-2.0% crystalline sodium pyrophosphate; 0-0.5% titanium dioxide; and 0-0.5% cooling agent.

[0033] Preferably, the sweetener is selected from any one or more of saccharin sodium, sucralose, and stevioside;

[0034] The present invention also provides a method for preparing the gum protecting and hemostatic toothpaste, comprising the following steps: according to the proportion,

[0035] S1: dissolving fibronectin, Panax notoginseng extract, Bletilla striata extract, and moisturizer in water to form a solution;

[0036] If sweeteners, dipotassium glycyrrhizinate, sodium fluoride, crystalline sodium pyrophosphate or preservative components are included, they are all added in step S1 to prepare a solution;

[0037] If titanium dioxide is included, it is added after the solution is prepared in step S1 and dispersed evenly;

[0038] S2: Mix the abrasive and thickener evenly, add them into the solution in S1, and stir them evenly in a vacuum to form a paste; thus, a gum protecting and hemostatic toothpaste is prepared;

[0039] If the surfactant includes K12 component, mix K12 with the abrasive and thickener evenly;

[0040] S3: adding a surfactant to the paste formed in step S2, and stirring evenly under vacuum to prepare a gum protecting and hemostatic toothpaste;

[0041] If essence and cooling agent components are included, the cooling agent is dissolved in the essence, and then added to the paste formed in step S2 together with the surfactant, and vacuum stirred evenly to prepare a gum protecting and hemostatic toothpaste.

[0042] The present invention has the following beneficial effects:

[0043] The gum protecting and hemostatic toothpaste of the present invention has significant gum protecting and hemostatic effects by adding fibronectin, Bletilla striata extract and Panax notoginseng extract. The three have a synergistic effect and can effectively improve gum bleeding and oral inflammation problems, achieve the effects of analgesia and swelling reduction, and meet people's daily oral care needs. DETAILED DESCRIPTION

[0044] In order to elaborate on the technical content, purpose and effect of the present invention, the technical solution of the present invention is clearly and completely described in combination with the implementation method below, but the described embodiment is only a part of the embodiment of the present invention. Based on the embodiment of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0045] The raw materials used in the embodiments of the present invention are described as follows, but are not limited to the following raw materials:

[0046] Fibronectin: Fibronectin from Qidian Biotechnology, 500 ppm fibronectin;

[0047] Bletilla striata extract: contains about 2% Bletilla striata polysaccharide (Bletilla striata gum), with a molecular weight of 1000DA-30KDA;

[0048] The method is as follows: after the tubers of Bletilla striata are dug, the fibrous roots are removed, washed, steamed in boiling water until there is no white core, then sun-dried until half-dried, the outer skin is removed, and then sun-dried to obtain a dried tuber material of Bletilla striata. Then, qualified tuber materials of Bletilla striata (no worm eyes, no mildew, and uniform size) are soaked in 50°C water for 4 hours, with a material-liquid ratio of 1:40, and after crushing, ultrasonic extraction is performed at a temperature of 60°C for 80 minutes, wherein the ultrasonic power is 450w, and then appropriate amounts of water and ethanol are added, reflux extraction is performed at 60°C for 120 minutes, filtered, the filtrate is collected, and the filter residue is added with 85°C hot water for extraction again, with a liquid-to-material ratio of 1:45, ultrasonic extraction is performed for 50 minutes, filtered, the filtrate is combined, the obtained filtrate is concentrated at a temperature of 85°C, filtered with a 1μm filter membrane, and sterilized by high pressure, and the filtrate is collected, and a preservative and water are added to obtain a Bletilla striata extract.

[0049] Panax notoginseng extract: the total saponin content of Panax notoginseng is more than 75%;

[0050] It is prepared by the following method: high-quality Panax notoginseng raw materials (consistent size, no worm eyes, no mildew) are screened from the dried roots and rhizomes of Panax notoginseng, crushed, added with 70% ethanol, the solid-liquid ratio is 1:12, reflux extraction is carried out at a temperature of 60°C for 50 minutes, concentrated by freeze-drying to obtain a concentrated extract, dissolved in water, filtered, 80% ethanol is added to the filtrate, D101 macroporous adsorption resin is used, washed with water until the effluent is colorless, eluted with 50% ethanol, and the elution end point is checked by TLC to obtain a second concentrated extract, then water and 95% ethanol are added to dissolve, and then activated carbon is added for decolorization, and then a filtrate is obtained by filtering with a titanium rod, which is refined and concentrated to obtain an extract, the extract is vacuum dried, crushed into fine powder, sieved, and a Panax notoginseng extract is obtained.

[0051] Preparation method of toothpaste of embodiment and comparative example: according to the proportion in Table 1,

[0052] S1: dissolving the hemostatic composition, dipotassium glycyrrhizinate, sodium saccharin, sodium fluoride, sodium benzoate, PEG400, and sorbitol in water to form a solution, and then adding titanium dioxide to disperse evenly;

[0053] S2: Mix hydrated silica, thickener and K12 evenly, add the solution in S1, stir evenly in a vacuum to form a paste;

[0054] S3: dissolving the cooling agent with essence, and adding it and sodium lauroyl sarcosinate into the paste of S2, stirring evenly under vacuum, to prepare a gum protecting and hemostatic toothpaste containing the hemostatic composition.

[0055] Table 1 Component formula of toothpaste of Examples 1-7 and Comparative Examples 1-9 (wt%)

[0056]

[0057] Connect to Table 1

[0058]

[0059] Connect to Table 1

[0060]

[0061]

[0062] 1. Hemostasis test verification

[0063] The toothpastes prepared in Examples 1-7 and Comparative Examples 1-9 were taken as experimental samples.

[0064] 160 New Zealand rabbits that passed the quarantine, weighing 2.0kg to 2.5kg, female, were divided into 16 groups on average. 30mg / kg of 3% sodium pentobarbital was slowly injected through the ear vein. After the rabbits were anesthetized successfully, the abdomen was opened layer by layer to expose the liver. A 1cm*1cm*3cm wound was clamped at the lower edge of the left lobe of the liver in the same part of each animal. After the blood filled the wound, 1.0g of the test sample was immediately applied to the entire wound, covered with gauze, and a 50g weight was used to apply pressure on the gauze to observe the hemostatic effect. The bleeding of the wound was observed every 30s, and the filter paper strip was gently dipped and absorbed until the blood stopped oozing out, that is, there was no blood on the filter paper strip, and the required time was recorded as the bleeding time. If the bleeding has not stopped for more than 12min, press to stop the bleeding, and the bleeding time is counted as 12min. The animals were euthanized after the experiment. Statistical analysis, experimental data are expressed as mean ± standard deviation The experimental results are shown in Table 2 below.

[0065] Table 2 Hemostatic effect data of Examples 1-7 and Comparative Examples 1-9

[0066]

[0067]

[0068] 2. Verification of anti-inflammatory effect

[0069] The toothpastes prepared in Example 1-7 and Comparative Example 1-9 were used to conduct an experiment on the effect of p-xylene on the ear swelling of mice to study their anti-inflammatory effects. The deionized water and dexamethasone sodium phosphate injection group were used as the control group.

[0070] 160 SPF KM mice that passed the quarantine were randomly divided into 10 groups, 16 mice in each group, SPF KM mice, 18-22g, male. After the mice were quarantined and grouped, the left ear was not treated as the background value, and 30μL of xylene solution was applied to the inside and outside of the right ear. After 30min, except for the model control group, 0.1g of sample was applied to both sides of the right ear of the mice in the test sample group, and 50μL of dexamethasone sodium phosphate injection was applied to the dexamethasone sodium phosphate injection group. The injection was applied for the second time 30min later. After 1h of sample application, the mouse eyeball was removed to collect blood, and the mice were killed by cervical dislocation, the samples were wiped clean, the ears were cut off, and the ear pieces with a diameter of 8mm (the same part of the left and right ears) were weighed and recorded. The weight difference between the left and right ears of the same animal is the swelling degree.

[0071] Swelling degree = weight of right ear piece - weight of left ear piece

[0072] Swelling inhibition rate = (average swelling degree of model control group - average swelling degree of treatment group) / average swelling degree of model control group * 100%)

[0073] The test results are shown in Table 3 below.

[0074] Table 3 Anti-inflammatory effect data of Examples 1-7 and Comparative Examples 1-9

[0075] Group Ear swelling (mg) Ear swelling inhibition rate (%) Model control group 21.3±3.7 - Example 1 9.8±2.5 53.99 Example 2 7.2±3.3 66.20 Example 3 12.1±5.0 43.19 Example 4 10.5±2.0 50.70 Example 5 9.2±2.6 56.80 Example 6 10.7±2.3 49.77 Example 7 12.6±3.1 40.85 Comparative Example 1 11.6±2.7 45.54 Comparative Example 2 11.3±3.3 16.94 Comparative Example 3 9.4±3.2 55.87 Comparative Example 4 10.9±4.0 48.83 Comparative Example 5 13.4±3.2 37.09 Comparative Example 6 17.0±3.4 20.19 Comparative Example 7 15.1±2.9 29.11 Comparative Example 8 14.1±2.5 33.80 Comparative Example 9 20.7±2.9 2.82 Dexamethasone sodium phosphate injection group 15.4±4.3 27.70

[0076] It can be seen from the above results that the gum protecting and hemostatic toothpaste of the present invention, by adding fibronectin, Bletilla striata extract and Panax notoginseng extract, has a synergistic effect of the three and has significant gum protecting and hemostatic effects. It can effectively improve gum bleeding and oral inflammation problems and achieve the effect of analgesia and swelling reduction.

[0077] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent transformations made using the specification of the present invention, or directly or indirectly applied in related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A gum protecting and hemostatic toothpaste, characterized in that: By weight percentage, it includes the following components: Fibronectin 0.0001%-0.2%; Panax notoginseng extract 0.01%-1%; Bletilla striata extract 0.01%-1%; Moisturizer 31%-70%; Thickener 0.1%-3%; Friction agent 5%-30%; Surfactant 0.3-5%; Water balance.

2. The gum protecting and hemostatic toothpaste according to claim 1, characterized in that: The weight ratio of the fibronectin, the Bletilla striata extract and the Panax notoginseng extract is 1:(1-5000):(1-1000).

3. The hemostatic composition according to claim 1, characterized in that The weight ratio of fibronectin, Bletilla striata extract and Panax notoginseng extract is 1:(2-400):(1-120).

4. The hemostatic composition according to claim 1, characterized in that The weight ratio of fibronectin, Bletilla striata extract and Panax notoginseng extract is 1:(4-200):(1-40).

5. The gum protecting and hemostatic toothpaste according to claim 1, characterized in that: The weight content of the bletilla striata polysaccharide in the bletilla striata extract is 1.94-2.2%, and the weight average molecular weight of the bletilla striata polysaccharide is 1000DA-30KDA; the weight content of the notoginseng total saponin in the notoginseng extract is not less than 75%.

6. The gum protecting and hemostatic toothpaste according to claim 1, characterized in that: The preparation method of the bletilla striata extract comprises the following steps: soaking the bletilla striata tuber raw material in 45-55°C water for 4-5h, with a solid-liquid ratio of 1:(6-40), crushing, performing ultrasonic extraction at a temperature of 55-65°C for 50-80min, wherein the ultrasonic power is 120-450w, then adding water and ethanol, reflux extraction at 55-65°C for 120-150min, filtering, collecting the filtrate, and adding 80-90°C hot water to the filter residue for extraction again, with a liquid-to-solid ratio of 1:(45-50), ultrasonic extraction for 50-70min, filtering, collecting the filtrate, combining the filtrate, concentrating the obtained filtrate at a temperature of 85-95°C, filtering and collecting the filtrate for high-pressure sterilization, and obtaining the bletilla striata extract.

7. The gum protecting and hemostatic toothpaste according to claim 1, characterized in that: The preparation method of the Panax notoginseng extract comprises the following steps: crushing the Panax notoginseng raw material, adding 70%-75% ethanol, the solid-liquid ratio is 1:(12-15), reflux extraction at a temperature of 60-70°C for 40-60min, concentrating by freeze drying to obtain a concentrated extract, adding water to dissolve, filtering, adding 80% ethanol to the filtrate, and then concentrating by adsorption resin to obtain a second concentrated extract, then adding water and 90-95% ethanol to dissolve, then adding activated carbon to decolorize, and then filtering with a titanium rod to obtain a filtrate, refining and concentrating to obtain an extract, vacuum drying the extract, crushing it into fine powder, sieving, and obtaining the Panax notoginseng extract.

8. The gum protecting and hemostatic toothpaste according to claim 1, characterized in that: The moisturizer is selected from any one or more of sorbitol, glycerin, and PEG-400; the thickener is selected from any one or more of carrageenan, xanthan gum, and hydroxymethyl cellulose gum; the abrasive is selected from any one or more of silicon dioxide and calcium carbonate; the surfactant is selected from any one or more of K12, sodium lauroyl sarcosinate, and cocamidopropyl betaine.

9. The gum protecting and hemostatic toothpaste according to claim 1, characterized in that: Calculated by weight percentage, it also includes: 0.01-1.0% sweetener; 0.1-2% flavor; 0-0.5% preservative; 0.01-0.5% dipotassium glycyrrhizinate; 0.05-0.33% sodium fluoride; 0-2.0% crystalline sodium pyrophosphate; 0-0.5% titanium dioxide; and 0-0.5% cooling agent.

10. The method for preparing the gum protecting and hemostatic toothpaste according to claims 1-8, characterized in that: The following steps are included: according to the ratio, S1: dissolving fibronectin, Panax notoginseng extract, Bletilla striata extract, and moisturizer in water to form a solution; If sweeteners, dipotassium glycyrrhizinate, sodium fluoride, crystalline sodium pyrophosphate or preservative components are included, they are all added in step S1 to prepare a solution; If titanium dioxide is included, it is added after the solution is prepared in step S1 and dispersed evenly; S2: Mix the abrasive and thickener evenly, add them into the solution in S1, and stir them evenly in a vacuum to form a paste; and prepare a gum protecting and hemostatic toothpaste; If the surfactant includes K12 component, mix K12 with the abrasive and thickener evenly; S3: adding a surfactant to the paste formed in step S2, and stirring evenly under vacuum to prepare a gum protecting and hemostatic toothpaste; If essence and cooling agent components are included, the cooling agent is dissolved in the essence, and then added to the paste formed in step S2 together with the surfactant, and vacuum stirred evenly to prepare a gum protecting and hemostatic toothpaste.

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