Bamboo leaf flavonoid toothpaste as well as preparation method and application thereof

Abstract

The invention relates to the technical field of toothpaste preparation, and particularly discloses bamboo leaf flavonoid toothpaste as well as a preparation method and application thereof. The bamboo leaf flavonoid toothpaste is prepared from the following raw materials in parts by weight: 26 to 30 parts of a wetting agent, 1.6 to 1.8 parts of a binding agent, 0.2 to 0.4 part of a sweetening agent, 20 to 24 parts of a friction agent, 1.2 to 1.6 parts of a surfactant, 0.3 to 0.5 part of a pH (Potential of Hydrogen) regulator, 2.4 to 2.8 parts of active microcapsules, 0.4 to 0.6 part of essence and 14 to 18 parts of de-ionized water. A core material of the active microcapsule is a nano-dispersion, a wall material of the active microcapsule is prepared from Arabic gum and chitosan through a complex coacervation method, the nano-dispersion is prepared from xanthan gum, a bamboo leaf flavone extract, xylitol, calcium chloride and modified pectin through a reaction, and the modified pectin is prepared by mixing degreased pectin and chlorogenic acid according to a specific proportion. Through the synergistic effect of the substances, the dispersibility and antibacterial and anti-inflammatory performance of the bamboo leaf flavonoid toothpaste are improved.

Description

Technical Field

[0001] This invention relates to the field of toothpaste preparation technology, and more specifically, to a bamboo leaf flavonoid toothpaste, its preparation method, and its application. Background Technology

[0002] Bamboo leaf flavonoids are flavonoid preparations extracted from the leaves of plants in the genus *Phyllostachys*. The raw materials are abundant. The main components of bamboo leaf flavonoids are C-glycoside flavonoids, with characteristic components including vitexin, isovitexin, vitexin, and isovitexin. Studies have shown that bamboo leaf flavonoids possess antioxidant, tyrosinase-inhibiting, free radical scavenging, anti-radiation, antibacterial, and anti-inflammatory biological effects, and have potential application value in the food, health product, and daily chemical industries.

[0003] However, bamboo leaf flavonoids have poor water and fat solubility, resulting in poor dispersibility in toothpaste products, which severely limits their large-scale and efficient application.

[0004] Therefore, it is particularly important to provide a bamboo leaf flavonoid toothpaste with high solubility and excellent antibacterial and anti-inflammatory properties. Summary of the Invention

[0005] To address the problems mentioned in the background section, this invention provides a bamboo leaf flavonoid toothpaste, its preparation method, and its application.

[0006] One objective of this invention is to provide a bamboo leaf flavonoid toothpaste comprising the following ingredients by weight: 26-30 parts humectant, 1.6-1.8 parts binder, 0.2-0.4 parts sweetener, 20-24 parts abrasive, 1.2-1.6 parts surfactant, 0.3-0.5 parts pH adjuster, 2.4-2.8 parts active microcapsules, 0.4-0.6 parts fragrance, and 14-18 parts deionized water; The active microcapsules are first cross-linked from xanthan gum, bamboo leaf flavonoid extract, xylitol, and modified pectin to obtain a nano-dispersion, and then prepared by complex coagulation with gum arabic and chitosan as wall materials and the nano-dispersion as core material. The modified pectin is prepared by treating high-ester pectin with pectin methyl esterase solution under ultra-high pressure to obtain deesterified pectin, which is then mixed with chlorogenic acid.

[0007] Furthermore, the wetting agent is at least one of glycerin, sorbitol, and propylene glycol.

[0008] Furthermore, the binder is hydroxyethyl cellulose or methyl cellulose.

[0009] Furthermore, the sweetener is xylitol or steviol glycosides.

[0010] Furthermore, the abrasive is at least one of calcium hydrogen phosphate, aluminum hydroxide, and calcium pyrophosphate.

[0011] Furthermore, the surfactant is sodium lauroyl sarcosinate or sodium lauroyl glutamate.

[0012] Furthermore, the pH adjuster is a citrate-sodium citrate buffer solution.

[0013] Furthermore, the flavoring is peppermint or spearmint.

[0014] Furthermore, the active microcapsules are prepared by the following steps: Step A1: Add xanthan gum to deionized water and stir until homogeneous. While stirring, add dropwise a mixture of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution, and anhydrous ethanol. After the addition is complete, evaporate under reduced pressure and spray dry to obtain a nano-dispersion. In the above process, xanthan gum is used as a stabilizer, xylitol as a solubilizer, modified pectin as a carrier, and calcium chloride as a crosslinking agent. The nano-dispersion is prepared by spray drying. Step A2: Add gum arabic to deionized water, heat to 65-75℃, stir evenly, then add nano-dispersion, stir and react for 25-35 minutes, adjust pH to 5.8-6.2, add chitosan-acetic acid solution dropwise while stirring, after the addition is complete, continue stirring and reacting for 1.6-2.2 hours, centrifuge, wash, and dry to obtain active microcapsules.

[0015] Further, in step A1, the mass ratio of xanthan gum, deionized water, and the mixture is 0.04-0.06:50:20-30, and the mass ratio of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution, and anhydrous ethanol in the mixture is 1:3-5:0.36-0.42:6-10:50-60.

[0016] Furthermore, in step A1, the specific process parameters for vacuum rotary evaporation are: vacuum degree of -0.06MPa to -0.09MPa, temperature of 40-60℃, and time of 18-22min.

[0017] Furthermore, in step A1, the specific process parameters for spray drying are: inlet air temperature 90-100℃, outlet air temperature 65-75℃, atomizer speed 16000-20000rpm, and feed rate 3-5mL / min.

[0018] Further, in step A2, the mass ratio of gum arabic, deionized water, nano-dispersion, and chitosan-acetic acid solution is 1-2:60-80:4-5:22-24.

[0019] Further, in step A2, the chitosan-acetic acid solution is prepared by mixing chitosan and aqueous acetic acid at a mass ratio of 2-4:30 at a temperature of 50-60℃, and then filtering through a microporous membrane.

[0020] Furthermore, the mass fraction of the acetic acid aqueous solution is 1-2%.

[0021] Furthermore, the modified pectin is prepared by the following steps: Step B1: Add high-ester pectin to deionized water, heat to 40-50℃, keep warm for 6-10 minutes, adjust pH to 3.5-4.5, then add pectin methyl esterase solution, under nitrogen protection, use ultra-high pressure to assist enzymatic hydrolysis, inactivate enzyme, cool, precipitate, filter, wash, and dry to obtain deesterified pectin. Step B2: Add the deesterified pectin to a sodium bicarbonate aqueous solution, adjust the pH to 6-8, stir well, add chlorogenic acid and Tween-20, continue stirring for 36-40 minutes, and dry to obtain modified pectin. In the above process, the phenolic hydroxyl groups on the chlorogenic acid molecule can form a dense hydrogen bond network with the carboxyl and hydroxyl groups on the deesterified pectin chain, improving the dispersibility of the prepared modified pectin.

[0022] Further, in step B1, the mass ratio of high-ester pectin, deionized water, and pectin methylesterase solution is 1:90-110:0.02-0.04.

[0023] Furthermore, in step B1, the specific process parameters for ultra-high pressure treatment-assisted enzymatic hydrolysis are as follows: ultra-high pressure treatment-assisted enzymatic hydrolysis pressure is 350-440 MPa, ultra-high pressure treatment-assisted enzymatic hydrolysis temperature is 40-50℃, and ultra-high pressure treatment-assisted enzymatic hydrolysis time is 12-18 min.

[0024] Furthermore, in step B1, the enzyme inactivation temperature is 95-105℃, and the enzyme inactivation time is 18-22 min.

[0025] Further, in step B2, the mass ratio of deesterified pectin, sodium bicarbonate aqueous solution, chlorogenic acid and Tween-20 is 1:8-10:0.2-0.3:0.03-0.05.

[0026] Furthermore, in step B2, the mass fraction of the sodium bicarbonate aqueous solution is 0.6-1%.

[0027] The second objective of this invention is to provide a method for preparing the above-mentioned biological bamboo leaf flavonoid toothpaste, which is obtained by the following steps: The humectant, binder, sweetener and deionized water are mixed evenly. While stirring, the abrasive, surfactant, pH adjuster and active microcapsules are added in sequence. Stirring is continued for 22-26 minutes. Then the fragrance is added, homogenized, vacuum-foamed, discharged and filled to obtain bamboo leaf flavonoid toothpaste.

[0028] Furthermore, the homogenization process parameters are as follows: homogenization pressure is 94-98 MPa, homogenization temperature is 32-40℃, and homogenization time is 6-10 min.

[0029] Furthermore, the specific process parameters for the vacuum degassing are: vacuum degree of -0.03 to -0.08 MPa, temperature of 40-60℃, and time of 16-22 min.

[0030] A third objective of this invention is to provide the application of the bamboo leaf flavonoid toothpaste described above in the preparation of oral care products for antibacterial and anti-inflammatory purposes.

[0031] Compared with the prior art, the present invention has the following beneficial effects: To improve the dispersibility of bamboo leaf flavonoids and enhance the antibacterial and anti-inflammatory properties of the toothpaste prepared from them, this invention incorporates active microcapsules. The core material of the active microcapsules is a nano-dispersion, which is prepared by physical cross-linking of bamboo leaf flavonoid extract, xylitol, calcium chloride, and modified pectin. The modified pectin is prepared by mixing deesterified pectin and chlorogenic acid in a specific ratio. The chlorogenic acid in the modified pectin contains abundant phenolic hydroxyl groups and other functional groups, which can not only encapsulate the bamboo leaf flavonoid extract in a hydrophilic chlorogenic acid-deesterified pectin network structure through hydrogen bonding, thus improving the dispersibility of bamboo leaf flavonoids, but also exert antibacterial and anti-inflammatory effects by disrupting microbial membranes and inhibiting inflammatory factors, thereby enhancing the antibacterial and anti-inflammatory effects of the bamboo leaf flavonoid toothpaste. Xylitol... Not only can it prevent the aggregation of nano-dispersions through hydrogen bonding, further improving the dispersibility of bamboo leaf flavonoid toothpaste, but it can also inhibit cariogenic bacteria in the oral cavity, reduce the production of acidic substances, and improve the antibacterial and anti-inflammatory properties of bamboo leaf flavonoid toothpaste. Calcium chloride can undergo ionic cross-linking with the carboxyl groups in modified pectin to form a three-dimensional gel network structure, further improving the dispersibility of bamboo leaf flavonoid toothpaste. The wall material is prepared by complex coagulation of gum arabic and chitosan. Gum arabic and chitosan have good water solubility and are quickly dissolved during brushing, allowing the encapsulated nano-dispersions to be released in time to exert antibacterial and anti-inflammatory effects. Moreover, chitosan itself has excellent antibacterial properties and can synergistically enhance the antibacterial and anti-inflammatory properties of the prepared bamboo leaf flavonoid toothpaste with the nano-dispersions. Detailed Implementation

[0032] To make the embodiments of the present invention easier to understand, the present invention will be described in detail below with reference to specific embodiments. These embodiments are for illustrative purposes only and are not limited to the application scope of the present invention.

[0033] Where specific techniques or conditions are not specified in the examples, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.

[0034] Xanthan gum was purchased from Tianxin (Qingdao) Food Co., Ltd.; xylitol was purchased from Shandong Fangchang Biotechnology Co., Ltd., CAS No. 87-99-0; bamboo leaf flavonoid extract was purchased from Lanzhou Waterles Biotechnology Co., Ltd.; chitosan was purchased from Shaanxi Yuanyou Biotechnology Co., Ltd.; citric acid-sodium citrate buffer was purchased from Shanghai Yuanye Biotechnology Co., Ltd., pH 5.6; high-ester pectin was purchased from Quzhou Pectin Co., Ltd., with a degree of esterification of 61.83±0.62%; pectin methyl esterase was Novoshape pectin methyl esterase from Novozymes China, with an enzyme activity of 10 U / mL.

[0035] The present invention will be further described in detail below with reference to embodiments and comparative examples.

[0036] Examples 1-3 and Comparative Examples 1-4 provide a bamboo leaf flavonoid toothpaste and its preparation method.

[0037] Example 1 A bamboo leaf flavonoid toothpaste comprises the following ingredients in parts by weight: 26 parts glycerin, 1.6 parts hydroxyethyl cellulose, 0.2 parts xylitol, 20 parts dicalcium phosphate, 1.2 parts sodium lauroyl sarcosinate, 0.3 parts citrate-sodium citrate buffer, 2.4 parts active microcapsules, 0.4 parts peppermint flavoring, and 14 parts deionized water; The preparation method of bamboo leaf flavonoid toothpaste is as follows: Glycerin, hydroxyethyl cellulose, xylitol, and deionized water were stirred at 60 rpm for 16 minutes until homogeneous. While maintaining the stirring speed, dicalcium phosphate, sodium lauroyl sarcosinate, citrate-sodium citrate buffer, and active microcapsules were added sequentially. The stirring was continued for 22 minutes, followed by the addition of peppermint flavor. The stirring speed was maintained, and the mixture was homogenized at 94 MPa and 32°C for 6 minutes. Vacuum degassing was then performed, with the following process parameters: vacuum degree -0.03 MPa, temperature 60°C, and time 16 minutes. The mixture was then discharged, filled, and the bamboo leaf flavonoid toothpaste was obtained. The active microcapsules are prepared by the following steps: Step A1: Add xanthan gum to deionized water and stir at 500 rpm for 16 minutes until homogeneous. Maintaining the stirring speed, while continuously stirring, add a mixture of bamboo leaf flavonoid extract, xylitol, modified pectin, a 0.6% (w / w) calcium chloride aqueous solution, and anhydrous ethanol dropwise over 15 minutes at a rate of 3 drops / second. After addition, perform rotary evaporation under reduced pressure. The specific process parameters for rotary evaporation under reduced pressure are: vacuum degree -0.06 MPa, temperature 60℃. The drying time was 18 minutes, and the specific process parameters for spray drying were: inlet air temperature 90℃, outlet air temperature 65℃, atomizer speed 16000 rpm, and feed rate 3 mL / min, to obtain a nano-dispersion. The mass ratio of xanthan gum, deionized water, and the mixture was 0.04:50:20. In the mixture, the mass ratio of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution, and anhydrous ethanol was 1:3:0.36:6:50. Step A2: Add gum arabic to deionized water, heat to 65℃, and stir at 540 rpm for 18 minutes until homogeneous. Then add the nano-dispersion, maintaining the stirring speed, and continue stirring for 25 minutes. Adjust the pH to 5.8 with citrate-sodium citrate buffer. While stirring, add chitosan-acetic acid solution dropwise, controlling the addition to be completed within 10 minutes at a rate of 3 drops / second. After the addition is complete, continue stirring for 1.6 hours. Centrifuge at 840 rpm for 6 minutes, and wash with 30% ethanol aqueous solution. Each time, the mass of the ethanol-water solution was 25% of the mass of deionized water. The freeze-drying was carried out at a temperature of -30℃, a vacuum of 11Pa, and a drying time of 24h to obtain active microcapsules. The mass ratio of gum arabic, deionized water, nano-dispersion, and chitosan-acetic acid solution was 1:60:4:22. The chitosan-acetic acid solution was prepared by mixing chitosan and 1% acetic acid aqueous solution at a mass ratio of 2:30 at 50℃ and 600rpm for 16min until uniformly mixed, and then filtered through a 0.2μm microporous membrane. The modified pectin is prepared by the following steps: Step B1: Add high-ester pectin to deionized water, heat to 40℃, keep warm for 6 min, adjust pH to 3.5 with 0.1% acetic acid aqueous solution, then add pectin methyl esterase solution, and perform ultra-high pressure treatment to assist enzymatic hydrolysis under nitrogen protection. The specific process parameters for ultra-high pressure treatment to assist enzymatic hydrolysis are: ultra-high pressure treatment pressure 350 MPa, ultra-high pressure treatment temperature 40℃, ultra-high pressure treatment time 12 min, enzyme inactivation, control enzyme inactivation temperature at 95℃, enzyme inactivation time 22 min, cool, add 95% ethanol aqueous solution (ethanol aqueous solution mass is twice the mass of deionized water) to precipitate, filter through 400 mesh filter cloth, wash 3 times with 60% ethanol aqueous solution (each time ethanol aqueous solution mass is 30% of deionized water), and dry at 36℃ to constant weight to obtain deesterified pectin. The mass ratio of high-ester pectin, deionized water and pectin methyl esterase solution is 1:90:0.02. Step B2: Add the deesterified pectin to a 0.6% sodium bicarbonate aqueous solution, adjust the pH to 6 with a 0.4% citric acid aqueous solution, stir for 10 minutes until homogeneous, add chlorogenic acid and Tween-20, continue stirring for 36 minutes, and dry at 52°C to constant weight to obtain modified pectin. The mass ratio of deesterified pectin, sodium bicarbonate aqueous solution, chlorogenic acid and Tween-20 is 1:8:0.2:0.03.

[0038] Example 2 A bamboo leaf flavonoid toothpaste comprises the following ingredients in parts by weight: 28 parts sorbitol, 1.7 parts methylcellulose, 0.3 parts steviol glycosides, 22 parts aluminum hydroxide, 1.4 parts sodium lauroyl glutamate, 0.4 parts citrate-sodium citrate buffer, 2.6 parts active microcapsules, 0.5 parts spearmint flavoring, and 16 parts deionized water; The preparation method of bamboo leaf flavonoid toothpaste is as follows: Sorbitol, methylcellulose, steviol glycosides, and deionized water were stirred at 80 rpm for 14 minutes until homogeneous. While maintaining the stirring speed, aluminum hydroxide, sodium lauroyl glutamate, citrate-sodium citrate buffer, and active microcapsules were added sequentially. The stirring was continued for 24 minutes. Spearmint flavoring was then added. The stirring speed was maintained, and the mixture was homogenized at 96 MPa and 36°C for 8 minutes. Vacuum degassing was then performed. The specific process parameters for vacuum degassing were: vacuum degree -0.05 MPa, temperature 50°C, and time 19 minutes. The mixture was then discharged, filled, and the bamboo leaf flavonoid toothpaste was obtained. The active microcapsules are prepared by the following steps: Step A1: Add xanthan gum to deionized water and stir at 550 rpm for 18 minutes until homogeneous. Maintaining the stirring speed, while continuously stirring, add a mixture of bamboo leaf flavonoid extract, xylitol, modified pectin, a 0.7% (w / w) calcium chloride aqueous solution, and anhydrous ethanol dropwise over 15 minutes at a rate of 4 drops / second. After addition, perform rotary evaporation under reduced pressure. The specific process parameters for rotary evaporation under reduced pressure are: vacuum degree -0.07 MPa, temperature 50℃. The drying time was 20 minutes, and the specific process parameters for spray drying were: inlet air temperature 95℃, outlet air temperature 70℃, atomizer speed 18000 rpm, and feed rate 4 mL / min, to obtain a nano-dispersion. The mass ratio of xanthan gum, deionized water, and the mixture was 0.05:50:25. The mass ratio of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution, and anhydrous ethanol in the mixture was 1:4:0.39:8:55. Step A2: Add gum arabic to deionized water, heat to 70℃, control the stirring speed at 580 rpm, stir for 16 min until homogeneous, then add the nano-dispersion, maintain the stirring speed, and continue stirring for 30 min. Adjust the pH to 6 with citrate-sodium citrate buffer, and add chitosan-acetic acid solution dropwise while stirring, controlling the addition to be completed within 10 min, controlling the dropping rate at 4 drops / second. After the addition is complete, continue stirring for 1.9 h, centrifuge at 840 rpm for 8 min, and wash 4 times with 35% ethanol aqueous solution (each... The ethanol aqueous solution (25% of the mass of deionized water) was freeze-dried at -35℃, with a vacuum of 12Pa and a drying time of 26h to obtain active microcapsules. The mass ratio of gum arabic, deionized water, nano-dispersion and chitosan-acetic acid solution was 1.5:70:4.5:23. The chitosan-acetic acid solution was prepared by mixing chitosan and acetic acid aqueous solution with a mass dispersion of 1.5% at a mass ratio of 3:30 at 55℃ and 650rpm for 14min until uniformly mixed, and then filtered through a 0.3μm microporous membrane. The modified pectin is prepared by the following steps: Step B1: Add high-ester pectin to deionized water, heat to 45℃, keep warm for 8 min, adjust pH to 4 with 0.06% acetic acid aqueous solution, then add pectin methyl esterase solution, and perform ultra-high pressure treatment to assist enzymatic hydrolysis under nitrogen protection. The specific process parameters for ultra-high pressure treatment to assist enzymatic hydrolysis are as follows: ultra-high pressure treatment pressure is 395 MPa, ultra-high pressure treatment temperature is 45℃, and ultra-high pressure treatment time is 15 min. Inactivate enzyme by controlling the enzyme inactivation temperature at 100℃ and the enzyme inactivation time at 20 min. Cool, add 95% ethanol aqueous solution (the mass of the ethanol aqueous solution is twice the mass of the deionized water) to precipitate, filter through a 400-mesh filter cloth, wash 4 times with 60% ethanol aqueous solution (each time the mass of the ethanol aqueous solution is 30% of the mass of the deionized water), and dry at 40℃ to constant weight to obtain deesterified pectin. The mass ratio of high-ester pectin, deionized water, and pectin methyl esterase solution is 1:100:0.03. Step B2: Add the deesterified pectin to a 0.8% sodium bicarbonate aqueous solution, adjust the pH to 7 with a 0.6% citric acid aqueous solution, stir for 15 minutes until homogeneous, add chlorogenic acid and Tween-20, continue stirring for 38 minutes, and dry at 54°C to constant weight to obtain modified pectin. The mass ratio of deesterified pectin, sodium bicarbonate aqueous solution, chlorogenic acid and Tween-20 is 1:9:0.25:0.04.

[0039] Example 3 A bamboo leaf flavonoid toothpaste comprises the following ingredients in parts by weight: 30 parts propylene glycol, 1.8 parts hydroxyethyl cellulose, 0.4 parts xylitol, 24 parts calcium pyrophosphate, 1.6 parts sodium lauroyl sarcosinate, 0.5 parts citrate-sodium citrate buffer, 2.8 parts active microcapsules, 0.6 parts peppermint flavoring, and 18 parts deionized water; The preparation method of bamboo leaf flavonoid toothpaste is as follows: Propylene glycol, hydroxyethyl cellulose, xylitol, and deionized water were stirred at 100 rpm for 12 minutes until homogeneous. While maintaining the stirring speed, calcium pyrophosphate, sodium lauroyl sarcosinate, citrate-sodium citrate buffer, and active microcapsules were added sequentially. The stirring was continued for 26 minutes, followed by the addition of peppermint flavor. The stirring speed was maintained, and the mixture was homogenized at 98 MPa and 40°C for 10 minutes. Vacuum degassing was then performed, with the following process parameters: vacuum degree -0.08 MPa, temperature 40°C, and time 22 minutes. The mixture was then discharged, filled, and the bamboo leaf flavonoid toothpaste was obtained. The active microcapsules are prepared by the following steps: Step A1: Add xanthan gum to deionized water and stir at 600 rpm for 20 minutes until homogeneous. Maintaining the stirring speed, while continuously stirring, add a mixture of bamboo leaf flavonoid extract, xylitol, modified pectin, a 0.8% (w / w) calcium chloride aqueous solution, and anhydrous ethanol dropwise over 15 minutes at a rate of 5 drops / second. After addition, perform rotary evaporation under reduced pressure. The specific process parameters for rotary evaporation under reduced pressure are: vacuum degree -0.09 MPa, temperature 40℃, and time... The time interval was 22 minutes, and the spray drying process parameters were as follows: inlet air temperature 100℃, outlet air temperature 75℃, atomizer speed 20000rpm, and feed rate 5mL / min, to obtain nano-dispersion. The mass ratio of xanthan gum, deionized water and mixture was 0.06:50:30. The mass ratio of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution and anhydrous ethanol in the mixture was 1:5:0.42:10:60. Step A2: Add gum arabic to deionized water, heat to 75℃, and stir at 620 rpm for 14 minutes until homogeneous. Then add the nano-dispersion, maintain the stirring speed, and continue stirring for 35 minutes. Adjust the pH to 6.2 with citrate-sodium citrate buffer. While stirring, add chitosan-acetic acid solution dropwise, controlling the addition to be completed within 10 minutes at a rate of 5 drops / second. After the addition is complete, continue stirring for 2.2 hours. Centrifuge at 860 rpm for 10 minutes, and wash with 40% ethanol aqueous solution. Five freeze-drying cycles were performed (each time the mass of the ethanol-water solution was 25% of the mass of the deionized water). The freeze-drying temperature was controlled at -40℃, the vacuum degree at 13Pa, and the drying time at 28h to obtain active microcapsules. The mass ratio of gum arabic, deionized water, nano-dispersion, and chitosan-acetic acid solution was 2:80:5:24. The chitosan-acetic acid solution was prepared by mixing chitosan and a 2% acetic acid aqueous solution at a mass ratio of 4:30 at 60℃ and 700rpm for 12min until homogeneous, and then filtering through a 0.4μm microporous membrane. The modified pectin is prepared by the following steps: Step B1: Add high-ester pectin to deionized water, heat to 50℃, maintain temperature for 10 min, adjust pH to 4.5 with 0.04% acetic acid aqueous solution, then add pectin methyl esterase solution. Under nitrogen protection, perform ultra-high pressure treatment to assist enzymatic hydrolysis. The specific process parameters for ultra-high pressure treatment to assist enzymatic hydrolysis are: ultra-high pressure treatment pressure 440 MPa, ultra-high pressure treatment temperature 50℃, ultra-high pressure treatment time 18 min, enzyme inactivation, and control. The enzyme inactivation temperature was 105℃, the inactivation time was 18 min, and after cooling, a 95% ethanol aqueous solution (the mass of the ethanol aqueous solution was twice the mass of the deionized water) was added to precipitate the product. The product was filtered through a 400-mesh filter cloth and washed three times with a 60% ethanol aqueous solution (each time the mass of the ethanol aqueous solution was 30% of the mass of the deionized water). The product was dried at 44℃ to constant weight to obtain deesterified pectin. The mass ratio of high-ester pectin, deionized water, and pectin methyl esterase solution was 1:110:0.04. Step B2: Add the deesterified pectin to a 1% sodium bicarbonate aqueous solution, adjust the pH to 8 with a 0.8% citric acid aqueous solution, stir for 20 minutes until homogeneous, add chlorogenic acid and Tween-20, continue stirring for 40 minutes, and dry at 56°C to constant weight to obtain modified pectin. The mass ratio of deesterified pectin, sodium bicarbonate aqueous solution, chlorogenic acid and Tween-20 is 1:10:0.3:0.05.

[0040] Comparative Example 1 Comparative Example 1 is the same as Example 1, except that in the preparation of modified pectin, deesterified pectin is replaced with an equal mass of high-ester pectin.

[0041] Comparative Example 2 Comparative Example 2 is the same as Example 1, except that chlorogenic acid is replaced with an equal mass of citric acid in the preparation of modified pectin.

[0042] Comparative Example 3 Comparative Example 3 is the same as Example 1, except that in the preparation of the active microcapsules, the chitosan-acetic acid solution is replaced with an equal mass of gelatin-acetic acid solution.

[0043] Comparative Example 4 Comparative Example 4 is the same as Example 1, except that xylitol is replaced with an equal mass of mannitol in the preparation of the active microcapsules.

[0044] Performance testing 1. Security Testing The toothpaste pastes prepared in Examples 1-3 and Comparative Examples 1-4 are uniform, free of foreign matters, do not overflow from the tube mouth after being filled into the tube, do not separate out liquid, have normal fragrance and color, meet the standards of GB / T 8372-2017, the arsenic content is far lower than the upper limit specified in GB / T 8372-2017 "Toothpaste", and the colony flora meets the relevant regulations of the "Technical Specifications for Cosmetics Safety", and all are qualified.

[0045] 2. Solubility test The solubility of the bamboo leaf flavonoid toothpaste prepared in Examples 1-3 and Comparative Examples 1-4 of the present application was tested respectively.

[0046] Test method: Take 1 g of the bamboo leaf flavonoid toothpaste prepared in Examples 1-3 and Comparative Examples 1-4 and place it in 1000 mL of artificial saliva (purchased from Jiangsu Magbio Technology Co., Ltd., product number BY0235), heat it to 37 °C, and stir it for 2 minutes at 300 rpm using the paddle method, and measure the dissolution degree of bamboo leaf flavonoids. The specific test results are shown in Table 1: Table 1 Test results of the dissolution degree of bamboo leaf flavonoids

[0047] It can be seen from the results shown in Table 1 that the dissolution degree of bamboo leaf flavonoids in the bamboo leaf flavonoid toothpaste prepared in Examples 1-3 of the present invention is significantly higher than that in Comparative Examples 1-4. This shows that the bamboo leaf flavonoid toothpaste prepared by the preparation method provided by the present invention has high solubility and broad application prospects.

[0048] 3. Anti-inflammatory test ICR mice provided by Shanghai Slack Experimental Animal Co., Ltd. with a body weight of 18-22 g (SCXK(Shanghai) 2017-0005) were used as experimental animals. The above mice were placed at 18-22 °C, relative humidity: 60-70%, light condition: 12 h / 12 h, light and dark alternation, and adaptively raised for one week.

[0049] Ninety qualified mice were randomly divided into 9 groups, namely the model control group, the anti-inflammatory control group, the Examples 1-3 groups and the Comparative Examples 1-4 groups, with 10 mice in each group. The left ears of the mice in each group were not treated as the background value. A total of 30 μL of xylene solution was applied to both the inner and outer sides of the right ears of the mice. After 30 minutes, except for the model control group, 0.1 g of the bamboo leaf flavonoid toothpaste prepared in each group was applied to both sides of the right ears of the mice in the Examples 1-3 groups and the Comparative Examples 1-4 groups, and 0.1 g of Youluosha Xing licorice toothpaste (containing dipotassium glycyrrhizinate) was applied to both the inner and outer sides of the right ears of the anti-inflammatory control group. After 1 h of sample application, the same parts of both ears were weighed and recorded, and the weight difference between the left and right ears was the swelling degree (unit: mg). The specific test results are shown in Table 2: Table 2 Test results of the inhibition of ear swelling in each group of mice (n = 9, ±s, %)

[0050] Note: In Table 2, a) P < 0.05 compared with the model control group; b) P < 0.05 compared with comparative groups 1-4 and the anti-inflammatory control group.

[0051] As shown in Table 2, compared with the model control group, the anti-inflammatory control group and the comparative groups 1-4, the ear swelling of mice that applied the toothpaste prepared in Examples 1-3 was significantly reduced, which indicates that the bamboo leaf flavonoid toothpaste formulation prepared in this invention has a more superior anti-inflammatory effect.

[0052] 4. Antibacterial test 4.1 Cultivation of inoculum P. gingivalis, P. intermedius, and F. nucleatum were inoculated into nutrient broth medium and cultured anaerobically at 37°C for 2–5 days. Single colonies from the plates were picked and a bacterial suspension was prepared in 5 mL of sterile PBS (50 mmol / L, pH 7.4), adjusted to a McFarland turbidity concentration of 0.5 (i.e., 1 x 10⁻⁶). 8 The pretreated bacterial suspension was prepared by mixing CFU / mL; a carboxymethyl cellulose solution was prepared separately (the carboxymethyl cellulose solution consisted of 50 mmol / L carboxymethyl cellulose and PBS solution at pH 7.4 in a mass ratio of 3:100), filtered through a 0.22 μm pore size filter membrane, and then mixed with the pretreated bacterial suspension to prepare an inoculated bacterial suspension containing 2% carboxymethyl cellulose.

[0053] 4.2 Establishment of an animal model of halitosis Ninety male SPF-grade Wistar rats, weighing 200±20g, were selected. The rats were healthy, active, with glossy fur, good appetite, and free from dental caries and periodontal disease. The inoculum culture obtained above (3×10⁻⁶) was used as the starting material. 6 The gingival index (CFU / mL) was applied to the gingiva of rats once a day for four consecutive weeks, and the gingival index and plaque index of rats were measured weekly.

[0054] 4.3 Animal Experiment Grouping Ninety qualified rats, after successfully modeling halitosis by applying a bacterial solution that easily causes bad breath to their oral cavity, were randomly divided into nine groups: a model control group, an antibacterial control group, groups 1-3 of Examples, and groups 1-4 of Comparative Examples, with ten rats in each group. Except for the model control group, groups 1-3 of Examples and groups 1-4 of Comparative Examples received 0.2 g / rat of the prepared bamboo leaf flavonoid toothpaste daily using cotton swabs. The antibacterial control group received 0.2 g / rat of Helicobacter pylori and licorice toothpaste (containing dipotassium glycyrrhizate) daily using cotton swabs. The treatment lasted for four weeks.

[0055] 4.4 Observation Indicators and Detection Methods Testing gingival index and plaque index The specific testing and scoring criteria for the Gingival Index are as follows: Using the CPI periodontal probe recommended by the WHO (World Health Organization), examine each tooth at four points: mesobob, buccal, distobuccal, and lingual. Score each point separately. The sum of the four scores divided by 4 gives the score for that tooth. 0 indicates healthy gums; 1 indicates mild gingival inflammation: slight change in gum color and mild edema, no bleeding on probing; 2 indicates moderate gingival inflammation: red, swollen, and shiny gums, bleeding on probing; 3 indicates severe gingival inflammation: significantly red and swollen gums or ulcers, with a tendency to bleed spontaneously. Average values ​​of 0-1 are defined as mild inflammation, 1-2 as moderate inflammation, and 2-3 as severe inflammation. The specific scoring criteria for the gingival index are as follows: The severity of the gingival index is scored from 0 to 3 points. Healthy gums with no signs of inflammation: 0 points; Mild inflammation: slight change in gum color (such as darkening), mild edema, no bleeding on probing: 1 point; Moderate inflammation: red, edematous, and shiny gums, bleeding on probing: 2 points; Severe inflammation: significantly red and swollen gums, possibly with ulcers, and a tendency to bleed spontaneously: 3 points. The specific testing and scoring criteria for the plaque index are as follows: Examine four points on each tooth: mesobob, buccal, distobuccal, and lingual surfaces. Score each point separately. The sum of the four scores divided by 4 gives the tooth's score. 0 indicates no plaque near the gingival margin; 1 indicates thin plaque near the gingival margin, invisible to the naked eye but scrapable with the side of a probe tip; 2 indicates moderate plaque on the gingival margin or proximal surfaces; 3 indicates a large amount of soft plaque in the gingival sulcus or on the gingival margin and proximal surfaces. Specific test results are shown in Table 3. Table 3. Results of antibacterial score test in rats of each group (n=9, ±s, %

[0056] Note: In Table 3, a) P < 0.05 compared with the model group; b) P < 0.05 compared with comparative groups 1-4 and the antibacterial control group.

[0057] As shown in Table 3, compared with the model control group, the antibacterial control group and the comparative groups 1-4, the plaque index and gingival index of rats applying the toothpaste prepared in Examples 1-3 were significantly reduced. This indicates that the bamboo leaf flavonoid toothpaste formulation prepared in this invention has a more superior antibacterial effect.

[0058] This specific embodiment is merely an explanation of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A bamboo leaf flavonoid toothpaste, characterized in that, The product comprises the following ingredients by weight: 26-30 parts wetting agent, 1.6-1.8 parts binder, 0.2-0.4 parts sweetener, 20-24 parts abrasive, 1.2-1.6 parts surfactant, 0.3-0.5 parts pH adjuster, 2.4-2.8 parts active microcapsules, 0.4-0.6 parts flavoring, and 14-18 parts deionized water; The active microcapsules are first cross-linked from xanthan gum, bamboo leaf flavonoid extract, xylitol, and modified pectin to obtain a nano-dispersion, and then prepared by complex coagulation with gum arabic and chitosan as wall materials and the nano-dispersion as core material. The modified pectin is prepared by enzymatic hydrolysis of high-ester pectin with pectin methyl esterase solution under ultra-high pressure to obtain deesterified pectin, which is then mixed with chlorogenic acid.

2. The bamboo leaf flavonoid toothpaste according to claim 1, characterized in that, The active microcapsules are prepared by the following steps: Step A1: Add xanthan gum to deionized water and stir well. While stirring, add dropwise a mixture of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution and anhydrous ethanol. After the addition is complete, evaporate under reduced pressure and spray dry to obtain nano-dispersion. Step A2: Add gum arabic to deionized water, heat to 65-75℃, stir evenly, then add nano-dispersion, stir and react for 25-35 minutes, adjust pH to 5.8-6.2, add chitosan-acetic acid solution dropwise, after the addition is complete, continue stirring and reacting for 1.6-2.2 hours, centrifuge, wash, and dry to obtain active microcapsules.

3. The bamboo leaf flavonoid toothpaste according to claim 2, characterized in that, In step A1, the mass ratio of xanthan gum, deionized water, and the mixture is 0.04-0.06:50:20-30. In the mixture, the mass ratio of bamboo leaf flavonoid extract, xylitol, modified pectin, calcium chloride aqueous solution, and anhydrous ethanol is 1:3-5:0.36-0.42:6-10:50-60.

4. The bamboo leaf flavonoid toothpaste according to claim 2, characterized in that, In step A2, the mass ratio of gum arabic, deionized water, nano-dispersion, and chitosan-acetic acid solution is 1-2:60-80:4-5:22-24.

5. The bamboo leaf flavonoid toothpaste according to claim 1, characterized in that, The modified pectin is prepared by the following steps: Step B1: Add high-ester pectin to deionized water, heat to 40-50℃, keep warm for 6-10 minutes, adjust pH to 3.5-4.5, then add pectin methyl esterase solution, under nitrogen protection, use ultra-high pressure to assist enzymatic hydrolysis, inactivate enzyme, cool, precipitate, filter, wash, and dry to obtain deesterified pectin. Step B2: Add the deesterified pectin to the sodium bicarbonate aqueous solution, adjust the pH to 6-8, stir well, add chlorogenic acid and Tween-20, continue stirring for 36-40 minutes, and dry to obtain modified pectin.

6. The bamboo leaf flavonoid toothpaste according to claim 5, characterized in that, In step B1, the specific process parameters for ultra-high pressure treatment-assisted enzymatic hydrolysis are as follows: ultra-high pressure treatment-assisted enzymatic hydrolysis pressure is 350-440 MPa, ultra-high pressure treatment-assisted enzymatic hydrolysis temperature is 40-50℃, and ultra-high pressure treatment-assisted enzymatic hydrolysis time is 12-18 min.

7. The bamboo leaf flavonoid toothpaste according to claim 5, characterized in that, In step B1, the mass ratio of the high-ester pectin, deionized water, and pectin methylesterase solution is 1:90-110:0.02-0.

04.

8. The bamboo leaf flavonoid toothpaste according to claim 5, characterized in that, In step B2, the mass ratio of deesterified pectin, sodium bicarbonate aqueous solution, chlorogenic acid and Tween-20 is 1:8-10:0.2-0.3:0.03-0.

05.

9. A method for preparing bamboo leaf flavonoid toothpaste according to any one of claims 1-8, characterized in that, It is prepared by the following steps: The humectant, binder, sweetener and deionized water are mixed evenly. While stirring, the abrasive, surfactant, pH adjuster and active microcapsules are added. Stirring is continued for 22-26 minutes. Then the fragrance is added, homogenized, vacuum-foamed, discharged and filled to obtain bamboo leaf flavonoid toothpaste.

10. The use of bamboo leaf flavonoid toothpaste as described in any one of claims 1-8 in the preparation of oral care products for antibacterial and anti-inflammatory purposes.

Images