Mint fragrance type whitening toothpaste capable of inhibiting halitosis for long time and preparation process of mint fragrance type whitening toothpaste

Abstract

The invention provides mint-flavor whitening toothpaste capable of inhibiting halitosis for a long time and a preparation process of the mint-flavor whitening toothpaste, and belongs to the technical field of toothpaste preparation. The preparation process comprises the following steps: preparing a lactoferrin-glycyrrhiza polysaccharide copolymer compound; preparing tannic acid nano cellulose composite particles; preparing the medicine mulberry and lemon compound enzyme; and preparing the mint fragrance type whitening toothpaste. The mint fragrance type whitening toothpaste prepared by adding the hyaluronic acid, the mulberry and lemon composite enzyme, the lactoferrin-glycyrrhiza polysaccharide copolymer compound, the tannic acid nano cellulose composite particles and the mint essence into the toothpaste base body can inhibit ozostomia for a long time and can also safely and effectively whiten teeth.

Description

Technical Field

[0001] The invention relates to the technical field of toothpaste preparation, and in particular to a mint-flavored whitening toothpaste capable of inhibiting halitosis for a long time and a preparation process thereof. Background Art

[0002] In the field of oral care, toothpaste, as an essential product for daily oral cleaning, has always attracted widespread attention from consumers. With the improvement of people's living standards, the functional requirements for toothpaste are becoming increasingly diverse. At present, there are many types of toothpastes on the market with different functions, mainly including cleaning teeth, preventing tooth decay, freshening breath, etc. However, existing toothpastes still have some shortcomings in suppressing bad breath and whitening teeth.

[0003] In terms of suppressing bad breath, although most toothpastes can freshen breath for a short time after brushing teeth, the effect is difficult to last. Bad breath is mainly caused by bacterial growth in the mouth, fermentation of food residues, and oral diseases. Existing toothpastes can only temporarily cover up the odor and cannot fundamentally suppress bacterial growth, causing the bad breath problem to recur quickly.

[0004] When it comes to whitening teeth, some whitening toothpastes achieve whitening effects by adding abrasives or chemical bleaching agents. However, excessive use of abrasives may damage tooth enamel and affect tooth health, while chemical bleaching agents may irritate the oral mucosa and cause discomfort.

[0005] In summary, the development of a toothpaste that can both inhibit bad breath for a long time and whiten teeth safely and effectively has important market demand and practical significance. The present invention aims to provide a mint-flavored whitening toothpaste that can inhibit bad breath for a long time and a preparation process thereof to solve the above problems existing in existing toothpastes. Summary of the invention

[0006] In view of the shortcomings of the prior art, the object of the present invention is to provide a mint-flavored whitening toothpaste with long-term bad breath inhibition and a preparation process thereof.

[0007] A preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition comprises the following steps: S1: Preparation of lactoferrin-licorice polysaccharide copolymer complex Licorice is defatted and extracted with deionized water to obtain licorice polysaccharide, and then the licorice polysaccharide solution and the lactoferrin solution are mixed and the pH is adjusted to 7.0, and then the mixture is reacted at 70-90° C. for 4-5 hours to obtain a lactoferrin-licorice polysaccharide copolymer complex; S2: Preparation of tannic acid nanocellulose composite particles The tannic acid solution is added dropwise to the cellulose nanofiber solution, and then a hydrochloric acid solution is added, mixed and reacted, and then centrifuged to prepare tannic acid nanocellulose composite particles; S3: Preparation of medicinal mulberry lemon compound enzyme The medicinal mulberry and lemon are added into deionized water in a mass ratio of 1-2:1, and then white sugar is added to homogenize, and then enzymolysis and fermentation are performed to prepare the medicinal mulberry and lemon composite enzyme; S4: Preparation of mint-flavored whitening toothpaste A toothpaste base is prepared by mixing glycerin, sorbitol, sodium carboxymethyl cellulose, cocamidopropyl betaine, hydrated silica and deionized water, and then 0.3-0.5 weight parts of hyaluronic acid, 3-5 weight parts of medicinal mulberry lemon composite enzyme, 2-3 weight parts of lactoferrin-licorice polysaccharide copolymer complex, 2-3 weight parts of tannic acid nanocellulose composite particles and 0.3-0.5 weight parts of mint essence are added to the toothpaste base and mixed to prepare a mint-flavored whitening toothpaste.

[0008] Furthermore, step S1 of preparing the lactoferrin-licorice polysaccharide copolymer complex specifically comprises the following steps: S1.1: Grind the licorice root and pass it through a 100-120 mesh sieve. Then, add the sieved powder into 95% (v / v) ethanol and stir to defat at 70-72°C for 3-4 hours. Then, centrifuge at 2000-3000 r / min for 10-12 minutes and dry to obtain defatted licorice powder. S1.2: Add defatted licorice powder to 3-5 times the amount of deionized water, extract at 90-95°C for 2-3h, then centrifuge at 2000-3000r / min to obtain a filter residue and a first filtrate, add the filter residue to 3-5 times the amount of deionized water again, extract at 90-95°C for 2-3h, then centrifuge at 2000-3000r / min to obtain a second filtrate, concentrate the first filtrate and the second filtrate under reduced pressure, and precipitate with 80% (v / v) anhydrous ethanol at 4-5°C for 12-14h, then dry the precipitate and deproteinize to obtain licorice polysaccharide; S1.3: Add glycyrrhizin polysaccharide and lactoferrin into deionized water respectively, stir for 2-3 hours, and then place at 4-5℃ for 12-14 hours to obtain glycyrrhizin polysaccharide solution and lactoferrin solution with a concentration of 10 mg / mL. Mix the glycyrrhizin polysaccharide solution and lactoferrin solution in equal proportions, adjust the pH to 7.0, and then react at 70-90℃ for 4-5 hours. After the reaction is completed, cool rapidly in an ice water bath to obtain a lactoferrin-glycyrrhizin polysaccharide copolymer complex.

[0009] Furthermore, step S2 of preparing tannic acid nanocellulose composite particles specifically comprises the following steps: S2.1: adding 5-8 parts by weight of cellulose nanofibers to 500-550 parts by weight of deionized water, stirring and mixing at 200-300 r / min for 5-10 min to obtain a cellulose nanofiber solution, adding 1-2 parts by weight of tannic acid to 4-5 parts by weight of deionized water, stirring and mixing at 200-300 r / min for 5-10 min to obtain a tannic acid solution; S2.2: Add tannic acid solution dropwise to the cellulose nanofiber solution, then add 2-3 parts by weight of hydrochloric acid solution, and then mix with magnetic stirring at 60-70°C for 2-3 hours. After the reaction is completed, centrifuge at 8000-10000rpm for 5-10min, and then centrifuge at 12000-15000rpm for 5-10min. Wash the precipitate with anhydrous ethanol and deionized water for 2-3 times respectively, and finally freeze it in a refrigerator for 12-14 hours, and then freeze-dry it to obtain tannic acid nanocellulose composite particles.

[0010] Furthermore, step S3, the preparation of the medicinal mulberry-lemon compound enzyme, specifically comprises the following steps: S3.1: Select fresh medicinal mulberry and lemon, wash them respectively, then add the medicinal mulberry and lemon in a mass ratio of 1-2:1 to 3-4 times the amount of deionized water, squeeze the juice and homogenize to obtain a homogenate, then add white sugar, stir and mix evenly to obtain a composite fruit pulp; S3.2: adding pectinase to the composite fruit pulp, and then ultrasonically treating it at 300-330W and 43-45°C for 1.5-2h, and then inactivating the enzyme at 90-93°C for 20-30min to obtain the enzymatically hydrolyzed composite fruit pulp; S3.3: Inoculate 0.1-0.2% of the total mass of the enzymatically hydrolyzed composite pulp with a composite fermentation agent, and then ferment at 35-37°C for 70-72h. After the fermentation is completed, filter and sterilize to obtain the medicinal mulberry-lemon composite enzyme.

[0011] Furthermore, step S4 is the preparation of the mint flavored whitening toothpaste, specifically comprising the following steps: S4.1: Add 10-12 parts by weight of glycerol, 5-8 parts by weight of sorbitol and 50-60 parts by weight of deionized water into a stirring pot, then stir at 50-100 r / min for 10-15 min, mix thoroughly, then add 1-2 parts by weight of sodium carboxymethyl cellulose, stir at 100-200 r / min for 10-15 min, then add 1-2 parts by weight of cocamidopropyl betaine and 20-23 parts by weight of hydrated silica, stir at 150-200 r / min for 10-15 min, to obtain a toothpaste base; S4.2: Add 0.3-0.5 parts by weight of hyaluronic acid, 3-5 parts by weight of medicinal mulberry lemon complex enzyme, 2-3 parts by weight of lactoferrin-licorice polysaccharide copolymer complex, 2-3 parts by weight of tannic acid nanocellulose composite particles, and 0.3-0.5 parts by weight of mint essence to the toothpaste base, stir and mix at 200-300 r / min for 20-30 min, maintain bubbling at a vacuum degree of ≥0.094 MPa for 2-3 min, discharge the material, and fill it to obtain a mint-flavored whitening toothpaste.

[0012] Furthermore, the hydrochloric acid solution in step S2.2 is specifically a hydrochloric acid solution obtained by dissolving 100 µL of concentrated hydrochloric acid in 1 mL of deionized water.

[0013] Furthermore, the amount of white sugar added in step S3.1 is 10-12% of the total mass of the homogenate.

[0014] Furthermore, in step S3.2, the amount of pectinase added is 0.28-0.3% of the total mass of the composite fruit pulp.

[0015] Furthermore, in step S3.3, the composite fermentation agent is composed of 3-4 parts by weight of Lactobacillus plantarum N13, 2-1 parts by weight of Lactobacillus bulgaricus, 1-0.5 parts by weight of Lactobacillus helveticus, 2-1 parts by weight of Leuconostoc mesenteroides subsp. mesenteroides and 1-0.5 parts by weight of Streptococcus thermophilus.

[0016] A mint-flavored whitening toothpaste for long-term halitosis suppression is prepared by any of the preparation processes for a mint-flavored whitening toothpaste for long-term halitosis suppression.

[0017] Compared with the prior art, the present invention has at least the following beneficial effects: 1. The lactoferrin in the present invention has a broad-spectrum antibacterial activity. It can deprive the iron element required for bacterial growth by combining with the iron ions on the surface of bacteria, thereby inhibiting the growth and reproduction of bacteria. At the same time, licorice polysaccharide also has a certain antibacterial ability. The copolymer formed by the two can more effectively target the odor-producing bacteria in the oral cavity, such as Streptococcus mutans, Porphyromonas gingivalis, etc., reduce the production of odorous substances such as hydrogen sulfide by these bacteria decomposing food residues and oral secretions, and inhibit the generation of bad breath from the root. In addition, the lactoferrin-licorice polysaccharide copolymer complex can regulate the oral cavity. The structure of the microbial community promotes the growth of beneficial bacteria, such as bifidobacterium and lactobacillus, inhibits the over-reproduction of harmful bacteria, and restores the oral microbial community to a normal balance, thereby reducing the problem of bad breath caused by microbial imbalance. The lactoferrin-licorice polysaccharide copolymer complex can also interfere with the adhesion of bacteria on the tooth surface and prevent the formation of dental plaque. At the same time, the lactoferrin-licorice polysaccharide copolymer complex has a certain decomposition and removal effect on the already formed dental plaque and stains, making the tooth surface cleaner, reducing pigmentation, and achieving the effect of whitening teeth.

[0018] 2. The tannic acid in the tannic acid nanocellulose composite particles prepared by the present invention has good antibacterial properties, and has a significant inhibitory effect on common harmful bacteria in the oral cavity, such as Streptococcus mutans, Porphyromonas gingivalis, etc., and can effectively prevent the occurrence of oral diseases such as caries and periodontitis. Nanocellulose as a carrier can make tannic acid better dispersed in the toothpaste system, enhance its contact probability with bacteria, thereby exerting a more efficient broad-spectrum antibacterial effect, and nanocellulose has a large specific surface area and rich pore structure, which can adsorb pigment molecules on the surface of teeth, such as exogenous pigmentation caused by smoking, drinking coffee, drinking tea, etc., and tannic acid can react chemically with some pigments to form insoluble complexes, further promoting the removal of pigments. The combination of the two helps to restore the whiteness of teeth. The tannic acid nanocellulose composite particles can reduce the formation of dental plaque by inhibiting bacterial growth and destroying biofilms. Reducing dental plaque helps to keep teeth clean and white, and prevent tooth discoloration from the root.

[0019] 3. The medicinal mulberry lemon compound enzyme added in the present invention contains a variety of enzymes and active ingredients, which can act on the key enzymes of bacteria to inhibit their activity, thereby reducing the number of bacteria in the oral cavity. The medicinal mulberry lemon compound enzyme can also change the charge or structure of the bacterial surface, making it difficult for it to adhere to the teeth, thereby reducing the colonization ability of bacteria in the oral cavity, playing a role in inhibiting bacteria and preventing oral diseases. The medicinal mulberry lemon compound enzyme is rich in reducing substances such as vitamin C, has a strong antioxidant ability, can undergo redox reaction with the pigment on the surface of the teeth, and decompose the pigment into colorless or light-colored substances, thereby achieving a whitening effect, and the enzymes in the medicinal mulberry lemon compound enzyme can decompose organic dirt and residual food residues on the surface of the teeth. Through the decomposition of the enzyme, the tooth surface can be effectively cleaned, the attachment of dirt and pigments can be reduced, and the teeth can be restored to whiteness. The medicinal mulberry lemon compound enzyme can also penetrate into the tiny pores and grooves on the surface of the teeth, decompose and remove stubborn stains such as tooth stains deposited therein, thereby making the tooth surface smoother and showing a natural whitening effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The accompanying drawings, which are incorporated herein and constitute a part of the specification, illustrate embodiments of the invention and, together with the description, further serve to explain the principles of the invention and to enable those skilled in the relevant art to make and use the invention.

[0021] Figure 1 The present invention is a flow chart of the preparation process of a mint-flavored whitening toothpaste for long-term halitosis suppression used in an embodiment of the present invention.

[0022] Figure 2 The electrophoretic diagrams of the lactoferrin-licorice polysaccharide copolymer complex at different reaction temperatures in the examples of the present invention. DETAILED DESCRIPTION

[0023] The preparation process of a mint-flavored whitening toothpaste for long-term inhibition of halitosis provided by the present invention is described in detail below in conjunction with the accompanying drawings and specific embodiments. At the same time, it is explained here that in order to make the embodiments more detailed, the following embodiments are the best and preferred embodiments, and those skilled in the art may also adopt other alternatives to implement some known technologies; and the accompanying drawings are only for more specific description of the embodiments, and are not intended to specifically limit the present invention.

[0024] Example 1 A preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition, such as Figure 1 As shown, the following steps are included: S1: Preparation of lactoferrin-licorice polysaccharide copolymer complex S1.1: Grind the licorice root and pass it through a 100-mesh sieve. Then, add the sieved powder into 95% (v / v) ethanol and defatting by stirring at 70°C for 3 hours. Then, centrifuge at 2000 r / min for 10 minutes and dry to obtain defatted licorice powder. S1.2: Add defatted licorice powder to 3 times the amount of deionized water, extract at 90°C for 2 hours, then centrifuge at 2000r / min to obtain a filter residue and a first filtrate, add the filter residue to 3 times the amount of deionized water again, extract at 90°C for 2 hours, then centrifuge at 2000r / min to obtain a second filtrate, concentrate the first filtrate and the second filtrate under reduced pressure, and precipitate with 80% (v / v) anhydrous ethanol at 4°C for 12 hours, then dry the precipitate and deproteinize to obtain licorice polysaccharide; S1.3: Glycyrrhiza polysaccharide and lactoferrin were added to deionized water respectively, stirred for 2 hours, and then placed at 4°C for 12 hours to obtain a glycyrrhiza polysaccharide solution and a lactoferrin solution with a concentration of 10 mg / mL, and the glycyrrhiza polysaccharide solution and the lactoferrin solution were mixed in equal proportions, and the pH was adjusted to 7.0, and then reacted at 70°C for 4 hours. After the reaction was completed, the mixture was rapidly cooled in an ice water bath to obtain a lactoferrin-glycyrrhiza polysaccharide copolymer complex; S2: Preparation of tannic acid nanocellulose composite particles S2.1: adding 5 parts by weight of cellulose nanofibers to 500 parts by weight of deionized water, stirring and mixing at 200 r / min for 5 minutes to obtain a cellulose nanofiber solution, adding 1 part by weight of tannic acid to 4 parts by weight of deionized water, stirring and mixing at 200 r / min for 5 minutes to obtain a tannic acid solution; S2.2: Add the tannic acid solution dropwise to the cellulose nanofiber solution, then add 2 parts by weight of hydrochloric acid solution, and then stir and mix under magnetic stirring at 60°C for 2 hours. After the reaction is completed, centrifuge at 8000 rpm for 5 minutes, and then centrifuge at 12000 rpm for 5 minutes. Wash the precipitate twice with anhydrous ethanol and deionized water, respectively, and finally freeze it in a refrigerator for 12 hours, and then freeze-dry it to obtain tannic acid nanocellulose composite particles; The hydrochloric acid solution is a hydrochloric acid solution obtained by dissolving 100 µL of concentrated hydrochloric acid in 1 mL of deionized water; S3: Preparation of medicinal mulberry lemon compound enzyme S3.1: Select fresh medicinal mulberry and lemon, wash them respectively, then add the medicinal mulberry and lemon in a mass ratio of 1:1 to 3 times the amount of deionized water, squeeze the juice and homogenize to obtain a homogenate, then add 10% of the total mass of the homogenate of white sugar, stir and mix evenly to obtain a composite fruit pulp; S3.2: adding 0.28% pectinase to the composite fruit pulp, and then ultrasonically treating it at 300W and 43℃ for 1.5h, and then inactivating the enzyme at 90℃ for 20min to obtain the enzymatically hydrolyzed composite fruit pulp; S3.3: inoculating 0.1% of the total weight of the enzymatically hydrolyzed composite pulp with a composite fermentation agent into the enzymatically hydrolyzed composite pulp, and then fermenting at 35° C. for 70 hours. After the fermentation is completed, filtering and sterilizing are performed to obtain the medicinal mulberry-lemon composite enzyme; The composite fermentation agent is composed of 3 parts by weight of Lactobacillus plantarum N13, 2 parts by weight of Lactobacillus bulgaricus, 1 part by weight of Lactobacillus helveticus, 2 parts by weight of Leuconostoc mesenteroides subsp. mesenteroides and 1 part by weight of Streptococcus thermophilus; S4: Preparation of mint-flavored whitening toothpaste S4.1: Add 10 parts by weight of glycerol, 5 parts by weight of sorbitol and 50 parts by weight of deionized water into a stirring pot, and then stir at 50 r / min for 10 min to mix thoroughly, then add 1 part by weight of sodium carboxymethyl cellulose, and stir at 100 r / min for 10 min, then add 1 part by weight of cocamidopropyl betaine and 20 parts by weight of hydrated silica, and stir at 150 r / min for 10 min to obtain a toothpaste base; S4.2: Add 0.3 parts by weight of hyaluronic acid, 3 parts by weight of medicinal mulberry lemon complex enzyme, 2 parts by weight of lactoferrin-licorice polysaccharide copolymer complex, 2 parts by weight of tannic acid nanocellulose composite particles, and 0.3 parts by weight of mint essence to the toothpaste base, stir and mix at 200 r / min for 30 minutes, maintain bubbling at a vacuum degree of ≥0.094 MPa for 2 minutes, discharge the material, and fill it to obtain a mint-flavored whitening toothpaste.

[0025] Example 2 A preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition, such as Figure 1 As shown, the following steps are included: S1: Preparation of lactoferrin-licorice polysaccharide copolymer complex S1.1: Grind the licorice root and pass it through a 100-mesh sieve. Then, add the sieved powder into 95% (v / v) ethanol and defatting by stirring at 70°C for 3 hours. Then, centrifuge at 2000 r / min for 10 minutes and dry to obtain defatted licorice powder. S1.2: Add the defatted licorice powder to 5 times the amount of deionized water, extract at 90°C for 2 hours, and then centrifuge at 2000r / min to obtain a filter residue and a first filtrate. Add the filter residue to 5 times the amount of deionized water again, extract at 90°C for 2 hours, and then centrifuge at 2000r / min to obtain a second filtrate. Concentrate the first filtrate and the second filtrate under reduced pressure, and precipitate with 80% (v / v) anhydrous ethanol at 4°C for 12 hours. Then dry the precipitate and deproteinize to obtain licorice polysaccharide. S1.3: Glycyrrhiza polysaccharide and lactoferrin were added to deionized water respectively, stirred for 2 hours, and then placed at 4°C for 12 hours to obtain a glycyrrhiza polysaccharide solution and a lactoferrin solution with a concentration of 10 mg / mL. The glycyrrhiza polysaccharide solution and the lactoferrin solution were mixed in equal proportions, the pH was adjusted to 7.0, and then reacted at 80°C for 4 hours. After the reaction was completed, the mixture was rapidly cooled in an ice water bath to obtain a lactoferrin-glycyrrhiza polysaccharide copolymer complex; S2: Preparation of tannic acid nanocellulose composite particles S2.1: 8 parts by weight of cellulose nanofibers are added to 550 parts by weight of deionized water, and the mixture is stirred at 200 r / min for 5 minutes to obtain a cellulose nanofiber solution; 2 parts by weight of tannic acid are added to 5 parts by weight of deionized water, and the mixture is stirred at 200 r / min for 5 minutes to obtain a tannic acid solution; S2.2: Add the tannic acid solution dropwise to the cellulose nanofiber solution, then add 3 parts by weight of hydrochloric acid solution, and then stir and mix under magnetic stirring at 60°C for 2 hours. After the reaction is completed, centrifuge at 8000 rpm for 5 minutes, and then centrifuge at 12000 rpm for 5 minutes. Wash the precipitate twice with anhydrous ethanol and deionized water, respectively, and finally freeze it in a refrigerator for 12 hours, and then freeze-dry it to obtain tannic acid nanocellulose composite particles; The hydrochloric acid solution is a hydrochloric acid solution obtained by dissolving 100 µL of concentrated hydrochloric acid in 1 mL of deionized water; S3: Preparation of medicinal mulberry lemon compound enzyme S3.1: Select fresh medicinal mulberry and lemon, wash them respectively, then add the medicinal mulberry and lemon in a mass ratio of 2:1 to 4 times the amount of deionized water, squeeze the juice and homogenize to obtain a homogenate, then add 12% of the total mass of the homogenate of white sugar, stir and mix evenly to obtain a composite fruit pulp; S3.2: adding 0.3% pectinase to the composite fruit pulp, and then ultrasonically treating it at 300W and 43℃ for 1.5h, and then inactivating the enzyme at 90℃ for 20min to obtain the enzymatically hydrolyzed composite fruit pulp; S3.3: inoculating 0.2% of the total weight of the enzymatically hydrolyzed composite pulp with a composite fermentation agent into the enzymatically hydrolyzed composite pulp, and then fermenting at 35° C. for 70 hours. After the fermentation is completed, filtering and sterilizing are performed to obtain the medicinal mulberry-lemon composite enzyme; The composite fermentation agent is composed of 4 parts by weight of Lactobacillus plantarum N13, 1 part by weight of Lactobacillus bulgaricus, 0.5 part by weight of Lactobacillus helveticus, 1 part by weight of Leuconostoc mesenteroides subsp. mesenteroides and 0.5 part by weight of Streptococcus thermophilus; S4: Preparation of mint-flavored whitening toothpaste S4.1: Add 12 parts by weight of glycerol, 8 parts by weight of sorbitol and 60 parts by weight of deionized water into a stirring pot, and then stir at 50 r / min for 10 min to mix thoroughly, then add 2 parts by weight of sodium carboxymethyl cellulose, and stir at 100 r / min for 10 min, then add 2 parts by weight of cocamidopropyl betaine and 23 parts by weight of hydrated silica, and stir at 150 r / min for 10 min to obtain a toothpaste base; S4.2: Add 0.5 parts by weight of hyaluronic acid, 5 parts by weight of medicinal mulberry lemon complex enzyme, 3 parts by weight of lactoferrin-licorice polysaccharide copolymer complex, 3 parts by weight of tannic acid nanocellulose composite particles, and 0.5 parts by weight of mint essence to the toothpaste base, stir and mix at 200 r / min for 20 minutes, maintain bubbling at a vacuum degree of ≥0.094 MPa for 2 minutes, discharge the material, and fill it to obtain a mint-flavored whitening toothpaste.

[0026] Example 3 A preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition, such as Figure 1 As shown, the following steps are included: S1: Preparation of lactoferrin-licorice polysaccharide copolymer complex S1.1: Grind the licorice root and pass it through a 120-mesh sieve. Then, add the sieved powder into 95% (v / v) ethanol and defat it by stirring at 72°C for 4 hours. Then, centrifuge it at 3000 r / min for 12 minutes and dry it to obtain defatted licorice powder. S1.2: Add defatted licorice powder to 3 times the amount of deionized water, extract at 95°C for 3 hours, then centrifuge at 3000r / min to obtain a filter residue and a first filtrate, add the filter residue again to 5 times the amount of deionized water, extract at 95°C for 3 hours, then centrifuge at 3000r / min to obtain a second filtrate, concentrate the first filtrate and the second filtrate under reduced pressure, and use 80% (v / v) anhydrous ethanol at 5°C for 12-14 hours, then dry the precipitate and deproteinize to obtain licorice polysaccharide; S1.3: Glycyrrhiza polysaccharide and lactoferrin were added to deionized water respectively, stirred for 3 hours, and then placed at 5°C for 14 hours to obtain a glycyrrhiza polysaccharide solution and a lactoferrin solution with a concentration of 10 mg / mL. The glycyrrhiza polysaccharide solution and the lactoferrin solution were mixed in equal proportions, the pH was adjusted to 7.0, and then reacted at 90°C for 4 hours. After the reaction was completed, the mixture was rapidly cooled in an ice water bath to obtain a lactoferrin-glycyrrhiza polysaccharide copolymer complex; S2: Preparation of tannic acid nanocellulose composite particles S2.1: adding 5 parts by weight of cellulose nanofibers to 500 parts by weight of deionized water, stirring and mixing at 300 r / min for 10 min to obtain a cellulose nanofiber solution, adding 1 part by weight of tannic acid to 4 parts by weight of deionized water, stirring and mixing at 300 r / min for 10 min to obtain a tannic acid solution; S2.2: Add the tannic acid solution dropwise to the cellulose nanofiber solution, then add 2 parts by weight of hydrochloric acid solution, and then stir and mix under magnetic stirring at 70°C for 3 hours. After the reaction is completed, centrifuge at 10,000 rpm for 10 minutes, and then centrifuge at 15,000 rpm for 10 minutes. Wash the precipitate with anhydrous ethanol and deionized water for 3 times, and finally freeze it in a refrigerator for 14 hours, and then freeze-dry it to obtain tannic acid nanocellulose composite particles; The hydrochloric acid solution is a hydrochloric acid solution obtained by dissolving 100 µL of concentrated hydrochloric acid in 1 mL of deionized water; S3: Preparation of medicinal mulberry lemon compound enzyme S3.1: Select fresh medicinal mulberry and lemon, wash them respectively, then add the medicinal mulberry and lemon in a mass ratio of 1:1 to 3 times the amount of deionized water, squeeze the juice and homogenize to obtain a homogenate, then add 10% of the total mass of the homogenate of white sugar, stir and mix evenly to obtain a composite fruit pulp; S3.2: 0.28% pectinase was added to the composite fruit pulp, followed by ultrasonic treatment at 330W and 45°C for 2h, followed by enzyme inactivation treatment at 93°C for 30min to obtain enzymatically hydrolyzed composite fruit pulp; S3.3: Inoculate the enzymatically hydrolyzed composite pulp with a composite fermentation agent of 0.1% of the total mass of the enzymatically hydrolyzed composite pulp, and then ferment at 37°C for 72 hours. After the fermentation is completed, filter and sterilize to obtain the medicinal mulberry-lemon composite enzyme; The composite fermentation agent is composed of 3 parts by weight of Lactobacillus plantarum N13, 2 parts by weight of Lactobacillus bulgaricus, 1 part by weight of Lactobacillus helveticus, 2 parts by weight of Leuconostoc mesenteroides subsp. mesenteroides and 1 part by weight of Streptococcus thermophilus; S4: Preparation of mint-flavored whitening toothpaste S4.1: Add 10 parts by weight of glycerol, 5 parts by weight of sorbitol and 50 parts by weight of deionized water into a stirring pot, and then stir at 100 r / min for 15 min to mix thoroughly, then add 1 part by weight of sodium carboxymethyl cellulose, and stir at 200 r / min for 15 min, then add 1 part by weight of cocamidopropyl betaine and 20 parts by weight of hydrated silica, and stir at 200 r / min for 15 min to obtain a toothpaste base; S4.2: Add 0.3 parts by weight of hyaluronic acid, 3 parts by weight of medicinal mulberry lemon complex enzyme, 2 parts by weight of lactoferrin-licorice polysaccharide copolymer complex, 2 parts by weight of tannic acid nanocellulose composite particles, and 0.3 parts by weight of mint essence to the toothpaste base, stir and mix at 300 r / min for 30 minutes, maintain bubbling at a vacuum degree of ≥0.094 MPa for 3 minutes, discharge the material, and fill it to obtain a mint-flavored whitening toothpaste.

[0027] Comparative Example 1 Compared with Example 1, the difference of Comparative Example 1 is that the lactoferrin-licorice polysaccharide copolymer complex in steps S1 and S4.2 is removed in Comparative Example 1, and the other steps remain unchanged to prepare a mint-flavored whitening toothpaste, which is recorded as Comparative Example 1.

[0028] Comparative Example 2 Compared with Example 1, the difference of Comparative Example 2 is that Comparative Example 2 removes the tannic acid nano-cellulose composite particles in step S2 and step S4.2, and the other steps remain unchanged to prepare a mint-flavored whitening toothpaste, which is recorded as Comparative Example 2.

[0029] Comparative Example 3 Compared with Example 1, the difference of Comparative Example 3 is that Comparative Example 3 removes the medicinal mulberry-lemon compound enzyme in step S3 and step S4.2, and the other steps remain unchanged to prepare the mint-flavored whitening toothpaste, which is recorded as Comparative Example 3.

[0030] Comparative Example 4 Compared with Example 1, the difference of Comparative Example 4 is that the medicinal mulberry in step S3.1 is removed in Comparative Example 4, and the other steps remain unchanged to prepare the mint-flavored whitening toothpaste, which is recorded as Comparative Example 4.

[0031] Comparative Example 5 Compared with Example 1, the difference of Comparative Example 5 is that the lemon in step S3.1 is removed in Comparative Example 5, and the other steps remain unchanged to prepare the mint-flavored whitening toothpaste, which is recorded as Comparative Example 5.

[0032] Oral mucosal irritation test: According to YY / T0127.3-2009, biological evaluation of oral medical devices, unit 2 test methods, oral mucosal irritation test requirements, the mint flavored whitening toothpaste prepared in Examples 1-3 was tested for irritation index. The test results are shown in Table 1.

[0033] Table 1. Results of irritation index determination in Examples 1-3 It can be seen from the data in Table 1 that the mint-flavored whitening toothpaste prepared by the present invention is highly safe and has no irritation to the oral mucosa.

[0034] Evaluation of antibacterial effect: The antibacterial rates of the mint-flavored whitening toothpastes prepared in Examples 1-3 and Comparative Examples 1-5 against Streptococcus mutans, Porphyromonas gingivalis, Prevotella intermedia, and Fusobacterium nucleatum were tested. The experiment was repeated 3 times and the average value was taken. The results are shown in Table 2.

[0035] Table 2. Determination results of antibacterial rate of mint flavored whitening toothpastes prepared in Examples 1-3 and Comparative Examples 1-5 As can be seen from the data of Table 2, the mint flavor whitening toothpaste prepared by the present invention has an antibacterial rate of Streptococcus mutans, Porphyromonas gingivalis, Prevotella intermedia, and Fusobacterium nucleatum higher than 99%, indicating that the mint flavor whitening toothpaste prepared by the present invention has a good antibacterial effect on common oral pathogens such as Streptococcus mutans, Porphyromonas gingivalis, Prevotella intermedia, and Fusobacterium nucleatum, and can fundamentally inhibit bacterial growth, avoid the recurrence of halitosis, and achieve the effect of long-term inhibition of halitosis. As can be seen from the data of Comparative Example 1, adding lactoferrin-licorice polysaccharide copolymer complex can more effectively target the odor-producing bacteria in the oral cavity, such as Streptococcus mutans, Porphyromonas gingivalis, etc., reduce the number of these bacteria, thereby inhibiting the generation of halitosis from the root. As can be seen from the data of Comparative Example 2, tannic acid nano-cellulose composite particles have a significant inhibitory effect on the common harmful bacteria of the oral cavity, and can also improve the antibacterial effect of mint flavor whitening toothpaste, thereby achieving the effect of long-term inhibition of halitosis. From the data of comparative examples 3-5, it can be seen that the added medicinal mulberry lemon compound enzyme can reduce the number of bacteria in the oral cavity and achieve an antibacterial effect, and the medicinal mulberry lemon has a certain synergistic antibacterial effect.

[0036] Whitening effect evaluation: Preparation of staining solution: First, dissolve gastric mucin with hot water, then add coffee and black tea and stir evenly, let it cool, and add ferric chloride solution stored at 4°C before use. The final concentration of each component is: gastric mucin 3g / L, coffee 5g / L, black tea 5g / L, ferric chloride 0.05g / L.

[0037] The acid-etched bovine tooth enamel blocks were soaked in a 37°C dyeing solution for one week, taken out and smoked with tobacco for 30 minutes to obtain dyed bovine tooth enamel blocks. The blocks were then randomly divided into 8 groups, and the mint-flavored whitening toothpastes prepared in Examples 1-3 and Comparative Examples 1-5 were used to simulate brushing for 800 times, and then washed and dried.

[0038] Measure the color of tooth enamel before brushing , tooth enamel color after brushing , and calculate the time before and after brushing Difference of values The results are shown in Table 3.

[0039] Table 3. Whitening effect of mint flavored whitening toothpaste prepared in Examples 1-3 and Comparative Examples 1-5 It can be seen from the data in Table 3 that the mint-flavored whitening toothpaste prepared in Examples 1-3 has a good whitening effect. It can be seen from the data in Comparative Examples 1-2 that the addition of lactoferrin-licorice polysaccharide copolymer complex and tannic acid nanocellulose composite particles can improve the whitening effect of the mint-flavored whitening toothpaste. It can be seen from the data in Comparative Examples 3-5 that the addition of mulberry-lemon composite enzyme can effectively improve the whitening effect of the mint-flavored whitening toothpaste, and the composite enzyme prepared by composite preparation of mulberry and lemon has a better effect than that of a single ingredient.

[0040] Toothpaste stability determination: According to GB / T8372, the mint flavored whitening toothpastes prepared in Examples 1-3 were subjected to a paste stability test. The test results are shown in Table 4.

[0041] Table 4. Results of toothpaste stability tests in Examples 1-3 It can be seen from the data in Table 4 that the mint flavored whitening toothpaste prepared by the present invention has good stability.

[0042] Figure 2In the electrophoresis diagram, lane 1 is lactoferrin, lane 2 is a physical mixture of lactoferrin and glycyrrhiza polysaccharide, lane 3 is the lactoferrin-licorice polysaccharide copolymer complex of Example 1, lane 4 is the lactoferrin-licorice polysaccharide copolymer complex of Example 2, lane 5 is the lactoferrin-licorice polysaccharide copolymer complex of Example 3, and lane 6 is the standard protein. It can be seen from the electrophoresis diagram that new bands are generated at the tops of lanes 3-5, proving that high molecular polymers are generated in Examples 1-3, indicating that lactoferrin-licorice polysaccharide copolymer complexes are successfully synthesized in Examples 1-3.

[0043] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A preparation process for a mint-flavored whitening toothpaste for long-term halitosis inhibition, characterized in that: The steps include: S1: Preparation of lactoferrin-licorice polysaccharide copolymer complex: Licorice is defatted and extracted with deionized water to obtain licorice polysaccharide, and then the licorice polysaccharide solution and the lactoferrin solution are mixed and the pH is adjusted to 7.0, and then the mixture is reacted at 70-90° C. for 4-5 hours to obtain a lactoferrin-licorice polysaccharide copolymer complex; S2: Preparation of tannic acid nanocellulose composite particles: The tannic acid solution is added dropwise to the cellulose nanofiber solution, and then a hydrochloric acid solution is added, mixed and reacted, and then centrifuged to prepare tannic acid nanocellulose composite particles; S3: Preparation of medicinal mulberry lemon compound enzyme: The medicinal mulberry and lemon are added into deionized water in a mass ratio of 1-2:1, and then white sugar is added to homogenize, and then enzymolysis and fermentation are performed to prepare the medicinal mulberry and lemon composite enzyme; S4: Preparation of mint flavored whitening toothpaste: A toothpaste base is prepared by mixing glycerin, sorbitol, sodium carboxymethyl cellulose, cocamidopropyl betaine, hydrated silica and deionized water, and then 0.3-0.5 weight parts of hyaluronic acid, 3-5 weight parts of medicinal mulberry lemon composite enzyme, 2-3 weight parts of lactoferrin-licorice polysaccharide copolymer complex, 2-3 weight parts of tannic acid nanocellulose composite particles and 0.3-0.5 weight parts of mint essence are added to the toothpaste base and mixed to prepare a mint-flavored whitening toothpaste.

2. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 1, characterized in that: Step S1: Preparation of lactoferrin-licorice polysaccharide copolymer complex, specifically comprising the following steps: S1.1: Grind the licorice root and pass it through a 100-120 mesh sieve. Then, add the sieved powder into 95% (v / v) ethanol and stir to defat at 70-72°C for 3-4 hours. Then, centrifuge at 2000-3000 r / min for 10-12 minutes and dry to obtain defatted licorice powder. S1.2: Add defatted licorice powder to 3-5 times the amount of deionized water, extract at 90-95°C for 2-3h, then centrifuge at 2000-3000r / min to obtain a filter residue and a first filtrate, add the filter residue to 3-5 times the amount of deionized water again, extract at 90-95°C for 2-3h, then centrifuge at 2000-3000r / min to obtain a second filtrate, concentrate the first filtrate and the second filtrate under reduced pressure, and precipitate with 80% (v / v) anhydrous ethanol at 4-5°C for 12-14h, then dry the precipitate and deproteinize to obtain licorice polysaccharide; S1.3: Add glycyrrhizin polysaccharide and lactoferrin into deionized water respectively, stir for 2-3 hours, and then place at 4-5℃ for 12-14 hours to obtain glycyrrhizin polysaccharide solution and lactoferrin solution with a concentration of 10 mg / mL. Mix the glycyrrhizin polysaccharide solution and lactoferrin solution in equal proportions, adjust the pH to 7.0, and then react at 70-90℃ for 4-5 hours. After the reaction is completed, cool rapidly in an ice water bath to obtain a lactoferrin-glycyrrhizin polysaccharide copolymer complex.

3. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 2, characterized in that: Step S2: Preparation of tannic acid nanocellulose composite particles, specifically comprising the following steps: S2.1: adding 5-8 parts by weight of cellulose nanofibers to 500-550 parts by weight of deionized water, stirring and mixing at 200-300 r / min for 5-10 min to obtain a cellulose nanofiber solution, adding 1-2 parts by weight of tannic acid to 4-5 parts by weight of deionized water, stirring and mixing at 200-300 r / min for 5-10 min to obtain a tannic acid solution; S2.2: Add tannic acid solution dropwise to the cellulose nanofiber solution, then add 2-3 parts by weight of hydrochloric acid solution, and then mix with magnetic stirring at 60-70°C for 2-3 hours. After the reaction is completed, centrifuge at 8000-10000rpm for 5-10min, and then centrifuge at 12000-15000rpm for 5-10min. Wash the precipitate with anhydrous ethanol and deionized water for 2-3 times respectively, and finally freeze it in a refrigerator for 12-14 hours, and then freeze-dry it to obtain tannic acid nanocellulose composite particles.

4. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 3, characterized in that: Step S3 is the preparation of the medicinal mulberry lemon compound enzyme, which specifically comprises the following steps: S3.1: Select fresh medicinal mulberry and lemon, wash them respectively, then add the medicinal mulberry and lemon in a mass ratio of 1-2:1 to 3-4 times the amount of deionized water, squeeze the juice and homogenize to obtain a homogenate, then add white sugar, stir and mix evenly to obtain a composite fruit pulp; S3.2: adding pectinase to the composite fruit pulp, and then ultrasonically treating it at 300-330W and 43-45°C for 1.5-2h, and then inactivating the enzyme at 90-93°C for 20-30min to obtain the enzymatically hydrolyzed composite fruit pulp; S3.3: Inoculate 0.1-0.2% of the total mass of the enzymatically hydrolyzed composite pulp with a composite fermentation agent, and then ferment at 35-37°C for 70-72h. After the fermentation is completed, filter and sterilize to obtain the medicinal mulberry-lemon composite enzyme.

5. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 4, characterized in that: Step S4 is the preparation of mint flavored whitening toothpaste, specifically comprising the following steps: S4.1: Add 10-12 parts by weight of glycerol, 5-8 parts by weight of sorbitol and 50-60 parts by weight of deionized water into a stirring pot, then stir at 50-100 r / min for 10-15 min, mix thoroughly, then add 1-2 parts by weight of sodium carboxymethyl cellulose, stir at 100-200 r / min for 10-15 min, then add 1-2 parts by weight of cocamidopropyl betaine and 20-23 parts by weight of hydrated silica, stir at 150-200 r / min for 10-15 min, to obtain a toothpaste base; S4.2: Add 0.3-0.5 parts by weight of hyaluronic acid, 3-5 parts by weight of medicinal mulberry lemon complex enzyme, 2-3 parts by weight of lactoferrin-licorice polysaccharide copolymer complex, 2-3 parts by weight of tannic acid nanocellulose composite particles, and 0.3-0.5 parts by weight of mint essence to the toothpaste base, stir and mix at 200-300 r / min for 20-30 min, maintain bubbling at a vacuum degree of ≥0.094 MPa for 2-3 min, discharge the material, and fill it to obtain a mint-flavored whitening toothpaste.

6. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 3, characterized in that: The hydrochloric acid solution in step S2.2 is specifically a hydrochloric acid solution obtained by dissolving 100 µL of concentrated hydrochloric acid in 1 mL of deionized water.

7. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 4, characterized in that: The amount of white sugar added in step S3.1 is 10-12% of the total mass of the homogenate.

8. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 4, characterized in that: In step S3.2, the amount of pectinase added is 0.28-0.3% of the total mass of the composite fruit pulp.

9. The preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition according to claim 4, characterized in that: In step S3.3, the composite starter culture comprises 3-4 parts by weight of Lactobacillus plantarum N13, 2-1 parts by weight of Lactobacillus bulgaricus, 1-0.5 parts by weight of Lactobacillus helveticus, 2-1 parts by weight of Leuconostoc mesenteroides subsp. mesenteroides and 1-0.5 parts by weight of Streptococcus thermophilus.

10. A mint-flavored whitening toothpaste for long-term halitosis inhibition, characterized in that: The toothpaste is prepared by the preparation process of a mint-flavored whitening toothpaste for long-term halitosis inhibition as described in any one of claims 1 to 9.

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