Mild gum-protecting toothpaste and preparation method thereof

Abstract

The invention relates to mild gum-protecting toothpaste and a preparation method thereof. The mild gingiva-protecting toothpaste comprises the following components in percentage by weight: 20-50% of a friction agent; 0.3 to 3% of xanthan gum; 0.5 to 10% of polyethylene glycol; 0.5 to 5% of a nonionic surfactant compound; 15-60% of a wetting agent; 0.3 to 3.5 percent of chelating agent; 0.05%-0.5% of a preservative; 0-1% of a sweetening agent; 0-2% of a flavoring agent; and the balance of deionized water. Wherein the nonionic surfactant compound comprises at least two kinds of nonionic surfactants. According to the scheme provided by the invention, the toothpaste product is small in irritation to the oral cavity and high in safety, and can achieve the effect of K12 in the aspect of foaming ability, so that the toothpaste has a mild cleaning effect.

Description

Technical Field

[0001] The present application relates to the technical field of daily chemical products, and in particular to a mild gum-protecting toothpaste and a preparation method thereof. Background Art

[0002] Toothpaste plays a vital role in daily oral care, mainly used to clean teeth, prevent oral diseases and keep breath fresh.

[0003] The main method of maintaining oral hygiene is brushing teeth, applying toothpaste to the tooth surface in a frictional manner, and using mechanical friction to clean the teeth and their surroundings. Common toothpastes are usually composed of a variety of ingredients such as abrasives, moisturizers, thickeners, foaming agents, flavoring agents, sweeteners, preservatives, etc. Among them, foaming agents are also called surfactants, which can play the role of foaming, emulsification, and auxiliary cleaning and decontamination, and are an indispensable ingredient in toothpaste.

[0004] The most common toothpaste surfactant on the market is sodium lauryl sulfate (K12), which has the advantages of short foaming time and strong foaming ability, so it is widely used in toothpaste formulas. However, K12 is highly irritating to the oral mucosa and can cause damage to the oral mucosa. In addition, K12 is in powder form and is very easy to scatter during production operations, causing damage to the respiratory tract of production personnel and bringing production safety issues.

[0005] Therefore, how to apply surfactants with low irritation, high safety and foaming ability not lower than K12 in toothpaste formulation is a problem that needs to be solved at present. Summary of the invention

[0006] In order to solve or partially solve the problems existing in the related art, the present application provides a mild gum protection toothpaste and a preparation method thereof. The toothpaste product has little irritation to the oral cavity, high safety, and can achieve the K12 effect in terms of foaming ability, so that the toothpaste has a mild cleaning effect.

[0007] The first aspect of the present application provides a mild gum protection toothpaste, comprising the following components in percentage by weight: Friction agent 20~50% Xanthan gum 0.3~3% Polyethylene glycol 0.5~10% Nonionic surfactant complex 0.5~5% Wetting agent 15~60% Chelating agent 0.3~3.5% Preservatives 0.05~0.5% Sweetener 0~1% Fragrance 0~2% The balance is deionized water; Wherein, the nonionic surfactant complex comprises at least two nonionic surfactants.

[0008] A nonionic surfactant complex is obtained by arbitrarily combining at least two nonionic surfactants. The complex has surfactant diversity and utilizes the synergy between multiple nonionic surfactants to have good surface activity and improved foaming performance when used in toothpaste. Furthermore, since the nonionic surfactant can form a stable film at the oil-water interface, reduce interfacial tension, and have a good wetting effect, it has good compatibility with other ingredients in toothpaste. At the same time, since most of the nonionic surfactants are converted from natural ingredients, or are produced by organisms, or extracted from plants, they have high biodegradability, low toxicity, are environmentally friendly, highly safe, and low irritation. When used in toothpaste, they have little irritation to the oral mucosa, achieving the effects of mild decontamination and gum protection.

[0009] In some optional embodiments, the nonionic surfactant complex comprises a combination of one or more of glycolipid surfactants, glycoside surfactants and plant saponin surfactants. The glycolipid surfactant is selected from one or more of trehalose lipids, rhamnolipids, sophorolipids and mannosyl erythritol lipids; the glycoside surfactant is selected from alkyl glycosides; and the plant saponin surfactant is selected from one or more of soapberry extract, camellia seed extract and saponin extract.

[0010] Among them, glycolipid surfactants have good biocompatibility and biodegradability, low toxicity, strong specificity, high antibacterial properties, and can still maintain good surface activity under extreme conditions. For example, rhamnolipid is a bacterial biosurfactant, generally produced by Pseudomonas aeruginosa, composed of long-chain fatty acids or hydroxylated fatty acids, which not only has good foaming properties, but also has good antibacterial properties, can inhibit the formation of oral biofilm, and has good biodegradability, is green and environmentally friendly, and can be used as an emulsifier, antibacterial agent, foaming agent and wetting agent.

[0011] Glycoside surfactants such as alkyl glycosides are synthesized by condensation reaction of glucose and fatty alcohol converted from natural plant starch. They have the characteristics of high surface activity, low surface tension, strong wetting ability, strong detergency, rich and delicate foam, non-toxic and non-irritating, etc., and they have good compatibility with other non-ionic surfactants and other components in toothpaste, and can produce synergistic effects with other non-ionic surfactants to improve foaming stability.

[0012] Plant saponin surfactants are 100% natural, green, environmentally friendly, safe and mild, with no or low irritation to the skin. For example, the main components of soapberry extract are triterpenoid saponins and sesquiterpenoid glycoside compounds, which have strong surface activity, and are green, non-toxic, mild and safe, and easy to degrade, as well as anti-inflammatory, antibacterial and sterilization effects; the main components of camellia seed extract are oil, starch, protein, tea seed polysaccharides, polyphenols, flavonoids, saponins, tissue fibers and other components. In addition, it also contains camellia glycosides, camellia saponins, tea polyphenols and other biologically active substances. Generally, pentacyclic triterpenoid compounds extracted from Camellia plants such as camellia oil and tea trees are collectively referred to as tea saponins. The surface of tea saponins is composed of triterpenoids, steroids or steroid-alkaloid groups. The hydrophobic structure, which makes it have good foaming, emulsification and wetting effects.

[0013] In some optional embodiments, it is characterized in that: the non-ionic surfactant complex comprises rhamnolipid and alkyl glycoside, and the mass ratio of rhamnolipid to alkyl glycoside is (1-5): (1-5); or, The nonionic surfactant complex comprises camellia seed extract and alkyl glycoside, and the mass ratio of the camellia seed extract to the alkyl glycoside is (1-5): (1-5).

[0014] The non-ionic surfactant complex of the combination of rhamnolipid and alkyl glycoside, camellia seed extract and alkyl glycoside, and the strong compounding ability of alkyl glycoside enable rhamnolipid or camellia seed extract to maintain good compatibility with other components in toothpaste, exert good foaming properties, and can be stably used in toothpaste formulas, which are safe, mild and less irritating; in addition, rhamnolipid or camellia seed extract can also exert its antibacterial and antimicrobial properties in toothpaste formulas, and to a certain extent play the role of preservatives and prevent tooth decay.

[0015] In some optional embodiments, the mass ratio of the non-ionic surfactant complex to polyethylene glycol is (0.8~1.1):5.

[0016] In toothpaste formulas, polyethylene glycol is mainly used as a humectant ingredient, which helps to maintain the moisture of the toothpaste and improve the viscosity stability and product stability of the toothpaste; when polyethylene glycol is used in combination with a non-ionic surfactant complex, polyethylene glycol acts as a dispersant / solvent for the non-ionic surfactant complex, which also helps the non-ionic surfactant complex to be compatible with other components in the toothpaste formula, thereby improving the stability of the toothpaste formula.

[0017] In some optional embodiments, the friction agent includes bamboo cellulose and at least one of sugarcane silica and rice husk silica, and the particle size of the friction agent is 6-250 μm.

[0018] Bamboo cellulose, sugarcane silica and rice husk silica are all naturally derived plant abrasives with natural and safe ingredients. They are biodegradable and sustainable raw materials. They are non-chemical products that are non-irritating to the skin, safe and gentle, and suitable for people with oral problems or sensitive skin.

[0019] Furthermore, the particle size of bamboo cellulose is 120μm~250μm, and the particle size of sugarcane silica and rice husk silica is 6~58μm. Through two plant abrasives with different particle sizes, small-particle sugarcane silica and rice husk silica have low wear on tooth enamel, and their apparent density is greater than or equal to 0.3g / mL, and their iron content, lead content and arsenic content are much lower than traditional silica. The ingredients are safe, the adsorption performance is good, and it can be more compatible with other ingredients in toothpaste; large-particle bamboo cellulose has good cleaning performance. When the two are used together, they can effectively remove stains on the tooth surface without damaging the tooth enamel; moreover, the abrasive used in combination has better temperature stability, stable chemical properties in the oral environment, and will not react adversely with other ingredients in toothpaste. It can also use its good adsorption to assist in the adsorption and removal of stains on the tooth surface, achieving a good cleaning effect. Plant abrasives with a particle size in the range of 1-250μm have a large particle span. Plant abrasives with different particle sizes can also exert different friction and cleaning effects at different locations on the tooth surface, adapting to different cleaning needs at different locations, thereby achieving the effect of comprehensive cleaning of teeth without damaging tooth enamel.

[0020] In some optional embodiments, the mass ratio of the bamboo cellulose, sugarcane silica, and rice husk silica is (1-2): 1:1.

[0021] The reasonable ratio of three different plant abrasives can not only play a good friction cleaning effect, but also be evenly distributed. When used in combination with non-ionic surfactants, it can provide high adsorption energy at the fluid interface, thereby improving the structural strength and viscosity of instant noodles and improving the stability of instant noodles. At this time, the abrasives, xanthan gum and polyethylene glycol play the role of foam stabilizers.

[0022] In some optional embodiments, the mass ratio of the abrasive, xanthan gum and non-ionic surfactant complex is (25-35):1:2.

[0023] Xanthan gum acts as a thickener in toothpaste formulas, which can increase the viscosity and consistency of toothpaste, maintain the stability of toothpaste on the toothbrush, and help stabilize the abrasive components in toothpaste, prevent the precipitation of abrasive solid powder, and reduce the wear of abrasives on the tooth surface. At the same time, when xanthan gum is used in combination with abrasives, it plays a role in stabilizing foam and improving the foaming performance of the toothpaste formula.

[0024] In some optional embodiments, the wetting agent includes sorbitol and glycerol, and the mass ratio of sorbitol to glycerol is 4.5:1.

[0025] In addition to its moisturizing effect in toothpaste formula, which helps to maintain the moistness of toothpaste and maintain the shape and structure of toothpaste, sorbitol also has a certain degree of antiseptic effect, so it can reduce the addition of other antiseptic ingredients in toothpaste formula, with high safety, and can improve the compatibility of other ingredients in toothpaste formula, increase the viscosity of toothpaste, and make toothpaste have a double, comfortable and delicious sweet taste, which is conducive to the use of toothpaste. In addition to its moisturizing effect, glycerin in toothpaste formula also has the effect of thickening, stabilizing and increasing the sweetness of toothpaste, which can reduce the wear of abrasives on the tooth surface, making toothpaste products have a mild cleaning and gum protection effect.

[0026] The second aspect of the present application provides a method for preparing a mild gum protection toothpaste, comprising: Add the chelating agent, preservative and sweetener into deionized water and stir until completely dissolved; then add the wetting agent and part of polyethylene glycol, mix well and pour into the paste making machine; After mixing the friction agent and xanthan gum, add them into the paste making machine and control the vacuum degree to be within the range of (-0.04) MPa to (-0.08) MPa while stirring and mixing; The nonionic surfactant complex and the remaining polyethylene glycol are dispersed uniformly to obtain a premixed surfactant; The premixed surfactant and flavoring agent are added into a paste making machine, and the vacuum degree is controlled to be above 0.09 MPa for stirring and mixing, and then deaerated and filled to obtain a mild gum-protecting toothpaste.

[0027] The staged mixing of the components is beneficial to the fusion of the components, thereby improving the compatibility of the components and avoiding the impact of poor dispersion of solid powders such as abrasives on the stability of toothpaste products.

[0028] In some optional embodiments, the polyethylene glycol used in the premix of the non-ionic surfactant complex accounts for 50 wt % to 70 wt % of all polyethylene glycols.

[0029] Polyethylene glycol has a wetting effect when added to a paste making machine together with a wetting agent, and has a dispersing effect when premixed with a non-ionic surfactant complex, which helps the premixed surfactant to quickly mix with other components in the toothpaste formula when added to the paste making machine, thereby improving the compatibility between the components of the toothpaste product and improving the formula stability.

[0030] The technical solution provided by the present application may include the following beneficial effects: the surfactant in the toothpaste formula adopts a non-ionic surfactant complex, and the combined use of at least two non-ionic surfactants is used to provide a surfactant component that can be applied to toothpaste products with low irritation, high safety, and can achieve the K12 effect in terms of foaming ability, so that the toothpaste has the effect of gentle cleaning and safe gum protection.

[0031] By compounding a variety of abrasive materials, the hardness of the toothpaste product is balanced, and the particles with different friction coefficients can be used for friction cleaning at different positions of the teeth in the mouth, thereby achieving efficient, gentle cleaning with good cleaning effect and little damage to the gums. When used in combination with a non-ionic surfactant complex, it can not only effectively remove stains on the tooth surface, but also improve the stability of the foam, further improving the cleaning effect of the toothpaste.

[0032] It should be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Exemplary embodiments of the present application are described in more detail with reference to the accompanying drawings.

[0034] Figure 1 and Figure 2 It is a schematic diagram of the foam performance test results shown in the examples and comparative examples of the present application. DETAILED DESCRIPTION

[0035] To make the present invention easy to understand, the present invention will be described in detail below. However, before describing the present invention in detail, it should be understood that the present invention is not limited to the specific embodiments described. It should also be understood that the terms used herein are only for describing specific embodiments and are not intended to be limiting.

[0036] The terms used in this application are for the purpose of describing specific embodiments only and are not intended to limit this application. The singular forms of "a", "said" and "the" used in this application and the appended claims are also intended to include plural forms unless the context clearly indicates other meanings. It should also be understood that the term "and / or" used herein refers to and includes any or all possible combinations of one or more associated listed items.

[0037] Where a numerical range is provided, it is to be understood that each intermediate value between the upper and lower limits of the range and any other provisions or intermediate values ​​in the specified range is encompassed within the present invention. The upper and lower limits of these smaller ranges may be independently included in the smaller ranges and are also encompassed within the present invention, subject to any explicitly excluded limits in the specified range. Where a specified range includes one or two limits, the scope excluding any or both of those included limits is also encompassed within the present invention. In the description of the present application, the meaning of "multiple" is two or more, unless otherwise clearly and specifically limited.

[0038] Unless otherwise defined, all terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the invention belongs. Although any methods and materials or equivalent methods and materials described herein can also be used in the practice or testing of the present invention, preferred methods and materials are now described.

[0039] The most common toothpaste surfactant on the market is sodium lauryl sulfate (K12), which has the advantages of short foaming time and strong foaming ability, so it is widely used in toothpaste formulas. But at the same time, K12 is highly irritating to the oral mucosa and can cause damage to the oral mucosa. In addition, K12 is in powder form and is very easy to scatter during production operations, causing damage to the respiratory tract of production personnel and bringing production safety problems. However, most surfactants with lower irritation are not as good as K12 in terms of foaming, formula compatibility stability, and taste improvement.

[0040] The embodiment of the present application provides a mild gum protection toothpaste, whose surfactant adopts a non-ionic surfactant complex. By using at least two non-ionic surfactants in combination, a surfactant component with low irritation, high safety, and the ability to achieve the K12 effect in foaming ability is provided and applied to the toothpaste product, so that the toothpaste has the effect of mild cleaning and gum protection.

[0041] The mild gum protection toothpaste of the embodiment of the present application includes the following components in percentage by weight: Friction agent 20~50% Xanthan gum 0.3~3% Polyethylene glycol 0.5~10% Nonionic surfactant complex 0.5~5% Wetting agent 15~60% Chelating agent 0.3~3.5% Preservatives 0.05~0.5% Sweetener 0~1% Fragrance 0~2% The balance is deionized water; The nonionic surfactant complex comprises at least two nonionic surfactants.

[0042] In some specific embodiments, the abrasive may include bamboo cellulose and at least one of sugarcane silica and rice husk silica, and the particle size of the abrasive is 6~250μm; the wetting agent may be selected from sorbitol and glycerol; the chelating agent may be selected from sodium pyrophosphate; the preservative may be selected from sodium benzoate; the sweetener may be selected from sodium saccharin, etc.

[0043] That is, the mild gum protection toothpaste may include the following components in percentage by weight: Silicon dioxide 20~50% Xanthan gum 0.3~3% Polyethylene glycol ~80.5~10% Nonionic surfactant complex 0.5~5% Sorbitol 15~50% Glycerin 5~15% Sodium pyrophosphate 0.3~3.5% Sodium benzoate 0.05~0.5% Saccharin sodium 0~1% Fragrance 0~2% The balance was deionized water.

[0044] The flavoring agent may be, for example, a mint flavoring agent, a spearmint flavoring agent, a fruit flavoring agent, etc., which is not limited in the present application. The flavoring agent and the sweetener (such as sodium saccharin) in the formula may be deleted based on actual product requirements.

[0045] Furthermore, in the friction agent, the mass ratio of bamboo cellulose with a particle size of 120 μm to 250 μm, sugarcane silica with a particle size of 16 to 58 μm, and rice husk silica with a particle size of 6 to 14 μm is (1 to 2): 1:1; preferably 1:1:1.

[0046] In some specific embodiments, the mass ratio of the abrasive, xanthan gum and the non-ionic surfactant complex is (25-35):1:2, for example, 30:1:2.

[0047] In some specific embodiments, the nonionic surfactant complex may include a glycolipid surfactant and a glycoside surfactant, a glycolipid surfactant and a plant saponin surfactant, a glycoside surfactant and a plant saponin surfactant, or a combination of two glycolipid surfactants or two plant saponin surfactants.

[0048] For example, the nonionic surfactant complex may include rhamnolipid and alkyl glycoside, and the mass ratio of rhamnolipid to alkyl glycoside is (1-5): (1-5), preferably 1: 1. The nonionic surfactant complex may include camellia seed extract and alkyl glycoside, and the mass ratio of camellia seed extract to alkyl glycoside is (1-5): (1-5), preferably 1: 1. The nonionic surfactant complex may include saponin extract and alkyl glycoside, and the mass ratio of camellia seed extract to alkyl glycoside is (1-5): (1-5), preferably 1: 1.

[0049] The mass ratio of the nonionic surfactant complex to the polyethylene glycol is (0.8-1.1), preferably 1:5.

[0050] The wetting agent includes sorbitol and glycerin, and the mass ratio of sorbitol to glycerin is 4.5:1.

[0051] The mild gum protection toothpaste of the embodiment of the present application comprises the following steps: Add the chelating agent, preservative and sweetener into deionized water and stir until completely dissolved; then add the wetting agent and part of polyethylene glycol, mix well and pour into the paste making machine; After mixing the friction agent and xanthan gum, add them into the paste making machine and control the vacuum degree to be within the range of (-0.04) MPa to (-0.08) MPa while stirring and mixing; The nonionic surfactant complex and the remaining polyethylene glycol are dispersed uniformly to obtain a premixed surfactant; The premixed surfactant and flavoring agent are added into a paste making machine, and the vacuum degree is controlled to be above 0.09 MPa for stirring and mixing, and then deaerated and filled to obtain a mild gum-protecting toothpaste.

[0052] The polyethylene glycol used for premixing the nonionic surfactant complex accounts for 50 wt % to 70 wt %, for example 60 wt % of all polyethylene glycols.

[0053] In order to make the present invention easier to understand, the present invention will be further described in detail below in conjunction with examples, which are merely illustrative and are not intended to limit the scope of application of the present invention. The raw materials or components used in the present invention can be obtained by commercial routes or conventional methods unless otherwise specified.

[0054] Example 1: Friction and cleaning performance test 1.1 Sample preparation Example 1a (1) Add sodium pyrophosphate, sodium benzoate, and sodium saccharin to deionized water and stir until completely dissolved. Then add sorbitol, glycerol, and 50 wt% of all polyethylene glycol-8, stir for 5 minutes to form a liquid phase, and then pour into a paste making machine.

[0055] (2) Add silicon dioxide and xanthan gum into a container and stir evenly. Add into a paste making machine, turn on the scraper and double stirring of the paste making machine, control the vacuum degree within the range of (-0.04) MPa to (-0.08) MPa, and stir for 20 minutes.

[0056] (3) Pour alkyl polyglycoside (APG) and rhamnolipid into the premix barrel, add the remaining polyethylene glycol-8, stir and disperse, and set aside.

[0057] (4) Finally, add the flavoring agent, premixed alkyl polyglycoside (APG), and rhamnolipid into the paste making machine, control the vacuum degree to be above 0.09 MPa, stir for 15 minutes, degas, and fill to obtain a mild gum-protecting toothpaste.

[0058] Wherein, the toothpaste components include: Silicon dioxide 15% Sorbitol 45% Glycerin 10% Polyethylene glycol - 85% Xanthan gum 0.5% Sodium pyrophosphate 0.5% Sodium benzoate 0.3% Saccharin sodium 0.3% Alkyl polyglycoside (APG) 0.5% Rhamnolipid 0.5% Fragrance 1% Deionized water balance.

[0059] The friction agent uses 30μm~100μm silica.

[0060] Examples 1b-1g The difference from Example 1a is that the friction agent adopts the material shown in Table 1.

[0061] 1.2 Performance Testing The toothpaste products of Examples 1a to 1g were respectively prepared into 1% toothpaste slurries, and the friction value tests were respectively carried out with reference to GB / T 35832-2018 "Test method for friction value of toothpaste"; and the cleaning power tests were respectively carried out with reference to GB / T 43576-2023 "Laboratory test method for the effect of toothpaste on removal of exogenous stains of oral care products". The test results are shown in Table 1.

[0062] Table 1

[0063] Note: The particle size of silica is between 30μm and 100μm; the particle size of bamboo fiber powder is between 120μm and 250μm; the particle size of sugarcane silica is between 16μm and 58μm; the particle size of rice husk silica is between 6μm and 14μm.

[0064] 1.3 Result analysis: As shown in Table 1, it can be found that the friction values ​​of plant abrasives with different materials added are lower than that of silica alone, and the cleaning power of the abrasive compounded with bamboo cellulose and rice husk silica or sugarcane silica is close to that of silica, but the friction value is lower; the abrasive compounded with bamboo cellulose, rice husk silica and sugarcane silica has a low friction value and a high cleaning power, and has the same or better cleaning effect as silica. It can be considered that this embodiment achieves the effect of efficient cleaning while being gentle and not damaging to teeth.

[0065] Example 2: Foam and stimulation performance test 1.1 Sample preparation The friction agent used in the above embodiment 1g was selected, and the materials of the surfactant were adjusted as shown in Table 2 to prepare embodiments 2-3 and comparative examples 1-8.

[0066] Comparative Example 9 The difference from Example 1g is that xanthan gum is replaced by sodium carboxymethyl cellulose.

[0067] Table 2

[0068] Note: K12 is sodium lauryl sulfate; APG is alkyl glucoside; CGA is sodium cocoyl glutamate.

[0069] 1.2 Foam performance test The toothpaste products of Example 1g, Example 2, Example 3 and Comparative Examples 1-8 were respectively prepared into 1% toothpaste slurry, and the foam performance was analyzed by stirring using a foam analyzer, with a stirring time of 60s and a stirring speed of 1500rpm. Each sample was measured 3 times. The foam performance was compared in terms of 60s foaming amount and foam particle size. The measurement results are shown in Figure 2. Figure 1 and Figure 2 shown.

[0070] according to Figure 1 and Figure 2 From the comparison chart of Chinese toothpaste foaming combination, we can see that: 1. The foaming volume of the formula containing 1.5% K12 alone is not as good as that of the combination with APG. The foaming volume of the surfactant combination toothpaste of 1% K12 + 0.5% APG in 60s is up to 126ml; 2. The highest foaming volume in 60s for the foaming combination toothpaste containing natural surfactants is 110ml for 0.5% camellia seed extract + 0.5% APG and 104ml for 0.5% rhamnolipid + 0.5% APG. The foaming volume is comparable to that of the formula containing 1.5% K12.

[0071] In summary, the nonionic surfactant composite of the embodiment of the present application has good foaming performance, which is comparable to that of K12, and can replace K12 in terms of foaming performance.

[0072] 1.3 Formulation stability test The stability of toothpaste was determined by referring to the national standard GB / 8372-2017 toothpaste stability investigation method, with slight changes: 2 toothpaste samples of the above embodiment and comparative example were taken, one was stored at room temperature, and the other was placed in a constant temperature incubator at 45±1°C, and taken out at different time periods and compared with that at room temperature to check the stability; Compare the extruded paste with the sample stored at room temperature to see if the appearance, color, and smell are normal, and if there are any abnormal phenomena such as coarsening, water separation, etc. Then cut the tube to check if the paste has any abnormal phenomena such as granulation, coarsening, water separation, and shelling. If not, the stability is considered normal. Record the test results in Table 3.

[0073] Table 3 High temperature stability of toothpaste

[0074] The toothpaste samples shown in Table 3 were accelerated aged for 3 months at a temperature of 45°C. The relevant indicators of the products were tested as shown in the following: the test results of the samples in the embodiment showed normal, good overall stability, normal physical and chemical indicators, good compatibility of the formula components, no water-oil separation phenomenon, and excellent quality; and the toothpaste samples obtained by combining CGA with rhamnolipid or saponin extract showed that the surfactant combination formula described in the embodiment of the present application had a better improvement effect on the stability of the toothpaste formula. After the xanthan gum was replaced, the coarseness phenomenon appeared. It can be seen that even if the surfactant combination formula shown in Example 1g is used, the components of the toothpaste formula have changed, which affects the compatibility of the toothpaste formula as a whole, and thus affects the stability of the toothpaste formula.

[0075] 1.4 Sensory evaluation test The retention test was adopted, and each toothpaste of the embodiment and the comparative example was scored independently. The brushing interval of each toothpaste was not less than 30 minutes. The scoring standard was 1 point as the worst and 5 points as the best. 20 evaluators were invited to test brush and score the toothpastes with different surfactant combinations based on the four dimensions of overall taste, aroma intensity, foam volume, and foam density. The scoring table is shown in the following table.

[0076] Table 4 Evaluation of toothpaste taste with different surfactant combinations

[0077] The scoring results are shown in the following table.

[0078] Table 5 Evaluation of toothpaste taste

[0079] The toothpaste samples shown in the table above have relatively concentrated scores in different dimensions, all of which are above 3 points, which is above the medium level. Overall, the highest taste score is the gum protection toothpaste containing 0.5% camellia seed extract + 0.5% APG, followed by the gum protection toothpaste containing 1.5% K12.

[0080] In terms of overall taste, the highest-scoring toothpaste was the gum-protecting toothpaste with 0.5% camellia seed extract + 0.5% APG; in terms of aroma intensity, the best performing toothpaste was the gum-protecting toothpaste with 0.5% camellia seed extract + 0.5% APG, while the gum-protecting toothpastes with 0.5% rhamnolipid + 0.5% APG and 0.5% rhamnolipid + 0.5% CGA scored lower, mainly because the toothpaste had a unique fermentation smell, which is the special smell of rhamnolipid; in terms of foam index, the gum-protecting toothpaste with 0.5% camellia seed extract + 0.5% APG and the gum-protecting toothpaste with 0.5% rhamnolipid + 0.5% APG were basically on par with the gum-protecting toothpaste containing 1.5% K12 and the gum-protecting toothpaste containing 1.5% K12 + 0.5% APG, and the overall score difference was not much.

[0081] In summary, the combination of 0.5% camellia seed extract + 0.5% APG surfactant has the best taste evaluation and can replace the K12 formula. Although other surfactant combinations are slightly inferior in taste, smell, foam, etc., their overall acceptability scores are at an upper-middle level and can still be used as surfactant combinations to replace the K12 solution.

[0082] 1.5 Application irritation assessment test The toothpaste samples of Example 2, Comparative Example 1 and Comparative Example 2 were used for testing.

[0083] About 24 hours before the test, the hair on both sides of the rabbit's back spine was cut off without damaging the skin surface. The hair removal range was 3cm×3cm. 0.5mL of the test substance was applied to one side of the skin, with an application area of ​​2.5cm×2.5cm, and then covered with two layers of gauze (2.5cm×2.5cm) and one layer of cellophane, and then fixed with non-irritating adhesive tape and bandage. The other side of the skin was not treated as a control.

[0084] A closed test was used with an application time of 2 hours. After the test, the residual test substance was removed with pure water and the results were observed. The rabbits were scored according to the scoring criteria for skin irritation / corrosion test in the "Technical Specifications for Safety of Cosmetics" (2015 edition). The control area and the test area were treated in the same way.

[0085] Observe the skin reaction at the application site 1, 24, 48 and 72 hours after removing the test substance, and perform skin reaction scoring according to the skin irritation / corrosion test in the "Technical Specifications for Safety of Cosmetics" (2015 edition).

[0086] A comprehensive evaluation is conducted based on the average score of the test animals. The skin irritation intensity is determined according to the skin irritation / corrosion test in the Technical Specifications for Safety of Cosmetics (2015 edition) based on the average of the highest scores at each observation time point of 24, 48 and 72 hours, and other toxic effects besides irritation are observed.

[0087] Table 6 Record of skin irritation reaction of gum-protecting toothpaste containing (0.5% camellia seed + 0.5% APG) on rabbits

[0088] Table 7 Record of skin irritation reaction of rabbits to gum-protecting toothpaste containing (1.5% K12)

[0089] Table 8 Record of skin irritation reaction of rabbits to gum-protecting toothpaste containing (1% K12 + 0.5% APG)

[0090] 1.6 Application of oral mucosal irritation evaluation test The oral mucosal irritation test method refers to the pharmaceutical industry standard of the People's Republic of China YY / T0127.13-2018 "Biological Evaluation of Oral Medical Devices Part 13: Oral Mucosal Irritation Test". The irritation of the test samples to the oral mucosa of the hamster was evaluated by contacting the test samples (Example 2, Comparative Example 1, Comparative Example 2) with the buccal mucosa of the golden hamster.

[0091] Preparation of test samples and control samples: Place the test sample directly at the bottom of the hamster cheek pouch; inject the control sample directly at the bottom of the hamster cheek pouch. Contact method After the animal is anesthetized, turn the cheek pouch over and rinse with water to check whether there is any abnormality in the cheek pouch mucosa. Place the test sample in the right cheek pouch, which is the test side; place the control sample in the left cheek pouch, which is the control side. Place the test sample at the bottom of the cheek pouch on the test side and keep it in contact with the buccal mucosa for 10 minutes; inject the control sample at the bottom of the cheek pouch on the control side, and the contact time is the same as the test side.

[0092] After completion, remove the test sample and control sample, clean the mucosa and put it back into the cheek pouch. Repeat once every hour for a total of 4 times. After 24 hours, the animals were killed by intraperitoneal injection of an overdose of anesthetic. (2) Observe the clinical signs of the animals every day and record abnormal manifestations. ① Macroscopic observation: The animals were killed 24 hours after the start of the experiment. After removing the sample, observe the changes in the mucosa at the site where the sample was placed with the naked eye, and observe whether the buccal mucosa has congestion, swelling, erosion, ulcers and other reactions. Compare the mucosa on the test side and the control side, and score the clinical manifestations of the oral mucosa according to Table 8. The observation scores of each animal are added and then divided by the total number of observed animals to obtain the average score of each animal; ② Histological observation: After the animals were killed, the mucosa and surrounding tissues at the site of contact with the sample were taken, fixed in 10% formalin liquid, and histopathological sections were made. HE staining, histopathological observation and evaluation were performed. The treatment method of the control group was the same as that of the test group. The tissue reaction score of each animal was calculated according to the tissue reaction scoring system in Table 9; (3) Result evaluation: The irritation index was obtained by subtracting the average score of the control group from the average score of the experimental group. The degree of oral mucosal tissue reaction was graded according to the irritation index (Table 10). The final result evaluation was performed in combination with the results of naked eye observation.

[0093] Table 9 Oral mucosal reaction scoring system

[0094] Table 10 Oral mucosal tissue reaction scoring system

[0095] Table 11 Oral mucosal tissue reaction grading

[0096] The test results are shown in the table below.

[0097] Table 12 Oral mucosal macroscopic findings observation score sheet

[0098] Table 13 Histopathological evaluation results

[0099] Table 14 Summary and comparison of irritation results of different surfactant combinations in toothpaste formulations

[0100] The acute skin irritation and oral mucosal irritation of toothpastes with different surfactant combinations were evaluated. The results of the irritation evaluation are summarized in the table above. It can be seen that: The acute skin irritation of the three surfactant combination toothpastes was all shown as no irritation, while the irritation to the oral mucosa was different. The toothpaste containing K12 alone showed mild irritation, and the surfactant combination toothpaste containing K12 showed no to very mild irritation, which verified that K12 had a certain irritation to the oral mucosa, but the surfactant combination toothpaste containing the embodiment of the present application showed no irritation to the oral mucosa, and could be used as a mild surfactant combination to replace K12 in toothpaste formulas.

[0101] The embodiments of the present application have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or improvements to the technology in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims

1. A mild gum protection toothpaste, characterized in that: The following components are included in weight percentage: Friction agent 20~50% Xanthan gum 0.3~3% Polyethylene glycol 0.5~10% Nonionic surfactant complex 0.5~5% Wetting agent 15~60% Chelating agent 0.3~3.5% Preservatives 0.05~0.5% Sweetener 0~1% Fragrance 0~2% The balance is deionized water; Wherein, the nonionic surfactant complex comprises at least two nonionic surfactants.

2. The mild gum protection toothpaste according to claim 1, characterized in that: The nonionic surfactant is selected from trehalose lipids, rhamnolipids, sophorolipids, mannolipids, erythritol lipids, alkyl glycosides, soapberry extract, camellia seed extract or saponin extract.

3. The mild gum protection toothpaste according to claim 2, characterized in that: The nonionic surfactant complex comprises rhamnolipid and alkyl glycoside, and the mass ratio of rhamnolipid to alkyl glycoside is (1-5): (1-5); or, The nonionic surfactant complex comprises camellia seed extract and alkyl glycoside, and the mass ratio of the camellia seed extract to the alkyl glycoside is (1-5): (1-5).

4. The mild gum protection toothpaste according to claim 1, characterized in that: The mass ratio of the nonionic surfactant complex to polyethylene glycol is (0.8-1.1):

5.

5. The mild gum protection toothpaste according to claim 1, characterized in that: The friction agent includes bamboo cellulose and at least one of sugarcane silica and rice husk silica, and the particle size of the friction agent is 6-250 μm.

6. The mild gum protection toothpaste according to claim 5, characterized in that: The mass ratio of the bamboo cellulose, sugarcane silica and rice husk silica is (1-2): 1:

1.

7. The mild gum protection toothpaste according to claim 5, characterized in that: The mass ratio of the abrasive, xanthan gum and non-ionic surfactant composite is (25-35):1:

2.

8. The mild gum protection toothpaste according to claim 1, characterized in that: The wetting agent includes sorbitol and glycerol, and the mass ratio of sorbitol to glycerol is 4.5:

1.

9. A method for preparing a mild gum-protecting toothpaste, characterized in that: include: Add the chelating agent, preservative and sweetener into deionized water and stir until completely dissolved; then add the wetting agent and part of polyethylene glycol, mix well and pour into the paste making machine; After mixing the friction agent and xanthan gum, add them into the paste making machine and control the vacuum degree to be within the range of (-0.04) MPa to (-0.08) MPa while stirring and mixing; The nonionic surfactant complex and the remaining polyethylene glycol are dispersed uniformly to obtain a premixed surfactant; The premixed surfactant and flavoring agent are added into a paste making machine, and the vacuum degree is controlled to be above 0.09 MPa for stirring and mixing, and then deaerated and filled to obtain a mild gum-protecting toothpaste.

10. The method for preparing the mild gum protection toothpaste according to claim 9, characterized in that: The polyethylene glycol used for the premix of the nonionic surfactant complex accounts for 50 wt % to 70 wt % of all polyethylene glycols.

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