Oral care compositions, toothpastes and methods of making the same

Abstract

The present application relates to a kind of oral care compositions, toothpaste its preparation method.The oral care compositions are made of saponin surfactant and polyol;The saponin surfactant is soap fruit extract and / or soap extract;The polyol is made of octyl glycol and ethyl hexyl glycerol;The mass ratio of octyl glycol and ethyl hexyl glycerol in the polyol is 2-4:1.The toothpaste is added with the oral care compositions as preservative and surfactant in the application.The new oral care compositions are added in toothpaste, which can make toothpaste have good stability and cleaning performance, while having very excellent preservative performance, and improve the safety of toothpaste use.

Description

Technical Field

[0001] This invention belongs to the field of daily chemical products technology, and relates to oral care products, specifically to an oral care composition, toothpaste and its preparation method. Background Technology

[0002] Oral care products such as toothpaste are susceptible to microbial growth during production, storage, and use due to various factors including environment and usage methods. When these microorganisms develop to a certain level, they can affect the normal use of the oral care products and even cause illness, posing a threat to people's health. Therefore, preservatives are needed to prevent the growth of bacteria, mold, yeast, and other microorganisms. Currently, commonly used preservatives in toothpaste formulations include traditional preservatives such as parabens, sodium benzoate, and benzyl alcohol; however, these traditional preservatives pose several potential safety risks.

[0003] Hydroxyl, carbonyl, and carboxylic acid derivatives in polyols such as ethylhexylglycerin, 1,2-hexanediol, p-hydroxyacetophenone, and glyceryl caprylate can act on the structure of microbial cells, affecting their physiological functions and reducing water activity. They have antimicrobial effects and are a class of mild antibacterial substances with good safety that have emerged in recent years, and are known as alternative preservatives.

[0004] Another major component of toothpaste is surfactant. Surfactants are an essential ingredient in toothpaste, functioning to reduce the surface tension of liquids and possessing excellent wetting, foaming, emulsifying, and cleaning properties. Their emulsifying effect helps oily substances such as fragrances to evenly combine with other components in the toothpaste into a stable system. Rinsing removes plaque suspended in the rich foam produced during brushing, thus achieving oral cleaning. Surfactants can be classified into cationic surfactants, anionic surfactants, and nonionic surfactants. Commonly used surfactants include sodium lauryl sulfate (SLS), sodium lauroyl sarcosinate (LS), and poloxamer.

[0005] The inventors of this invention discovered that when polyol compounds are added to toothpaste as preservatives, they exhibit solubilization-complexation interactions with some commonly added surfactants in toothpaste. These interactions form complex ionic micelles, which reduces the concentration of free polyols in the system, thus affecting the preservative effect of the polyol compounds in the toothpaste. In other words, there is an antagonistic effect between some commonly used surfactants in toothpaste and polyol preservatives, thereby affecting their preservative performance.

[0006] Currently, toothpaste preservative systems still primarily rely on traditional preservatives. However, to improve product safety, meet consumer demands, reduce the use of traditional preservatives, and develop milder, greener, and more environmentally friendly preservative systems, finding alternatives has become a necessary trend in toothpaste formulation. However, alternative preservatives often exhibit antagonistic effects with commonly used surfactants in toothpaste, hindering their antibacterial efficacy. Therefore, it is essential to develop safe and environmentally friendly new preservative systems that improve their preservative performance in toothpaste while ensuring safety. Summary of the Invention

[0007] Therefore, the purpose of this invention is to provide a novel anti-corrosion system that improves its anti-corrosion performance in toothpaste while ensuring safety.

[0008] The technical solutions for achieving the above objectives include the following.

[0009] In a first aspect, the present invention provides an oral care composition comprising a saponin surfactant and a polyol; wherein the saponin surfactant is a soapberry fruit extract and / or a soapberry extract; and the polyol is composed of caprylyl glycol and ethylhexylglycerin, wherein the mass ratio of caprylyl glycol to ethylhexylglycerin in the polyol is 2-4:1.

[0010] The mass ratio of the saponin surfactant to the polyol is 0.5-4:1, preferably 1-3:1, and more preferably 2:1; the mass ratio of octyl glycol to ethylhexylglycerin in the polyol is preferably 2-3:1, and more preferably 7:3.

[0011] Secondly, the present invention provides the use of the oral care composition as a preservative and surfactant in the preparation of toothpaste.

[0012] Thirdly, the present invention also provides a toothpaste in which the oral care composition described in the present invention is added as a preservative and a surfactant.

[0013] The saponin surfactant in the oral care composition is preferably 0.5%-2% by mass in the toothpaste, preferably 0.8%-1.5%, preferably 0.8%-1.2%, and more preferably 1% by mass in the toothpaste; the polyol in the oral care composition is preferably 0.2%-1.5% by mass in the toothpaste, preferably 0.4%-1%, preferably 0.4%-0.6%, and more preferably 0.5%.

[0014] Fourthly, the present invention provides a method for preparing toothpaste, comprising the following steps:

[0015] Step 1: Pre-disperse the polyol in a portion of the humectant; pre-dissolve the flavoring agent;

[0016] Step 2: Add water, pH adjuster, and anti-caries active ingredients to a premixing pot and stir until the raw materials are dissolved. Add humectant and pre-dispersed polyol and stir evenly to obtain mixture 1. Add mixture 1 to the ointment making machine.

[0017] Step 3: Mix and disperse the abrasive and thickener evenly to obtain mixture 2. Add mixture 2 to a paste-making machine and vacuum stir at high speed for 10-20 minutes.

[0018] Step 4: Add the pre-dissolved flavoring agent and saponin surfactant to the toothpaste making machine, and mix and disperse them thoroughly under vacuum for 10-15 minutes to obtain the toothpaste.

[0019] The present invention has the following beneficial effects:

[0020] To address the challenge of achieving good preservative properties with polyols in toothpaste, the inventors of this invention have developed a novel oral care composition through extensive experimental research. This composition comprises specific polyols (caprylyl glycol and ethylhexylglycerin) and saponin-based surfactants. Adding this novel oral care composition to toothpaste imparts both good stability and cleaning performance, along with excellent preservative properties. Even at relatively low concentrations, the resulting toothpaste exhibits a log reduction in bacteria and fungi of greater than 4 after both 7 and 28 days in preservative challenge experiments. This solves the problem that conventionally added surfactants in toothpaste often fail to achieve good preservative effects due to antagonism.

[0021] The oral care composition of the present invention uses mild, safe, and green polyol compounds in combination with highly safe, green, and non-toxic saponin surfactants in toothpaste, avoiding the safety risks associated with the use of traditional preservatives and improving the safety of toothpaste use. Detailed Implementation

[0022] To facilitate understanding of the present invention, a more complete description will be provided below. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the present invention.

[0023] Unless otherwise specified, experimental methods in the following examples are generally performed under standard conditions or as recommended by the manufacturer. All commonly used chemical reagents used in the examples are commercially available products.

[0024] Unless otherwise defined, all technical and scientific terms used in this invention have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. The term "and / or" as used in this invention includes any and all combinations of one or more of the associated listed items.

[0025] Furthermore, as used herein, the term "or" is an inclusive "or" sign and is equivalent to the term "and / or" unless the context clearly specifies otherwise. The term "based on" is not exclusive and allows for basing on other factors not described unless the context clearly specifies otherwise. Additionally, throughout the specification, the meanings of "an," "a," and "the" include plural indicators. The meaning of "in" includes both "in" and "on."

[0026] During their research on toothpaste preservatives, the inventors of this invention discovered that when polyol compounds are added to toothpaste as preservatives, they exhibit a solubilization-complexation reaction with conventionally added surfactants. This forms complex ionic micelles, reducing the concentration of free polyols in the system and thus affecting their preservative effect. In other words, there is an antagonistic effect between conventionally added surfactants and polyol preservatives, impacting their preservative performance. To address this issue, the inventors conducted extensive experimental research and discovered a surfactant that can be compounded with specific polyols. This specific type of surfactant, when compounded with a specific polyol, does not produce an antagonistic effect. When added together to toothpaste, it achieves excellent preservative effects at low dosages, while also providing the toothpaste with good stability and cleaning properties.

[0027] Based on the above findings, some embodiments of the present invention relate to an oral care composition comprising a saponin surfactant and a polyol; wherein the saponin surfactant is a soapberry fruit extract and / or a soapberry extract; and the polyol is composed of caprylyl glycol and ethylhexylglycerin, wherein the mass ratio of caprylyl glycol to ethylhexylglycerin in the polyol is 2-4:1.

[0028] In some embodiments, the mass ratio of the saponin surfactant to the polyol is 0.5-4:1, preferably 1-3:1, more preferably 1.5-2.5:1, and even more preferably 2:1.

[0029] In some embodiments, the mass ratio of octyl glycol to ethylhexylglycerin in the polyol is 2-3:1, more preferably 7:3.

[0030] Adding the oral care composition described in this invention to toothpaste can act as both a preservative and a surfactant, enabling the toothpaste to have good stability and cleaning performance while also possessing excellent preservative properties. Even with a low addition amount, the resulting toothpaste can achieve a log reduction value of greater than 4 for bacteria and fungi in both 7-day and 28-day anti-corrosion challenge experiments.

[0031] Some embodiments of the present invention also relate to a toothpaste in which the oral care composition of the present invention is added as a preservative and a surfactant.

[0032] In some embodiments, the saponin surfactant in the oral care composition is 0.5%-2% by mass in the toothpaste, preferably 0.8%-1.5%, more preferably 0.8%-1.2%, and more preferably 1%.

[0033] In some embodiments, the polyol in the oral care composition is present in the toothpaste at a mass percentage of 0.2%-1.5%, preferably 0.4%-1%, preferably 0.4%-0.6%, and most preferably 0.5%.

[0034] The toothpaste of the present invention may also contain one or more other excipients acceptable to toothpaste, such as humectants, abrasives, thickeners, pH adjusters, flavoring agents, etc.; it may also contain various functional ingredients acceptable to toothpaste, such as one or more functional ingredients such as anti-caries, whitening, anti-sensitivity, and anti-tartar.

[0035] For example, in some embodiments, the toothpaste may be prepared from raw materials comprising the following mass percentages:

[0036]

[0037] In some preferred embodiments, the toothpaste may be prepared from raw materials comprising the following weight percentages:

[0038]

[0039] In some embodiments, the humectant may be selected from at least one of sorbitol, propylene glycol, glycerin, polyethylene glycol-6, polyethylene glycol-8, polyethylene glycol 12, polyethylene glycol 32, and polyethylene glycol 75. For example, it may be a combination of sorbitol, propylene glycol, and glycerin, with the mass ratio of sorbitol, propylene glycol, and glycerin preferably being 5-7:1:4-6, more preferably 32:5:25.

[0040] In some embodiments, the abrasive may be selected from at least one of thickening hydrated silica, friction hydrated silica, walnut kernel powder, and bamboo cellulose. For example, it may be a combination of hydrated silica 3, hydrated silica 1, and hydrated silica 2, wherein the mass ratio of hydrated silica 3, hydrated silica 1, and hydrated silica 2 is 1:2-4:1-2, more preferably 3:8:4.

[0041] In some embodiments, the thickener is selected from at least one of cellulose gum, xanthan gum, and carbomer. For example, it may be a combination of cellulose gum and xanthan gum, with the mass ratio of cellulose gum to xanthan gum preferably being 1:1-2, more preferably 2:3.

[0042] In some embodiments, the pH adjuster is selected from at least one of tetrasodium pyrophosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, pentasodium tripolyphosphate, and sodium citrate. In some embodiments, the anti-caries active ingredient is selected from at least one of sodium fluoride, sodium monofluorophosphate, and stannous fluoride.

[0043] In some embodiments, the flavoring agent is selected from at least one of menthol, flavoring, natural fruit extracts, trichlorogalactose, D-allulose, and steviol glycosides.

[0044] In some preferred embodiments, the toothpaste is prepared from raw materials comprising the following weight percentages:

[0045]

[0046] In some preferred embodiments, the toothpaste is prepared from raw materials comprising the following weight percentages:

[0047]

[0048]

[0049] The toothpaste of the present invention can be prepared by conventional methods in the art. In some embodiments, the preparation method of the toothpaste provided by the present invention includes the following steps:

[0050] Step 1: Pre-disperse the polyol in a portion of the humectant; pre-dissolve the flavoring agent;

[0051] Step 2: Add water, pH adjuster, and anti-caries active ingredients to a premixing pot and stir until the raw materials are dissolved. Add humectant and pre-dispersed polyol and stir evenly to obtain mixture 1. Add mixture 1 to the ointment making machine.

[0052] Step 3: Mix and disperse the abrasive and thickener evenly to obtain mixture 2. Add mixture 2 to a paste-making machine and vacuum stir at high speed for 10-20 minutes.

[0053] Step 4: Add the pre-dissolved flavoring agent and saponin surfactant to the toothpaste making machine, and mix and disperse them thoroughly under vacuum for 10-15 minutes to obtain the toothpaste.

[0054] The present invention will be further described in detail below with reference to specific embodiments.

[0055] The following describes some of the raw materials used in the examples:

[0056] Hydrated silica 1: White powder, medium-high friction type silica (type 115), purchased from Jin Sanjiang (Zhaoqing) Silicon Materials Co., Ltd.

[0057] Hydrated silica 2: white powder, medium-low friction type silica (MT type), purchased from Jin Sanjiang (Zhaoqing) Silicon Materials Co., Ltd.

[0058] Hydrated silica 3: white powder, thickened silica (type 165), purchased from Jin Sanjiang (Zhaoqing) Silicon Materials Co., Ltd.

[0059] The Sapindus mukorossi extract, composed of water and Sapindus mukorossi fruit extract, with a solid content of 15-20%, was purchased from Guangdong Jingcui Biotechnology Co., Ltd.

[0060] Soapberry extract, off-white powder, purchased from Yunnan Yingge Biotechnology Co., Ltd., product name Huanyan. TM Product code IG1017, it is extracted from the fruit of the soapberry plant.

[0061] Cellulose gum, an off-white powder, is composed of sodium carboxymethyl cellulose and was purchased from Changshu Weiyi Technology Co., Ltd.

[0062] Example 1

[0063] This embodiment provides a toothpaste in which Sapindus mukorossi fruit extract is added as a surfactant, and 70% caprylyl glycol + 30% ethylhexylglycerin is used as a combination of preservatives. The specific formulation is shown in Table 1.

[0064] The Sapindus mukorossi fruit extract was added in the form of Sapindus mukorossi extract purchased from Guangdong Jingcui Biotechnology Co., Ltd., with a solid content of 17.5%, that is, the amount of Sapindus mukorossi extract added was 5.71%, so that the weight percentage of Sapindus mukorossi fruit extract in the toothpaste of this embodiment was 1%.

[0065] Table 1. Toothpaste formulation composition

[0066]

[0067]

[0068] The toothpaste preparation method provided in this embodiment is as follows:

[0069] Step 1: Weigh all the ingredients in the formula according to the formula amount and set aside; pre-disperse caprylyl glycol and ethylhexylglycerin in a portion of propylene glycol and set aside; pre-dissolve menthol in the flavoring (specifically: add the flavoring and menthol to the flavoring premixing tank, heat in a water bath (the water bath temperature should not exceed 70℃, and the flavoring temperature should not exceed 42℃), stir until dissolved, and remove in time) and set aside;

[0070] Step 2: Add deionized water, tetrasodium pyrophosphate, and sodium fluoride to a premixing pot and stir for more than 15 minutes until the raw materials are dissolved. Then add sorbitol, propylene glycol, glycerin, and pre-dispersed caprylyl glycol and ethylhexylglycerin, and stir evenly to obtain mixture 1. Add mixture 1 to the ointment making machine.

[0071] Step 3: Mix and disperse the thickening hydrated silica, friction hydrated silica 1, friction hydrated silica 2, cellulose gum and xanthan gum evenly to obtain mixture 2. Add mixture 2 to the paste-making machine and vacuum stir at high speed for 15 minutes under the conditions of vacuum degree -0.06Mpa and speed of 1000rpm (10 to 20 minutes is acceptable, speed is 950rpm-1050rpm, and vacuum degree is within the range of -0.04Mpa to -0.08Mpa).

[0072] Step 4: Add the pre-dissolved menthol, fragrance, and soapberry extract to the toothpaste maker, and mix and disperse them thoroughly under vacuum for 10-15 minutes (start timing after the vacuum degree reaches -0.094Mpa, and the vacuum degree should not be lower than -0.092Mpa during the mixing and dispersion process) to obtain the toothpaste of this embodiment.

[0073] Example 2

[0074] This embodiment provides a toothpaste in which soapberry extract is added as a surfactant and caprylyl glycol 70% + ethylhexylglycerin 30% is used as a combined preservative. The specific formulation is shown in Table 2.

[0075] Table 2 Toothpaste formulation composition

[0076]

[0077] The toothpaste preparation method provided in this embodiment is the same as that in Embodiment 1.

[0078] Comparative Examples 1-13

[0079] The toothpastes provided in Comparative Examples 1-13 differ from those in Example 2 in that they contain different surfactants and / or preservatives; the other components, their amounts, and the preparation methods are the same as in Example 2. The surfactants and preservatives in each comparative example are shown in Table 3.

[0080] Table 3 shows the differences in surfactants and preservatives in the toothpaste prepared in the examples and comparative examples.

[0081]

[0082]

[0083] The specific names corresponding to the abbreviations of some surfactants in Table 3 are shown in Table 4.

[0084] Table 4

[0085] Surfactant properties Surfactant (abbreviation) Surfactant Name Amphoteric surfactants CAB Cocamidopropyl Betaine Nonionic surfactants APG Alkyl glycosides Anionic surfactants LS Sodium lauroyl sarcosinate Anionic surfactants CGA Sodium cocoyl glutamate

[0086] Example 3: Microbial Preservative Challenge Experiment

[0087] Preservative challenge experiments artificially simulate higher levels of microbial contamination in cosmetics or daily chemical products during production or use to determine whether the product's preservative system can resist such high levels of microbial contamination, thereby evaluating the preservative system of cosmetics or daily chemical products.

[0088] The bacterial strains used in this experiment are as follows:

[0089] Bacteria: Escherichia coli (ATCC 8739); Staphylococcus aureus (ATCC 6538); Pseudomonas aeruginosa (ATCC 9027);

[0090] Fungi: Aspergillus niger (ATCC 16404); Candida albicans (ATCC 10231).

[0091] The culture medium used in this experiment is as follows:

[0092] Slant culture medium: Soybean Casein Digest Agar Medium (SCDA) was used for bacteria; Sabouraud Dextrose Agar Medium (SDA) was used for fungi. The slant test tubes used were 18×180mm.

[0093] The culture media used for bacterial cell counting were: tryptic soy agar for bacteria and saponin agar for fungi.

[0094] Culture media for 7-day and 28-day tests: for bacteria, lecithin Tween 80 nutrient agar; for fungi, Sabouraud dextrose agar containing 0.7% Tween 80 and 0.1% soybean lecithin.

[0095] The instruments and consumables used in this experiment are as follows:

[0096] Biosafety cabinet (HR-II-A2); vertical pressure steam sterilizer (LT-CPS38D); micropipette (NPX-1000); vortex mixer (XW-80A); disposable plastic petri dishes (9×1.5cm); constant temperature incubator (SPX-250B-Z); borosilicate glass reagent bottle (blue cap, 100mL); glass test tubes (15×150mm); sodium chloride (chemically pure), Tween-80 (chemical reagent), etc.

[0097] The specific steps are as follows:

[0098] 1. Preparation of bacterial suspension

[0099] 1.1 Preparation of bacterial suspension

[0100] 1.1.1 Inoculate three bacterial strains onto TSA slant agar and incubate at 36°C for 18-24 h. Substitute 1-2 times consecutively. The bacterial strains should not be passaged more than 5 times (calculated from the original strain).

[0101] 1.1.2 Each of the three bacterial strains was eluted from the above-mentioned slant or plate with 2-3 mL of sterile physiological saline (0.85%) to achieve a bacterial concentration of 1-10 × 10⁻⁶. 8 Each culture was placed into a 15mL sterile centrifuge tube as the initial bacterial culture (10). 0 The bacterial suspension must be used immediately (if not used immediately, it must be placed in a 4°C refrigerator within 2 hours and used within 24 hours).

[0102] 1.2 Preparation of fungal suspension

[0103] 1.2.1 Two fungal strains were inoculated onto SDA slant medium (or SDA plate) and cultured at 22.5±2.5℃. Yeast was cultured for 40-48 h and mold for 6-10 d (until the mold formed sufficient spores). The strains were subcultured 1-2 times. The number of generations of fungal strains should not exceed 5 (calculated from the original strain).

[0104] 1.2.2 Elute the bacterial cultures with 2-3 mL of 0.85% sterile physiological saline. For molds, elute the spores with physiological saline containing 0.05% Tween-80 to achieve a concentration of 1-10 × 10⁻⁶. 7 Each culture was placed into a 15mL sterile centrifuge tube as the initial bacterial culture (10). 0 Yeast suspensions should be used immediately (if not used immediately, they should be placed in a 4°C refrigerator within 2 hours and used within 24 hours), while mold suspensions can be stored in the refrigerator for up to 7 days.

[0105] 2. Counting of bacterial suspensions

[0106] 2.1 Using a micropipette, transfer 1 mL of the bacterial suspension from step 1.1.2 into 9 mL of sterile physiological saline, and vortex to mix. This dilution is 1:10. Then, using a micropipette, transfer 1 mL of the 10-fold diluted bacterial suspension into 9 mL of sterile physiological saline; this is a 100-fold dilution. Repeat this process for the remaining solutions, diluting to 100-fold. -10 (Depending on bacterial concentration) gradient;

[0107] 2.2 Using a micropipette, transfer 1 mL of the bacterial suspension from step 1.2.2 into 9 mL of sterile physiological saline, and vortex to mix. This dilution is 1:10. Then, using a micropipette, transfer 1 mL of the 10-fold diluted bacterial suspension into 9 mL of sterile physiological saline; this is a 100-fold dilution. Repeat this process for the remaining solutions, diluting to 100-fold. -8 (Depending on bacterial concentration) gradient;

[0108] 2.3 Select appropriate gradients for culture and counting: bacterial culture temperature: 36℃, culture time: 1-2 days; yeast culture temperature: 28℃, culture time: 2-5 days; mold culture temperature: 28℃, culture time: 2-5 days. The specific culture time depends on the microbial growth, but the petri dishes should be kept in the incubator for at least the longest possible time to determine if colonies will subsequently grow. Counting rules should follow the requirements of the "Cosmetic Safety Technical Specifications" (2015).

[0109] 3. Sample preparation

[0110] 3.1 Sterilize the borosilicate reagent bottle (the cap should not be completely tightened, leaving a certain gap) at 121℃ for 20 minutes, then place it in a 60℃ oven to dry off the moisture, and cool it to room temperature. If the bottle is not used immediately, the cap should be tightened to prevent contamination.

[0111] 3.2 Using a sterile spoon or sterile syringe, take 50g of the sample prepared in each example and comparative example (prepare two portions of one sample, inoculated with bacteria and fungi respectively) into a sterile and dry high borosilicate reagent (the front part of the sample should be removed when squeezing the toothpaste sample).

[0112] 4. Inoculation of bacterial suspension

[0113] 4.1 Remove the prepared bacterial suspension from the refrigerator and let it stand at room temperature for 30 minutes.

[0114] 4.2 Use a micropipette to take 0.6 mL of a mixture of three bacterial suspensions (concentration ~1×10⁻⁶). 8 (CFU / mL) into a reagent bottle in section 3.2; use a micropipette to take 0.4 mL of a mixture of the two fungal suspensions (concentration ~1×10⁻⁶ CFU / mL). 7 (CFU / mL) in a 3.2-inch reagent bottle.

[0115] 4.3 Under aseptic conditions, stir and shake to ensure that the sample and bacterial solution are thoroughly mixed.

[0116] 5 Detection Count

[0117] 5.1 Take 3.0g from each of the well-mixed sample vials and add it to a 27mL Erlenmeyer flask containing sterile physiological saline and glass beads. Mix well. This is a 1:10 test solution. (A homogenizer bag can also be used for dilution).

[0118] 5.2 Using a micropipette, pipette 1 mL of the above test solution into 9 mL of sterile physiological saline, vortex to mix. This dilution factor is 100. Repeat the dilution to 100. -6 gradient.

[0119] 5.3 Cultivation Conditions

[0120] Bacteria were detected using Tween-80 nutrient agar and cultured at 36°C for 2–3 days. Fungi were detected using Sabouraud dextrose agar containing 0.7% Tween-80 and 0.1% soybean lecithin and cultured for 2–7 days. Counting was generally performed on the first and second days to prevent over-inoculation of bacteria that would prevent counting.

[0121] 5.4 The counting rules are the same as those in 2.3.

[0122] 6. Cultivation and Sampling

[0123] 6.1 Seal the sample reagent bottles and store them in an incubator at 22.5±2.5℃ for 28 days, protected from light.

[0124] 6.2 Samples were taken at 7 days and 28 days respectively; and tested according to the method in section 5.

[0125] 7. Test data recording and calculation

[0126] Calculate the logarithmic decrease in the number of microorganisms on day 7 and day 28.

[0127] Calculation formula: Logarithmic decrease = Log 10 (Initial bacterial count / Surviving bacterial count)

[0128] The test results are shown in Table 5.

[0129] Table 5 Results of Corrosion Resistance Challenge Tests

[0130]

[0131] The results of the anti-corrosion challenge experiment show that:

[0132] Examples 1 and 2 use Sapindus mukorossi fruit extract or soapberry extract as surfactants, and polyols caprylyl glycol and ethylhexylglycerin in a specific ratio as preservative and antibacterial ingredients, which can enable toothpaste to achieve the best preservative performance. The log reduction values ​​of bacteria and fungi after 7 days and 28 days can reach an excellent effect of greater than 4.

[0133] Comparative Examples 1-7 show that when bio-glycolipid surfactants such as rhamnolipids and sophorolipid 203, or conventional surfactants such as sodium lauroyl sarcosinate, are added to toothpaste, the polyols fail to exert excellent preservative effects, resulting in a 7-day reduction in fungal logarithmic count of less than 4. The preservative performance is significantly weaker compared to Examples 1 and 2. Even when sodium lauroyl sarcosinate and cocamidopropyl betaine, which have certain antibacterial properties, are added as surfactants in combination with the polyol (Comparative Example 5), the preservative effect of the resulting toothpaste is even lower than that of the toothpaste without added polyol preservatives (Comparative Example 10). This demonstrates a severe antagonistic effect between the surfactants and polyols in the comparative examples, preventing the polyols and / or surfactants themselves from achieving their original preservative effects in the toothpaste system.

[0134] As can be seen from Comparative Examples 7-9 and 11-13, the combination of different types of polyols has a significant impact on the preservative effect of the oral care composition. When a specific polyol is combined as a preservative and antibacterial ingredient, it needs to be combined with a specific surfactant to minimize or avoid the antagonistic effect between the two and obtain a better preservative effect.

[0135] Example 4: Stability Test of Toothpaste

[0136] Two toothpaste samples prepared in Examples 1 and 2 were placed in a constant temperature incubator at 45±1℃. They were taken out at different time periods and compared with the samples stored at room temperature to check their stability. The toothpaste was squeezed out and compared with the samples stored at room temperature to check whether the appearance, color and smell were normal, and whether there were any abnormal phenomena such as coarsening or water separation. Then, the tube was cut open to check whether there were any abnormal phenomena such as granulation, coarsening, water separation or shelling. If none of these were found, the stability was considered normal.

[0137] The test results are shown in Table 6.

[0138] Table 6. High-temperature stability results of toothpaste

[0139]

[0140]

[0141] Example 5: Evaluation of the antibacterial performance of toothpaste against oral pathogens

[0142] The toothpaste samples prepared in Examples 1 and 2 were evaluated for their antibacterial performance against oral pathogens. The antibacterial rate was tested by short-term contact between bacteria and toothpaste paste, thereby determining their antibacterial performance.

[0143] 1.1 Experimental Materials

[0144] 1.1.1 Preparation of inoculum

[0145] Oral pathogens: Inoculate Streptococcus mutans (GDMCC1.530) into broth medium and anaerobic culture at 37°C for 18-24 hours (do not exceed 24 hours, otherwise the strain will age) for later use;

[0146] 1.1.2 Culture medium

[0147] 1.1.2.1 Detection medium: Brain heart extract agar medium.

[0148] 1.1.3 Experimental Consumables

[0149] Phosphate-buffered saline (PBS, 0.03 mol / L, pH 7.2–7.4), glass test tubes, anaerobic vacuum device, anaerobic culture jar, and constant temperature incubator;

[0150] 1.2 Operating Procedures

[0151] 1.2.1 Sample preparation for the experimental group: Add 75mL of sterile PBS and 25g of toothpaste sample to the homogenizer bag, shake and mix well to fully disperse the toothpaste into a homogenized solution (25%), and then take 9mL of toothpaste slurry and add it to a sterile glass test tube for later use.

[0152] 1.2.2 After eluting the pathogenic bacteria from 1.1.1 with sterile water, dilute each sample with sterile PBS to a concentration of 1×10⁻⁶. 6 ~5×10 6 CFU / mL concentration;

[0153] 1.2.3 Blank group: 1.0 mL of bacterial suspension (1×10⁻⁶) was taken from each group. 6 ~5×10 6 Add CFU / mL to 9 mL of sterile PBS solution, vortex to mix, incubate for 2 min, then take the mixture and dilute appropriately, and incubate anaerobically for 72 h before counting;

[0154] 1.2.4 Experimental group: 1.0 mL of bacterial suspension (1×10⁻⁶) was taken from each group. 6 ~5×10 6 (CFU / mL) was separately mixed with 9 mL of toothpaste paste by vortexing and incubation for 2 min. The mixture was then appropriately diluted and anaerobically incubated for 72 h before counting.

[0155] 1.2.5 Calculate the antibacterial rate using the following formula.

[0156]

[0157] 2 Evaluation Criteria

[0158] If the antibacterial rate is 50% ≤ and < 90%, the product has antibacterial effect; if the antibacterial rate is ≥ 90%, the product has strong antibacterial effect.

[0159] 3 Experimental Results

[0160] The test results (Table 7) show that the toothpaste samples prepared in Examples 1 and 2 have a strong antibacterial effect against oral pathogens (Streptococcus mutans) (antibacterial inhibition rate ≥90%), and can effectively reduce the growth of oral bacteria by >99.99%.

[0161] Table 7

[0162]

[0163]

[0164] Example 6 Sensory evaluation of toothpaste use

[0165] Sensory evaluations were conducted on the toothpaste samples prepared in Examples 1 and 2. Thirty participants were recruited to evaluate the toothpaste's taste. Participants used the toothpaste according to standard usage methods, using each toothpaste for at least one day consecutively, and completed questionnaires. A 7-point scoring system was used, with six dimensions: overall taste, foam volume, foam density, preference for foam density, foam satisfaction, and irritation / bitterness. The scoring criteria are shown in Table 7, and the results are shown in Table 8.

[0166] Table 7 Toothpaste Taste Evaluation Criteria

[0167]

[0168]

[0169] Table 8. Average Score Statistics of Survey Results

[0170]

[0171] The subjects rated the two toothpaste products on six dimensions: overall taste, amount of foam, density of foam, preference for density of foam, satisfaction with foam, and feedback on irritation / bitterness. All scores were around 6, indicating high satisfaction with the taste of both products. The toothpaste sample in Example 1 had better foam density and higher preference among the subjects.

[0172] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. An oral care composition, characterized in that, Composed of saponin surfactants and polyols; The saponin surfactant is Sapindus mukorossi fruit extract and / or soapberry extract; The polyol is composed of octyl glycol and ethylhexylglycerol; the mass ratio of octyl glycol to ethylhexylglycerol in the polyol is 2-4:

1.

2. The oral care composition according to claim 1, characterized in that, The mass ratio of the saponin surfactant to the polyol is 0.5-4:1, preferably 1-3:1, and more preferably 2:1; The mass ratio of octyl glycol to ethylhexylglycerin in the polyol is 2-3:1, more preferably 7:

3.

3. The use of the oral care composition of claim 1 or 2 as a preservative and surfactant in the preparation of toothpaste.

4. A toothpaste, characterized in that, The toothpaste contains the oral care composition of claim 1 or 2 as a preservative and surfactant.

5. The toothpaste according to claim 4, characterized in that, The saponin surfactant in the oral care composition is present in the toothpaste at a mass percentage of 0.5%-2%, preferably 0.8%-1.5%, more preferably 0.8%-1.2%, and most preferably 1%.

6. The toothpaste according to claim 4, characterized in that, The polyol in the oral care composition is present in the toothpaste at a mass percentage of 0.2%-1.5%, preferably 0.4%-1%, more preferably 0.4%-0.6%, and most preferably 0.5%.

7. The toothpaste according to claim 4, characterized in that, It is prepared from raw materials comprising the following percentages by mass: Preferably, the toothpaste is prepared from raw materials comprising the following weight percentages:

8. The toothpaste according to claim 7, characterized in that, The moisturizer is selected from at least one of sorbitol, propylene glycol, glycerin, polyethylene glycol-6, polyethylene glycol-8, polyethylene glycol 12, polyethylene glycol 32, and polyethylene glycol 75; and / or, The abrasive is selected from at least one of thickening hydrated silica, friction-type hydrated silica, walnut kernel powder, and bamboo cellulose; and / or, The thickener is selected from at least one of cellulose gum, xanthan gum, and carbomer; and / or, The pH adjuster is selected from at least one of tetrasodium pyrophosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, pentasodium tripolyphosphate, and sodium citrate; and / or, The anti-caries active ingredient is selected from at least one of sodium fluoride, sodium monofluorophosphate, and stannous fluoride; and / or, The flavoring agent is selected from at least one of menthol, flavoring, natural fruit extracts, trichlorogalactose, D-allulose, and steviol glycosides.

9. The toothpaste according to claim 7, characterized in that, It is prepared from raw materials comprising the following percentages by mass:

10. A method for preparing toothpaste according to any one of claims 7-9, characterized in that, Includes the following steps: Step 1: Pre-disperse the polyol in a portion of the humectant; pre-dissolve the flavoring agent; Step 2: Add water, pH adjuster, and anti-caries active ingredients to a premixing pot and stir until the raw materials are dissolved. Add humectant and pre-dispersed polyol and stir evenly to obtain mixture 1. Add mixture 1 to the ointment making machine. Step 3: Mix and disperse the abrasive and thickener evenly to obtain mixture 2. Add mixture 2 to a paste-making machine and vacuum stir at high speed for 10-20 minutes. Step 4: Add the pre-dissolved flavoring agent and saponin surfactant to the toothpaste making machine, and mix and disperse them thoroughly under vacuum for 10-15 minutes to obtain the toothpaste.

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