Toothpaste taking macadamia nut polypeptide and macadamia nut extract as main components

Abstract

The invention provides toothpaste taking macadamia nut polypeptide and macadamia nut extract as main components. The toothpaste comprises the following main components: macadamia nut polypeptide, macadamia nut green peel extract, macadamia nut leaf extract and houttuynia cordata extract. The composition is used for preparing antibacterial toothpaste. The toothpaste is prepared by taking the macadamia nut polypeptide and the extract as main components, and the macadamia nut polypeptide accounts for a large amount in the raw materials. Experiments show that the toothpaste provided by the invention has relatively good antibacterial performance and antioxidant function, meanwhile, the toothpaste is good in taste, fragrant in smell and free of bitter taste of polypeptide, in addition, macadamia nut polypeptide and houttuynia cordata have a synergistic interaction effect, the pure natural performance of the toothpaste is ensured through the common compatibility of the substances, and the toothpaste is suitable for popularization and application. In addition, the antibacterial effect and the oxidation resistance are remarkably improved, and the sensory score is good.

Description

Technical Field

[0001] The invention belongs to the technical field of toothpaste preparation, and particularly relates to a toothpaste with macadamia nut polypeptide and extract as main ingredients. Background Art

[0002] Toothpaste is an indispensable oral cleaning and health care product in people's daily life. Different toothpastes used when people brush their teeth will have different functions and effects. In recent years, with the continuous enhancement of consumers' health awareness, people are no longer satisfied with toothpaste that only has cleaning and health care functions, but require toothpaste to have good auxiliary treatment functions and the fragrance of natural plant ingredients. Based on this, since natural plant medicinal active ingredients have a good effect in treating oral and dental diseases, and are natural and environmentally friendly, with little toxic and side effects, they are in line with the natural and healthy consumer concept. Therefore, the research on adding active ingredients from natural plants to toothpaste formulas is also developing rapidly.

[0003] Some toothpastes currently on the market have tried to add medicinal active ingredients from plant nuts to provide corresponding health benefits, but so far the plant nut active ingredients used are relatively few and cannot be used as the main additive, and the health benefits of natural nuts cannot be fully utilized. In addition, a variety of Chinese medicinal plant ingredients are often added to nuts, and these Chinese medicinal herbs often have a strong and bitter smell, making the processing and production process of toothpaste more complicated in removing bitterness and masking the smell, and more importantly, the antibacterial effect is not obvious enough.

[0004] For example, Chinese patent document CN 107362088 A provides a toothpaste prepared with macadamia shell powder, which completely or partially replaces the abrasive in the toothpaste with macadamia shell powder, and takes advantage of its rich mineral content to achieve a certain effect on the human oral cavity and hemostasis; in addition, by adding macadamia shell edible alcohol extract instead of flavor, the toothpaste taste and smell are improved, so that the toothpaste has a unique nutty fragrance, and as a natural extract, it has certain antibacterial and anti-inflammatory effects. Although the patent adds macadamia natural extract, it is only added as an excipient, and its antibacterial effect is minimal.

[0005] In addition, Chinese patent document CN 106580779 A discloses a Chinese herbal toothpaste with macadamia nut extract as the main ingredient, which is composed of the following weight percentages of active pharmaceutical ingredients: 15%-20%, abrasive 20%-30%, moisturizer 20%-35%, foaming agent 2%-4%, thickener 0.5-1.5%, flavor 0.3%-0.5%, saccharin 0.2%, and the balance is deionized water. The active pharmaceutical ingredients are composed of the following components and weight ratios: 20-30 parts of macadamia nut extract, 10-20 parts of golden iron lock extract, 15 parts of Bidens pilosa extract, 15-20 parts of Scutellaria baicalensis extract, and 5-15 parts of Artemisia annua extract. However, the proportion of active pharmaceutical ingredients in this patent is relatively small, especially the proportion of macadamia nut ingredients is extremely small, and at the same time, there are too many other compounded Chinese herbal ingredients, which affects the taste and smell of the toothpaste, especially the unique fragrance of nuts cannot be reflected.

[0006] At present, due to the good health care effect of macadamia nuts, its additional functional products are being continuously developed, and more research focuses on the preparation of macadamia nut extracts, such as macadamia nut polypeptide extracts, macadamia nut green peel extracts, etc. However, the use of macadamia nut extracts and macadamia nut polypeptide extracts as toothpaste components to prepare an antibacterial toothpaste has not been studied. For example, none of the above patent documents involve how to add antioxidant ingredients such as macadamia nut polypeptide extracts to toothpaste formulas. More importantly, while giving toothpaste products antioxidant activity through macadamia nut polypeptide extracts, how to eliminate the bitterness of macadamia nut polypeptides and ensure the fresh taste of toothpaste, while also making the toothpaste formula have good formability, long shelf life, and excellent antibacterial effect, still requires a lot of exploration and research.

[0007] Therefore, how to successfully use multiple extract components of macadamia nuts as a formula based on existing technologies to develop a macadamia toothpaste product with significant antibacterial and antioxidant properties, while maintaining the fresh taste of the toothpaste, and also making it have good formability and a long shelf life to meet people's growing demand for oral health and treatment has become a technical problem that needs to be solved urgently. Summary of the invention

[0008] In view of this, the present invention provides a toothpaste product with natural plant ingredients as the main formula, and particularly relates to a macadamia nut toothpaste product with macadamia nut polypeptide as the main ingredient and a compound of multiple macadamia nut extracts as the main formula, so that macadamia nut polypeptide and other macadamia nut extracts can be used in toothpaste in larger amounts, fully utilizing the health benefits and natural fragrance of natural nut active ingredients, giving the toothpaste antibacterial and antioxidant properties, and solving the problems of poor formability and short shelf life of products with natural plant ingredients as the main raw materials; on the other hand, while increasing the antibacterial performance of toothpaste, it also further solves the problem of heavy bitterness and poor taste of such products due to the large amount of extracts such as macadamia nut polypeptide contained in such products.

[0009] In order to achieve the above object, the present invention adopts the following technical solution:

[0010] A toothpaste with macadamia polypeptide and extract as main ingredients, the toothpaste mainly comprising: macadamia polypeptide, macadamia green peel extract, macadamia leaf extract and houttuynia cordata extract; the weight ratio of each component is macadamia polypeptide: macadamia green peel extract: macadamia leaf extract: houttuynia cordata extract = 7-13: 1-3: 2-4: 2-5;

[0011] The preparation process of macadamia polypeptide is as follows: hydraulically pressed macadamia meal is crushed and passed through a 60-mesh sieve. After sieving, 15 g of macadamia meal is dissolved in 150 mL of distilled water, and the mixture is placed in a constant temperature water bath at 60°C for 15 min. 0.075 g of compound protease is added and stirred evenly. The mixture is enzymolyzed at 56°C for 3 h in a constant temperature water bath, and the enzyme is inactivated at 85°C for 15 min. After cooling, the mixture is filtered to obtain macadamia polypeptide, which is then placed in a refrigerator for refrigeration.

[0012] The preparation process of macadamia leaf extract is as follows: fresh leaves are picked, washed, dried, crushed and passed through a 40-mesh sieve, 12 g of macadamia leaf powder is stirred and dissolved with 960 mL of 70% ethanol, mixed and ultrasonicated at 40°C for 10 min, then shaken for extraction for 1 h, the macadamia leaf extract is centrifuged at 4000 r / min for 20 min, the supernatant is collected and vacuum evaporated at 60°C until there is no alcohol taste, to obtain the macadamia leaf extract, which is then refrigerated;

[0013] The preparation process of macadamia nut green peel extract is as follows: fresh macadamia nut green peel is selected, cleaned to remove surface impurities, placed in an electric heating blast drying oven at 40°C for drying, crushed and sieved through a 60-mesh sieve, 100g of macadamia nut green peel powder is mixed with 800mL of 80% ethanol, ultrasonically extracted at 60°C for 2h, the macadamia nut green peel extract is centrifuged at 4000r / min for 20min, the supernatant is collected and vacuum evaporated until there is no alcohol taste, and the macadamia nut green peel extract is obtained;

[0014] The preparation process of Houttuynia cordata extract is as follows: extract Houttuynia cordata with 60% ethanol at a constant temperature of 50° C. for 24 hours at a feed-liquid ratio of 1:20-30, filter, and concentrate under reduced pressure at 50° C. to a paste.

[0015] Preferably, the weight ratio of each component is macadamia polypeptide: macadamia peel extract: macadamia leaf extract: Houttuynia cordata extract = 13:1:3:3.

[0016] Preferably, the toothpaste further comprises hydrated silica; the weight ratio of each component is hydrated silica: macadamia polypeptide: macadamia peel extract: macadamia leaf extract: houttuynia cordata extract = 20-30: 7-13: 1-3: 2-4: 2-5.

[0017] Preferably, the weight ratio of each component is hydrated silica: macadamia polypeptide: macadamia peel extract: macadamia leaf extract: Houttuynia cordata extract = 30:13:1:3:3.

[0018] Preferably, the toothpaste further comprises a compound thickener, glycerin, xylitol, Germa BP, dipotassium glycyrrhizinate, and sodium lauryl sulfate; the weight ratio of each component is 1.9:35:2:0.05:0.02:0.01 (the other components mentioned above remain unchanged in the ratios mentioned above).

[0019] Preferably, the compound thickener comprises sodium carboxymethyl cellulose and hydroxyethyl cellulose, wherein the weight ratio of sodium carboxymethyl cellulose to hydroxyethyl cellulose is 1:1.

[0020] The preparation method of toothpaste with macadamia nut polypeptide and extract as main ingredients comprises the following steps:

[0021] (1) Predissolution: weigh xylitol, Germa BP, and dipotassium glycyrrhizinate in a beaker and dissolve them in distilled water;

[0022] (2) Mixing: Pour glycerin into the weighed sodium carboxymethyl cellulose and hydroxyethyl cellulose, and stir quickly to make the thickener evenly dissolved in the glycerin;

[0023] (3) Centrifugation: centrifuge the macadamia polypeptide, macadamia peel extract, and macadamia leaf extract at 8000 r / min for 10 min;

[0024] (4) Grinding: Grind sodium dodecyl sulfate in a mortar, add hydrated silica and continue grinding to mix evenly;

[0025] (5) Mixing and stirring: Heat the distilled water to 50°C, add the pre-dissolved solution, centrifuged solution and the mixed thickener and glycerin, stir evenly until the solution is thick, and add the ground hydrated silica and sodium dodecyl sulfate.

[0026] Preferably, the dissolving temperature in step (1) is 40-50°C.

[0027] Preferably, in step (2), the stirring speed is controlled to be 2000-3000 rpm.

[0028] Preferably, the particle size after grinding in step (4) is 10-15 μm.

[0029] The beneficial effects of the present invention are as follows:

[0030] The present invention uses macadamia polypeptide and other extracts as main ingredients to prepare an antibacterial toothpaste, which increases the amount of plant ingredients used, ensures the pure natural performance of the toothpaste, and improves the antibacterial effect and antioxidant performance. At the same time, since a large amount of macadamia polypeptide extract is used in the formula, it is easy to cause the toothpaste to taste bitter. The present invention solves this problem well and prepares a natural toothpaste product with a fresh taste and a strong nut aroma. In addition, in the toothpaste formula of the present application, there is a synergistic effect between macadamia polypeptide and other extracts and Houttuynia cordata. The combination of these substances significantly improves the antibacterial effect and antioxidant function of the toothpaste, and also makes it have the characteristics of good formability and long shelf life, and the sensory score is good. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0032] Attached Figure 1 is the antibacterial effect of toothpaste on Staphylococcus aureus and Candida albicans; a is the inhibitory effect of toothpaste on Staphylococcus aureus, 1 and 2 are toothpaste samples, and 3 is sterile distilled water; b is the inhibitory effect of toothpaste on Candida albicans, 1 and 2 are toothpaste samples, and 3 is sterile distilled water. DETAILED DESCRIPTION

[0033] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] Experimental materials: macadamia nut oil: provided by Yunnan Tropical Crops Science Research Institute; Jema BP: Beijing Sangpu Biochemical Technology Co., Ltd.; sodium laureth sulfate, cocamidopropyl betaine, lauryl glucoside: Shandong Yousuo Chemical Technology Co., Ltd.; mono- and di-glycerol stearic acid esters: Jialishi Additives (Hai'an) Co., Ltd.; disodium ethylenediaminetetraacetic acid: Sinopharm Chemical Reagent Co., Ltd.; citric acid: MacLean Biochemical Technology Co., Ltd.; phenol, anhydrous sodium sulfate: Sinopharm Chemical Reagent Co., Ltd.; concentrated sulfuric acid: Zunyi Normal University Chemical Reagent Factory; anhydrous ethanol: Tianjin Zhiyuan Chemical Reagent Co., Ltd.; ferrous sulfate: Tianjin Zhiyuan Chemical Reagent Co., Ltd.; sodium hydroxide: Shanghai Shisihewei Chemical Co., Ltd.; aluminum nitrate: Xilong Science Co., Ltd.; potassium sodium tartrate: Ron's reagent; Folin phenol: Ron's reagent ; Trichloroacetic acid: Chongqing Chuandong Chemical (Group) Co., Ltd.; Salicylic acid: Shanghai Xirun Chemical Industry Co., Ltd.; Sodium carbonate: Tianjin Fengchuan Chemical Reagent Technology Co., Ltd.; Copper sulfate: Tianjin Zhiyuan Chemical Reagent Co., Ltd.; DPPH: Tianjin Zhiyuan Chemical Reagent Co., Ltd.; ABTS: Hefei Bomei Biotechnology Co., Ltd.; Potassium persulfate: Beijing Red Star Chemical Plant; H2O2: Chongqing Wansheng Chuandong Chemical Co., Ltd.; Tryptic soytone liquid medium (Qingdao High-tech Industrial Park Haibo Biotechnology Co., Ltd.); Sabouraud glucose liquid medium (Qingdao High-tech Industrial Park Haibo Biotechnology Co., Ltd.); Agarose (Nanjing Quanlong Biotechnology Co., Ltd.); Staphylococcus aureus (ATCC6538) (Shanghai Lu Microbiology); Candida albicans (ATCC10231) (Shanghai Lu Microbiology).

[0035] The main instruments and equipment are shown in Table 1.

[0036] Table 1. Instruments and equipment for the preparation of macadamia toothpaste

[0037]

[0038]

[0039] Example 1 Preparation of macadamia polypeptide

[0040] The preparation process of macadamia polypeptide is as follows: take an appropriate amount of hydraulically pressed macadamia meal for crushing, pass through a 60-mesh sieve, take 15g of macadamia meal and dissolve it in 150mL of distilled water after sieving, bathe in a constant temperature water bath at 60°C for 15min, add 0.075g of compound protease and stir evenly, hydrolyze at 56°C for 3h in a constant temperature water bath, inactivate the enzyme at 85°C for 15min, filter after cooling to obtain macadamia polypeptide, and put it in a refrigerator for refrigeration.

[0041] Example 2 Preparation of Macadamia Leaf Extract

[0042] The preparation process of macadamia leaf extract is as follows: fresh leaves are picked, washed, dried, crushed and passed through a 40-mesh sieve, 12 g of macadamia leaf powder is stirred and dissolved with 960 mL of 70% ethanol, mixed and ultrasonicated at 40°C for 10 min, then shaken for extraction for 1 h, the macadamia leaf extract is centrifuged at 4000 r / min for 20 min, the supernatant is collected and evaporated at 60°C under reduced pressure until there is no alcohol taste, to obtain the macadamia leaf extract, which is then refrigerated.

[0043] Example 3 Preparation of macadamia nut green peel extract

[0044] The preparation process of macadamia nut green peel extract is as follows: select fresh macadamia nut green peel, wash and remove surface impurities, put it into an electric blast drying oven at 40°C for drying, grind it and pass it through a 60-mesh sieve, take 100g of macadamia nut green peel powder and 800mL80% ethanol, mix them evenly, perform ultrasonic extraction at 60°C for 2h, centrifuge the macadamia nut green peel extract at 4000r / min for 20min, collect the supernatant and evaporate it under reduced pressure until there is no alcohol taste, obtain the macadamia nut green peel extract, and put it in the refrigerator for refrigeration.

[0045] Example 4 Preparation of Houttuynia cordata Extract

[0046] The Houttuynia cordata herb was extracted with 60% (v / v) ethanol at a constant temperature of 50°C for 24 hours at a solid-liquid ratio of 1:20-30 (unit: g / mL), filtered, and concentrated under reduced pressure at 50°C to a paste.

[0047] Example 5 Preparation of toothpaste

[0048] (1) Predissolution: Weigh 2 parts of xylitol, 0.05 parts of Germa BP, and 0.02 parts of dipotassium glycyrrhizinate into a beaker and dissolve them in distilled water at 40-50° C. to obtain a predissolved solution.

[0049] (2) Mixing: Pour glycerin into 15.79 parts of sodium carboxymethyl cellulose and 14.21 parts of hydroxyethyl cellulose, and stir rapidly at 2000-3000 rpm to make the thickener evenly dissolved in the glycerin.

[0050] (3) Centrifugation: 13 parts of macadamia polypeptide, 1 part of macadamia green peel extract, 3 parts of macadamia leaf extract, and 3 parts of Houttuynia cordata extract were centrifuged at 8000 r / min for 10 min, and the supernatant was collected to obtain a centrifuge solution.

[0051] (4) Grinding: Grind 0.01 parts of sodium dodecyl sulfate in a mortar, add 30 parts of hydrated silica and continue grinding until the particle size is 10-15 μm, and mix well.

[0052] (5) Mixing and stirring: Heat the distilled water to 50°C, add the pre-dissolved solution, centrifuged solution and the mixed thickener and glycerin, stir evenly until the solution is thick, and add the ground hydrated silica and sodium dodecyl sulfate.

[0053] Experimental Exploration Example 1 Effect of Thickener Compound on Toothpaste Sensory Properties

[0054] According to the preliminary experimental results, samples were prepared according to the corresponding formula and production process in Example 5 to investigate the effect of different addition amounts of sodium carboxymethyl cellulose and hydroxyethyl cellulose (0.8:0.7, 0.9:0.8, 1.0:0.9, 1.1:1.0, 1.2:1.1, m:m) on the sensory properties of macadamia polypeptide toothpaste. The single factor experimental results of the addition amount of the compound thickener are shown in Table 2;

[0055] Table 2 Sensory evaluation of compound thickener addition

[0056]

[0057] From the sensory evaluation of the addition amount of compound thickener in Table 2, it can be seen that the sensory score of toothpaste is different with the different compound addition amount of thickener. Before the compound ratio is 1.0%:0.9%, the stiffness of the toothpaste is slightly poor and it is not easy to set. When it reaches 1.0%:0.9%, the sensory score reaches the highest, and then it decreases significantly. The reason is that the excessive addition of sodium carboxymethyl cellulose in the compound thickener leads to increased viscosity of the toothpaste, and the prepared paste has poor strip-forming properties. Taking comprehensive considerations, the most suitable ratio of sodium carboxymethyl cellulose:hydroxyethyl cellulose is selected as 1.0%:0.9%.

[0058] Experimental Exploration Example 2 Effect of the Addition Amount of Glycerin on the Sensory Properties of Toothpaste

[0059] The addition amount of sodium carboxymethyl cellulose and hydroxyethyl cellulose was determined, and samples were prepared according to the corresponding formula and production process of Example 5, and the effects of the single factor experimental design of different addition amounts of glycerol (20%, 25%, 30%, 35%, 40%, wt%) on the sensory properties of macadamia polypeptide toothpaste were investigated, as shown in Table 3;

[0060] Table 3 Sensory evaluation of glycerol addition

[0061] Glycerol addition amount / % 20 25 30 35 40 Sensory Rating 72.8 74 76 80 76

[0062] From the sensory evaluation of the amount of glycerol added in Table 3, it can be seen that with the increase of the amount of glycerol added, the sensory score of the macadamia polypeptide toothpaste first gradually increased to the highest and then decreased. When the amount of glycerol added reached 35%, the sensory score was the highest, the toothpaste had good color and stiffness, and it could be shaped and had sharp corners when picked up. When the amount of glycerol added was 40%, the toothpaste was too viscous and the stiffness was poor. This was due to the increase in the amount of moisturizer and the increase in the viscosity of the thickener. Taking all factors into consideration, the amount of glycerol added was 35%.

[0063] Experimental Exploration Example 3 Effect of Hydrated Silica Addition Amount on the Sensory Properties of Toothpaste

[0064] The addition amount of sodium carboxymethyl cellulose, hydroxyethyl cellulose and glycerol was determined, and samples were prepared according to the corresponding formula and production process of Example 5, and the effect of the single factor experimental design of different addition amounts of hydrated silica (15%, 20%, 25%, 30%, 35%, wt%) on the sensory properties of macadamia polypeptide toothpaste was investigated. The single factor experimental results of the addition amount of hydrated silica are shown in Table 4;

[0065] Table 4 Sensory evaluation of hydrated silica addition

[0066] Hydrated silica addition amount / % 15 20 25 30 35 Sensory Rating 70 72 81 88 76

[0067] From the sensory evaluation of the amount of hydrated silica added in Table 4, it can be seen that when the amount of hydrated silica is 30%, the sensory properties of the toothpaste are the best, the compatibility with the extract is better, and the paste is uniform and colored. When the added amount is less than 30%, the compatibility with the extract is poor, and the appearance of the toothpaste is apricot-colored. In summary, the amount of hydrated silica added is 30%.

[0068] Experimental Exploration Example 4 Effect of the Addition Amount of Macadamia Peptide on the Sensory Properties of Toothpaste

[0069] The addition amount of sodium carboxymethyl cellulose, hydroxyethyl cellulose, glycerin and hydrated silica was determined, and samples were prepared according to the corresponding formula and production process of Example 5 to investigate the effect of the single factor experimental design of different addition amounts of macadamia polypeptide (4%, 7%, 10%, 13%, 16%, wt%) on the sensory properties of macadamia polypeptide toothpaste. The single factor experimental results analysis of the addition amount of macadamia polypeptide is shown in Table 5;

[0070] Table 5 Sensory evaluation of macadamia nut peptide addition

[0071]

[0072]

[0073] As shown in Table 5, the sensory evaluation of the amount of macadamia polypeptide added shows that when the polypeptide content is 10%, the sensory score of the toothpaste is the highest. The amount of polypeptide added affects the color of the toothpaste. When the addition amount is less than 10%, the color of the paste is off-white. When the addition amount is greater than 10%, the color of the paste is white. However, excessive addition of polypeptide increases the moisture content in the toothpaste, and the stiffness is slightly poor and difficult to shape. Therefore, the optimal addition amount of macadamia polypeptide is 10%.

[0074] Experimental Exploration Example 5 Effect of the Addition Amount of Macadamia Nut Peel Extract on the Sensory Properties of Toothpaste

[0075] The addition amount of sodium carboxymethyl cellulose, hydroxyethyl cellulose, glycerin, hydrated silica, and macadamia polypeptide was determined, and samples were prepared according to the corresponding formula and production process of Example 5 to investigate the effect of different addition amounts of macadamia green peel extract (1%, 2%, 3%, 4%, 5%, wt%) on the sensory properties of macadamia polypeptide toothpaste by single factor experimental design. See Table 6;

[0076] Table 6 Sensory evaluation of the amount of macadamia nut green peel extract added

[0077]

[0078] As shown in Table 6, the sensory evaluation of the addition amount of macadamia nut green peel extract shows that the sensory score of macadamia nut green peel extract gradually increases before the addition amount reaches 2%, and the sensory score drops rapidly after the addition amount reaches 2%, and the sensory score is the highest when the addition amount of macadamia nut green peel extract is 2%, reaching 83 points. This is because macadamia nut green peel extract mainly affects the color of toothpaste. A certain amount of macadamia nut green peel extract can play an antioxidant role, but when the addition amount exceeds 2%, the color of the paste will be apricot due to the strong color of the extract itself. Comprehensively judging, the addition amount of macadamia nut green peel extract is determined to be 2%.

[0079] Experimental Exploration Example 6 Effect of the Addition Amount of Macadamia Leaf Extract on the Sensory Properties of Toothpaste

[0080] The addition amounts of sodium carboxymethyl cellulose, hydroxyethyl cellulose, glycerin, hydrated silica, macadamia polypeptide, and macadamia green peel extract were determined, and samples were prepared according to the corresponding formula and production process of Example 5. The effects of the single-factor experimental design of different addition amounts of macadamia leaf extract (2%, 3%, 4%, 5%, 6%, wt%) on the sensory properties of macadamia polypeptide toothpaste were investigated, as shown in Table 7.

[0081] Table 7 Sensory evaluation of the amount of macadamia leaf extract added

[0082]

[0083]

[0084] As shown in Table 7, the sensory evaluation of the added amount of macadamia leaf extract shows that with the increase of the added amount of macadamia leaf extract, the sensory score of the toothpaste first increases and then decreases. When the added amount of macadamia leaf extract is 4%, the score is the highest, and the color of the paste is white, which is more acceptable. When the added amount of macadamia leaf extract is too much, the color of the paste will be apricot, thus affecting the sensory quality of the toothpaste. In summary, the optimal addition amount of macadamia leaf extract is 4%.

[0085] Experimental Example 1 Orthogonal Experiment

[0086] According to the results of the single factor experiment, an orthogonal experiment of macadamia polypeptide toothpaste was conducted. Four factors were selected: A: hydrated silica, B: macadamia polypeptide, C: macadamia green peel extract, and D: macadamia leaf extract. Three levels were selected for each factor. The comprehensive score results of stability and sensory evaluation were used as the evaluation indicators to conduct an orthogonal experimental design. The factor levels are shown in Table 8, and the orthogonal experimental results are shown in Table 9.

[0087] Table 8 Orthogonal experimental design

[0088]

[0089] Table 9 Analysis of orthogonal experimental results of sensory evaluation of macadamia polypeptide toothpaste

[0090]

[0091]

[0092] The orthogonal experimental results of the sensory evaluation of macadamia polypeptide toothpaste in Table 9 show that the conditional correlation obtained by the analysis is that the amount of macadamia green peel extract added> the amount of macadamia polypeptide added> the amount of hydrated silica added> the amount of macadamia leaf extract added. The optimal combination is A3B3C1D2, so the amount of each raw material added in the toothpaste formula is calculated by weight percentage: the amount of macadamia green peel extract added is 1%, the amount of macadamia polypeptide added is 13%, the amount of hydrated silica added is 30%, and the amount of macadamia leaf extract added is 3%. Among them, the macadamia green peel extract has the greatest impact on the sensory evaluation of toothpaste. It has been verified by experiments that the macadamia polypeptide toothpaste made with the optimal combination (the toothpaste sample prepared using Example 5, the same below) has a white appearance, a fresh and natural smell, a good stiffness, a normal stability test result, and a sensory score of 88 points.

[0093] Experimental Example 2: Toothpaste Sensory Evaluation

[0094] The sensory evaluation of toothpaste was conducted by a professional sensory evaluation team of 5 people from four aspects: appearance, smell, stiffness and stability. The sensory evaluation standards are shown in Table 10:

[0095] Table 10 Sensory index scoring table

[0096]

[0097]

[0098] Experimental Example 3: Product Physical and Chemical Index Testing and Antioxidant Index Testing

[0099] 1. Determination of flavonoids

[0100] The flavonoid content in the product was determined according to the method of Guo Jing (Analysis of the main chemical components of different varieties of bamboo leaves and preparation of bamboo leaf toothpaste [D]. Shanghai University of Traditional Chinese Medicine, 2019), and the toothpaste without extract was used as a blank control, see Table 11;

[0101] Table 11 Flavonoid content of products

[0102] product toothpaste Toothpaste blank Flavonoids (mg / g) 4.15 0.42

[0103] From the flavonoid content in the products in Table 11, it can be seen that the flavonoid content of the toothpaste with added extract is 4.15 mg / g, and the flavonoid content of the blank toothpaste is 0.42 mg / g. The flavonoid content is significantly increased after adding the extract.

[0104] 2. Determination of total phenols

[0105] The total phenol content in the product was determined according to the method of Guo Gangjun et al. (Guo Gangjun, Hu Xiaojing, Fu Jiarong, et al. Analysis of functional components and antioxidant activity of macadamia nut green peel extracts with different polar solvents and their correlation [J]. Food Science, 2021, 42(07): 74-82), and toothpaste without extract was used as blank control. See Table 12.

[0106] Table 12 Total phenol content of products

[0107] product toothpaste Toothpaste blank Total phenols (μg / g) 12.96 0.15

[0108] From the total phenol content in the products in Table 12, it can be seen that there are obvious differences in the total phenol content of different toothpaste products. Among them, the total phenol content in the products with added extracts is much higher than that in the blank control products. The total phenol content in the toothpaste is 12.96μg / g, and the total phenol content in the blank toothpaste is 0.153μg / g. This shows that adding extracts can effectively increase the total phenol content in toothpaste products.

[0109] 3. Determination of polypeptide content in toothpaste

[0110] The standard curve obtained by the biuret method is: Y = 0.5009X + 0.0592, and the correlation coefficient R2 = 0.9988. The absorbance value measured by the ultraviolet spectrophotometer is substituted into the standard curve to calculate the polypeptide content in the toothpaste: 0.32 mg / ml.

[0111] 4. Determination of antioxidant activity

[0112] 1) ABTS free radical scavenging rate determination

[0113] Referring to the method of Wang Ying et al. (Wang Ying, Wang Xinyan, Xu Yushuang, et al. Study on the antibacterial and antioxidant properties of three plant essential oils and pure dew in shower gel and hand soap [J]. China Detergent Industry, 2023, (10): 14-23), toothpaste without extract was used as a blank control.

[0114] 2) DPPH free radical scavenging rate determination

[0115] Referring to the method of Lu Jing et al. (Lu Jing, Zhang Huan, Chen Xin. Research method on the antioxidant activity of propolis extract and its application in toothpaste [J]. Oral Care Products Industry, 2022, 32(01): 9-11), the DPPH free radical scavenging rate in the product was determined, and toothpaste without extract was used as a blank control. The total reducing capacity was determined by referring to the method of preparation process and antioxidant activity of macadamia nut polypeptides with different molecular weights by Fu Jiarong et al., and toothpaste without extract was used as a blank control. The results are shown in Table 13;

[0116] At the same time, set the following comparison ratio:

[0117] Comparative Example 1: removing macadamia polypeptide and keeping other components unchanged;

[0118] Comparative Example 2: Compared with the present invention, the macadamia nut green peel extract was removed, and the other components and weight portions remained unchanged;

[0119] Comparative Example 3: Compared with the present invention, the macadamia leaf extract was removed, and the other components and weight portions remained unchanged;

[0120] Comparative Example 4: Compared with the present invention, the houttuynia cordata extract was removed, and at the same time, the weight portion of the macadamia nut polypeptide was changed to 16 parts;

[0121] Comparative Example 5: Compared with the present invention, the macadamia nut polypeptide is removed, and at the same time, the weight portion of Houttuynia cordata extract is changed to 16 parts.

[0122] Table 13 Antioxidant activity of products

[0123]

[0124]

[0125] As shown in Table 13, the antioxidant activity of the products shows that there is a large difference in antioxidant activity between toothpaste products with and without extracts. The DPPH radical scavenging rate of toothpaste is 85.20%, the ABTS radical scavenging rate is 94.37%, and the reducing power is 0.254; the DPPH radical scavenging rate of blank toothpaste is 3.62%, the ABTS radical scavenging rate is 14.04%, and the reducing power is 0.037. This shows that adding extracts to toothpaste can make the product have better antioxidant capacity.

[0126] At the same time, it can be seen from Comparative Examples 4 and 5 that the inventor only added one of the macadamia polypeptide or the houttuynia extract, but ensured that the total weight of the overall formula remained unchanged. The measured data was significantly different from that of the present invention, which shows that the macadamia polypeptide and the houttuynia extract are not interchangeable. Only when the two exist at the same time can they exert a significant antioxidant effect, indicating that the two have a synergistic effect.

[0127] 5. Determination of product antibacterial activity

[0128] Weigh 10g of the toothpaste sample in a 50mL beaker, add sterile distilled water to make a suspension with a mass concentration of 0.5g / mL. Weigh 10g of the toothpaste sample in a 50mL beaker to make a suspension with a mass concentration of 1g / mL, and refrigerate for later use. Pick a ring of bacteria from the slant of the Staphylococcus aureus strain, inoculate it in the tryptic soytone liquid culture medium, and culture it at 36±1℃ for 18 to 24h. Pick a ring of bacteria from the slant of the Candida albicans strain, inoculate it in the Sabouraud glucose liquid culture medium, and culture it at 26±1℃ for 2 to 5 days. Use sterile distilled water to dilute the two bacterial solutions to a concentration of 1 to 9×10 5 CFU / mL bacterial suspension. Prepare TSA and SDA culture media, sterilize at 121℃ for 15min, cool to 50-60℃, pour 15-20mL of liquid culture medium into each plate, turn it upside down after solidification, and mark the position on the plate. Pipette 100μL of Staphylococcus aureus and Candida albicans suspension onto the plate respectively, and evenly spread it on the plate with an L-shaped coating rod, cover the plate, and dry it at room temperature for 5min. Take 2 sterile dry filter paper pieces and soak them in the toothpaste sample for 1-2s, and take another piece and soak it in sterile distilled water for 1-2s as a control sample. Paste 2 sample pieces on each plate, 1 piece for the photo, and make 2 parallels, cover the plate, seal it with sealing film, and place it in a constant temperature incubator for 16-18h and observe it. Take the outer edge of bacterial growth as the measurement point, use the cross method, and use a vernier caliper to accurately measure the diameter of the inhibition zone and take the average value. The toothpaste samples were tested in the same way. If the diameter of the antibacterial zone is greater than 7 mm, there is an antibacterial effect, otherwise there is no antibacterial effect. Figure 1 and Table 14.

[0129] Table 14 The results of the determination of the diameter of the inhibition zone of toothpaste against Staphylococcus aureus and Candida albicans

[0130] strain sample Diameter of inhibition zone (mm) Staphylococcus aureus toothpaste 13.08±1.31 Candida albicans toothpaste 9.09±0.46

[0131] The experimental results show that toothpaste has good antibacterial activity against Staphylococcus aureus and Candida albicans, and the average diameter of the antibacterial zone is greater than 8mm. According to the "Antimicrobial Susceptibility Test Implementation Standard" issued by the National Committee for Clinical Laboratory Standards (NCCLS), diameters > 20mm are extremely sensitive, 15-20mm are highly sensitive, 10-15mm are moderately sensitive, and <10mm are low sensitive. As can be seen from Table 14, toothpaste is moderately sensitive to Staphylococcus aureus and lowly sensitive to Candida albicans.

[0132] At the same time, the antibacterial properties of the toothpastes of Comparative Examples 1-5 were measured by the above method, as shown in Table 15;

[0133] Table 15 Antibacterial properties of comparative toothpaste

[0134]

[0135] It can be seen from Comparative Examples 4 and 5 that the inventor only used one of the macadamia polypeptide or the houttuynia extract, but ensured that the total weight of the overall formula remained unchanged. However, the measured data was significantly different from that of the present invention, which shows that the macadamia polypeptide and the houttuynia extract are not interchangeable. Only when the two exist at the same time can they exert a significant antioxidant effect, indicating that the two have a synergistic effect.

[0136] In addition, since the toothpaste prepared in Example 5 of the present invention has better antibacterial performance than the toothpaste prepared in Comparative Examples 1-5, the shelf life of the toothpaste of the present invention is longer. After experimental verification, under the same strain contamination, the shelf life of the toothpaste sample of the present invention is 1-3 months longer than that of Comparative Examples 1-5.

[0137] The various embodiments are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referred to in detail.

[0138] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A toothpaste with macadamia polypeptide and extract as main ingredients, characterized in that: The toothpaste mainly comprises: macadamia polypeptide, macadamia green peel extract, macadamia leaf extract and houttuynia cordata extract; the weight ratio of each component is macadamia polypeptide: macadamia green peel extract: macadamia leaf extract: houttuynia cordata extract=7-13:1-3:2-4:2-5; The preparation process of the macadamia polypeptide is as follows: hydraulically pressed macadamia meal is crushed, passed through a 60-mesh sieve, 15 g of macadamia meal is dissolved in 150 mL of distilled water after sieving, and the mixture is placed in a constant temperature water bath at 60° C. for 15 min, 0.075 g of a composite protease is added and stirred evenly, and enzymolysis is performed at 56° C. for 3 h in a constant temperature water bath, and the enzyme is inactivated at 85° C. for 15 min, and the macadamia polypeptide is filtered after cooling to obtain the macadamia polypeptide, which is then placed in a refrigerator for refrigeration; The preparation process of macadamia leaf extract is as follows: fresh leaves are picked, washed, dried, crushed and passed through a 40-mesh sieve, 12 g of macadamia leaf powder is stirred and dissolved with 960 mL of 70% ethanol, mixed and ultrasonicated at 40°C for 10 min, then shaken for extraction for 1 h, the macadamia leaf extract is centrifuged at 4000 r / min for 20 min, the supernatant is collected and vacuum evaporated at 60°C until there is no alcohol taste, to obtain the macadamia leaf extract, which is then refrigerated; The preparation process of macadamia nut green peel extract is as follows: fresh macadamia nut green peel is selected, cleaned to remove surface impurities, placed in an electric blast drying oven at 40°C for drying, crushed and sieved through a 60-mesh sieve, 100g of macadamia nut green peel powder is mixed with 800mL of 80% ethanol, ultrasonically extracted at 60°C for 2h, the macadamia nut green peel extract is centrifuged at 4000r / min for 20min, the supernatant is collected and vacuum evaporated until there is no alcohol taste, and the macadamia nut green peel extract is obtained; The preparation process of Houttuynia cordata extract is as follows: extract Houttuynia cordata with 60% ethanol at a constant temperature of 50° C. for 24 hours at a feed-liquid ratio of 1:20-30, filter, and concentrate under reduced pressure at 50° C. to a paste.

2. A toothpaste with macadamia polypeptide and extract as main ingredients according to claim 1, characterized in that: The weight ratio of each component is macadamia polypeptide: macadamia green peel extract: macadamia leaf extract: houttuynia cordata extract = 13:1:3:

3.

3. The toothpaste with macadamia polypeptide and extract as main ingredients according to claim 1, characterized in that: The toothpaste also includes hydrated silica; the weight ratio of each component is hydrated silica: macadamia polypeptide: macadamia green peel extract: macadamia leaf extract: houttuynia cordata extract = 20-30: 7-13: 1-3: 2-4: 2-5.

4. The toothpaste with macadamia polypeptide and extract as main ingredients according to claim 3, characterized in that: The weight ratio of each component is hydrated silica: macadamia polypeptide: macadamia peel extract: macadamia leaf extract; houttuynia cordata extract = 30:13:1:3:

3.

5. A toothpaste with macadamia polypeptide and extract as main ingredients according to any one of claims 1 to 4, characterized in that: The toothpaste also includes a compound thickener, glycerin, xylitol, Germa BP, dipotassium glycyrrhizinate and sodium lauryl sulfate; the weight ratio of each component is 1.9:35:2:0.05:0.02:0.

01.

6. The toothpaste with macadamia polypeptide and extract as main ingredients according to claim 5, characterized in that: The compound thickener comprises sodium carboxymethyl cellulose and hydroxyethyl cellulose, wherein the weight ratio of sodium carboxymethyl cellulose to hydroxyethyl cellulose is 1:0.

9.

7. A method for preparing a toothpaste with macadamia polypeptide and extract as main ingredients as claimed in any one of claims 5 to 6, characterized in that: The preparation method comprises the following steps: (1) Predissolution: weigh xylitol, Germa BP, and dipotassium glycyrrhizinate in a beaker and dissolve them in distilled water to obtain a predissolved solution; (2) Mixing: Pour glycerin into the weighed sodium carboxymethyl cellulose and hydroxyethyl cellulose, and stir quickly to make the thickener evenly dissolved in the glycerin; (3) Centrifugation: centrifuge the macadamia polypeptide, macadamia peel extract, and macadamia leaf extract at 8000 r / min for 10 min; (4) Grinding: Grind sodium dodecyl sulfate in a mortar, add hydrated silica and continue grinding to mix evenly; (5) Mixing and stirring: Heat distilled water to 50°C, add the pre-dissolved solution, centrifuged solution and the mixed thickener and glycerin, stir evenly until the solution is thick, and add the ground hydrated silica and sodium dodecyl sulfate.

8. The preparation method according to claim 7, characterized in that: The dissolving temperature in step (1) is 40-50°C.

9. The preparation method according to claim 7, characterized in that: In step (2), the stirring speed is controlled to be 2000-3000 rpm.

10. The preparation method according to claim 7, characterized in that: The particle size after grinding in step (4) is 10-15 μm.

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