WO2022179254A1 - Southern medicine compound toothpaste specifically for middle-aged and elderly people, and preparation method therefor - Google Patents

Abstract

A southern medicine compound toothpaste specifically for middle-aged and elderly people, and a preparation method therefor, which belong to the technical field of toothpaste processing. In accordance with the characteristics of the oral cavity of middle-aged and elderly people, and by means of multiple experimental screening, it is found that volatile oils of four southern medicines, which include Alpiniae officinarum rhizoma, Amomum longiligulare, Galangae fructus and Blumea balsamifera, are added to a toothpaste, so that the toothpaste has good antibacterial and anti-inflammatory effects. Moreover, the problem of the stability of the toothpaste being poor due to a high dosage being required when using a single Chinese herbal medicine, or the usability of the toothpaste being affected due to a pungent smell or a strong medicine flavor, is solved; and glycyrrhizic acid, citric acid and zinc citrate are compounded as a compound functional substance, so that the bacteriostasis performance and the desensitization effect of the toothpaste are enhanced. The southern medicine compound toothpaste specifically for middle-aged and elderly people does not damage dentin, has good cleanliness, is antibacterial, anti-inflammatory, anti-allergy, and is refreshing and comfortable. In addition, the toothpaste is suitable regarding the characteristics of susceptibility to allergies, a high incidence of bacterial caries, and common periodontitis and odontitis of the teeth of middle-aged and elderly people, has a clean, fine and smooth paste, moderate foam, is easy to extrude, has a good stability, and is easy to popularize and apply.

Description

A kind of south medicine compound toothpaste with special effect for middle-aged and elderly people and preparation method thereof technical field

The invention belongs to the technical field of toothpaste processing, and in particular relates to a compound toothpaste of southern medicine that is effective for middle-aged and elderly people and a preparation method thereof.

Background technique

The oral diseases of middle-aged and elderly people are different from those of young people, and the incidence rate is higher. The results of the third national oral health epidemiological survey show that the prevalence of dental caries in the middle-aged and elderly people in my country is as high as 88.1% and 98.4%, respectively. The health rate is 14.5% and 14.1% respectively. Oral disease is an important public health problem that threatens the health of middle-aged and elderly people in my country. Due to the changes of physiological age, the tissues of the middle-aged and the elderly are gradually aging, and the function of the organs is declining. The changes in the oral cavity also go through this natural development process, and various oral diseases are prone to occur, especially the teeth. Due to the wear and tear of chewing for decades , The enamel on the tooth surface is worn away in a large amount, the dentin is prone to allergies, and due to the easy retention of food in the mouth and the exposure of the gums, there are many cariogenic bacteria in the middle-aged and the elderly, and periodontal diseases such as gingivitis and periodontitis are common. Cause or aggravate heart disease, stomach disease, diabetes, cardiovascular disease and joint disease and complications, and seriously endanger the health of the whole body. Toothpaste is an oral hygiene product containing a variety of ingredients. It can not only remove the food residues remaining between the teeth and the dirt attached to the surface of the teeth, but also clean the oral cavity. Thereby it has a certain effect on preventing bacterial infection and reducing oral diseases.

At present, when a single Chinese herbal medicine is used in toothpaste in my country, the dosage required is generally higher, which often results in poor stability of the paste, or affects its usability due to irritating odor or strong medicinal taste. Therefore, two or two kinds of herbal medicines are generally used. The above drugs are used to form compound toothpaste and improve the curative effect of toothpaste. However, because most Chinese herbal toothpastes are added with extracts or extracts, the color and luster are darker and are not easily accepted by consumers, and a large amount of active ingredients needs to be added to achieve the effect. Affect paste stability. In addition, there are currently few Chinese herbal compound toothpastes on the market for the oral problems of the middle-aged and the elderly. To develop a toothpaste that does not damage the dentin, is antibacterial and anti-inflammatory, and resists dentin hypersensitivity, and does not affect the basic performance and sensory effects of the toothpaste, has become a kind of toothpaste. Problems to be solved.

SUMMARY OF THE INVENTION

In view of the deficiencies of the prior art, in order to solve the above-mentioned problems, the purpose of the present invention is to provide a kind of south medicine compound toothpaste that is effective for middle-aged and elderly people, aiming at the oral characteristics of the middle-aged and elderly people, screening the south medicine Chinese herbal medicines that can be used for oral hygiene products, The volatile oil of the main active ingredient of the southern medicine used in the present invention is added, which does not affect the color of the paste. By combining the volatile oil compound of four kinds of southern medicine with glycyrrhizic acid, citric acid and zinc citrate as the compound efficacy substances, it not only solves the problem of high dosage of a single Chinese herbal medicine Problems affecting the sensory effect of toothpaste, but also antibacterial, anti-inflammatory, and anti-dentin hypersensitivity. In addition, the present invention also finds that aluminum hydroxide with different particle sizes is combined with silicon dioxide as a toothpaste friction agent, which does not damage the dentin. Finally, the combination of peppermint and citron fruit oil not only covers the bad smell of Chinese herbal medicine, but also refreshes and refreshes.

The scheme of the present invention includes the following aspects:

On the one hand, the present invention provides a kind of south medicine compound toothpaste that is effective for middle-aged and elderly people, including the following raw materials by weight:

Preferably, the raw material also contains 0.05%-0.15% by weight of glycyrrhizic acid.

Preferably, the friction agent is aluminum hydroxide and silicon dioxide.

Preferably, the particle size of the aluminum hydroxide is 2.6 μm and 11 μm. Among them, the mass ratio of 2.6 μm particle size aluminum hydroxide, 11 μm particle size aluminum hydroxide and silica is 2:1:1. Choose two kinds of aluminum hydroxide with different particle sizes and silica, according to a certain ratio to make an abrasive toothpaste that does not damage the dentin, and the abrasive has stable chemical properties, does not react with the functional substances in the toothpaste, and has the best effect. compatibility.

Preferably, the essence includes menthol and citron fruit oil, the weight percentage of menthol in the raw material is 0.3%-0.6%, and the weight percentage of citron fruit oil in the raw material is 0.1%-0.2%. The menthol used has a strong effect of promoting penetration, which makes the toothpaste have a cool taste and fresh breath; the citron used is a traditional Chinese medicine with the same origin of medicine and food, and its volatile oil has a clear aroma and can be used as an odor inhibitor, which can make people feel comfortable and happy. It can also enhance antibacterial properties.

Preferably, the Amomum chinensis is Hainan Amomum chinensis.

Preferably, the mass concentration of the sorbitol liquid is 70%.

Preferably, the middle-aged and old-aged compound toothpaste is made from the following raw materials by weight:

In the above-mentioned raw material formula of the present invention, the volatile oils of southern medicine galangal, Hainan Amomum chinensis, red cardamom and aina incense are compounded in a certain proportion to play the role of inhibiting bacteria, reducing inflammation and promoting penetration. The compatibility and synergy of southern medicine with glycyrrhizic acid, citric acid and zinc citrate can enhance the antibacterial, anti-inflammatory and anti-allergic properties of toothpaste. The addition of desensitizers citric acid and zinc citrate, and the use of polyols (sorbitol and propylene glycol) as humectants can promote the penetration of citrate anions into dentin to enhance the effectiveness of desensitizers. The added volatile oil will affect the emulsification of the paste to a certain extent, and the sodium pyrophosphate in the formula is used as a stabilizer to prevent the oil phase from precipitation from the paste. The added hydroxyapatite is an inducing factor for bones or teeth. In the field of oral health care, it has good remineralization, desensitization, whitening and promotion of gingivitis healing, and has good effects on caries and periodontal diseases. A better prevention and control effect plays an auxiliary role here. The added foaming agent is the combination of sodium lauryl sulfate and sodium lauroyl sarcosinate, which can not only increase the fineness and fullness of the toothpaste foam, but also prevent the oil phase from separating out of the paste. The added sweeteners are sodium saccharin and glycyrrhizic acid. In addition to being a functional substance, glycyrrhizic acid can also be used as a sweetener in the formula. Its sweetness is 200 times that of sucrose, and the amount of sweetener used in the formula can be reduced. Mask the bitter taste of the functional substance.

On the other hand, the present invention also provides the preparation method of the described middle-aged and old-aged compound toothpaste, comprising the following steps:

S1: Take galangal oil, Aina sesame oil, Amomum oil and red cardamom oil, set aside;

S2: Take hydroxyapatite and sodium pyrophosphate, grind, sieve, and set aside;

S3: Glue preparation: pre-disperse CMC-Na in propylene glycol to obtain propylene glycol glue, then add sorbitol solution and water, stir until uniform without transparent particles, stir for 20- 30min, pay attention to prevent water from evaporating during the stirring process. After the end, let it stand, and wait until the glue is fully swelled for use;

S4: Preparation of paste: Weigh mud methyl methyl ester, sodium pyrophosphate, sodium saccharin, citric acid, and zinc citrate in proportion, add water for heating, fully stir and dissolve, add to the glue solution and stir evenly; then add water Add to the swollen glue in step S2, when heated to 70-75°C, first add a foaming agent and stir evenly; then add a friction agent and hydroxyapatite in turn, stir first and fully mix with the glue, then at a temperature of 70 -75℃, keep stirring at 800-1000rpm for at least 20min, then adjust the speed to 500-700rpm and stir for at least 30min to obtain the toothpaste base;

S5: When the temperature of the toothpaste paste base drops to 40-45°C, add galangal oil, Aina sesame oil, Amomum oil, cardamom oil, glycyrrhizic acid and essence in sequence, and fully stir for at least 30min under the condition of rotating speed 500-600rpm, vacuum After degassing, let it stand to get the toothpaste.

The beneficial effects obtained by the present invention:

(1) The present invention uses aluminum hydroxide (2.6 μm) and aluminum hydroxide (11 μm) with different micron-level friction agents of silica in a certain proportion to prepare non-damaging dentin abrasives, which are suitable for middle-aged and elderly people with severe tooth wear specialty.

(2) the present invention adopts the volatile oil of these four kinds of southern medicines of galangal, Hainan Amomum, red cardamom, Aina incense for compounding, plays the role of bacteriostasis, anti-inflammatory and promoting penetration in toothpaste, and is suitable for middle-aged and elderly bacterial caries High prevalence, gingivitis and periodontitis are common characteristics of periodontal disease.

(3) The present invention synergizes four kinds of southern medicines with glycyrrhizic acid, citric acid and zinc citrate to improve the antibacterial performance and anti-allergic performance of toothpaste, and is suitable for the characteristics of middle-aged and elderly people who are prone to tooth allergies.

(4) The present invention also adds hydroxyapatite as an adjuvant to enhance desensitization, reduce oral plaque, promote the healing of gingivitis, and can also be used as a tooth mineralization repair agent.

(5) The toothpaste fragrance type adopted by the present invention is through the screening of various fragrances, and it is unexpectedly found that the menthol fragrance and the citron fruit oil can not only cover up the bad smell of the medicinal substance, but also make the toothpaste achieve a refreshing and refreshing effect.

(6) The south medicine compound toothpaste specially effective for middle-aged and elderly people disclosed in the present invention has the effects of no damage to dentin, good cleanliness, antibacterial and anti-inflammatory, anti-allergic and refreshing and refreshing, and achieves the effect of preventing and treating oral diseases of the middle-aged and elderly people.

Description of drawings

Fig. 1: the preparation process flow chart of toothpaste of the present invention;

Figure 2: Real picture of toothpaste; in the figure, (A) is the toothpaste base; (B) is the sample toothpaste of the best level group; (C) is the sample toothpaste of the best level group.

Detailed ways

In order to better understand the technical content of the present invention, specific embodiments are provided below to further illustrate the present invention.

The raw materials of galangal, Hainan Amomum, red cardamom, and citron were collected from the South Medicine Germplasm Resource Garden, Institute of Tropical Crop Variety Resources, Chinese Academy of Tropical Agricultural Sciences;

Ainaxiang branches and leaves were collected from Ainaxiang Germplasm Resource Garden, Institute of Tropical Crop Variety Resources, Chinese Academy of Tropical Agricultural Sciences;

Other toothpaste accessories are purchased through online or offline stores according to quality requirements.

Embodiment 1 The preparation process optimization experiment of toothpaste of the present application

1.1 Screening of functional substances

According to the antibacterial properties of the volatile oils of galangal, Hainan Amomum, red cardamom, and Aina incense, the invention uses the volatile oils of these four kinds of southern medicines as the king medicine, supplemented by glycyrrhizic acid to enhance the antibacterial properties, and then according to the oral easiness of the middle-aged and elderly people. Allergy characteristics, with citric acid and zinc citrate as desensitizers, hydroxyapatite as tooth mineralization restoration agent.

1.2 Screening of basic ingredients of toothpaste

After decades of use on the teeth of middle-aged and elderly people, the enamel on the surface has been basically worn out. Therefore, in the selection of friction agents, raw materials with a small friction coefficient and no damage to the tooth quality should be used; aluminum hydroxide has stable performance and can clean teeth. It is strong and does not damage the quality of the teeth, and can also improve the water separation phenomenon of toothpaste. Silicon dioxide is a flexible friction agent with stable chemical properties. Compatibility, in addition, its structure is a round honeycomb polymer particle filled with small voids, which has a large contact area with the dirt on the tooth surface. The combination of the two different particle sizes can clean the teeth without damaging the dentine. Therefore, according to the Chinese According to the characteristics of the teeth of the elderly, aluminum hydroxide and silicon dioxide of different micron grades were selected as friction agents, and 2.6μm aluminum hydroxide was used as the main friction agent. Citric acid and zinc citrate are selected as functional substances as desensitizers, and polyols are used as humectants, which can promote the penetration of citric acid anions into dentin and enhance the effectiveness of desensitizers. Therefore, sorbitol and propylene glycol are selected as desensitizers. Moisturizer; Sodium carboxymethyl cellulose is selected as the adhesive; the added essential oil will affect the emulsification of the paste to a certain extent, and the sodium pyrophosphate in the formula is used as a stabilizer to prevent the oil phase from precipitating from the paste. The combination of sodium lauryl sulfate and sodium lauroyl sarcosinate as the foaming agent can not only increase the fineness and fullness of the toothpaste foam, but also avoid the precipitation of the effective substance oil phase from the paste. The sweetener is sodium saccharin. Due to the high sweetness of glycyrrhizic acid in the functional substance, it can also be used as a sweetener in the recipe; through many preliminary experiments, it was unexpectedly found that the combination of menthol and citron oil can not only cover up the functional substance The bitter and astringent taste can also make the toothpaste fresh and refreshing. The toothpaste ingredients are obtained through screening, as shown in Table 1.

Table 1 Toothpaste ingredient list

raw material name	Quality requirements
Galangal Oil	pure essential oil
Aina sesame oil	pure essential oil
Hainan Amomum Oil	pure essential oil
Cardamom Oil	pure essential oil
Glycyrrhizinate	Content≥98%
citric acid	Food grade, content ≥ 99.8%
Zinc citrate	Food grade, content ≥ 98%
Hydroxyapatite	Cosmetic grade, content ≥ 99%

Aluminum hydroxide (2.6um)	Particle size 5000, toothpaste grade
Aluminum hydroxide (11um)	Particle size 1250, toothpaste grade
silica	Particle size 1250, toothpaste grade
70% Sorbitol Liquid	Food grade, ≥70%
Propylene Glycol	Cosmetic grade, content ≥ 99.5%
CMC-Na (Sodium Carboxymethyl Cellulose)	Food grade, acid resistant and high viscosity
Sodium pyrophosphate	food grade
K12 (Sodium Lauryl Sulfate)	Industrial grade
Sodium Lauroyl Sarcosinate	Industrial grade
Mud gold methyl ester	food grade
Sodium Saccharin	food grade
Menthol	Pharmaceutical Grade
Citron Fruit Oil	fruity
Deionized water

1.3 Toothpaste formulation process

S1: Take the dried galangal rhizomes, the dried Aina incense leaves, Hainan Amomum chinensis and red cardamom fruits according to a certain amount, crush them to 40 meshes with a pulverizer, add 8-10 times the mass of the powder and soak them in distilled water for 2 hours. Then carry out steam distillation extraction, extract 3 times, and the extraction time is respectively 4 hours, 3 hours, 2 hours, and the volatile oils obtained for three times are combined to obtain respectively galangal oil, Aina sesame oil, Hainan Amomum oil and Cardamom oil for subsequent use.

S2: Take hydroxyapatite and sodium pyrophosphate, grind them into very fine powder first, then pass through a 150-mesh sieve for use;

S3: Glue preparation: pre-disperse CMC-Na in propylene glycol to obtain propylene glycol glue, then add 70% sorbitol solution and a small amount of water to the beaker, stir until uniform without transparent particles, at a temperature of 70-75°C and a rotation speed of 700-1000rpm Condition, stir for 20-30min, pay attention to prevent water from evaporating during the stirring process, after the end, stand still for about 12h, wait for the glue to fully swell, and set aside.

S4: Making ointment: Weigh mud methyl methyl ester, sodium pyrophosphate, sodium saccharin, citric acid, and zinc citrate into a beaker in proportion, add water for heating, fully stir until completely dissolved, and then add to the glue Stir well; then add the remaining deionized water to the swollen glue, when heated to 70-75 ℃, add the foaming agent first, and stir evenly. During the process, a large amount of foam is generated; then add friction agent and hydroxyapatite with different particle sizes in turn (adding at this time again plays a role in defoaming), first stir by hand and fully mix with the glue, and keep it at a temperature of 70-75 ° C. After fully stirring at 800-1000rpm for 20min, the speed is adjusted to 500-700rpm and then stirred for 30min, so that it is fully stirred to obtain a toothpaste base;

S5: When the temperature of the toothpaste base drops to 40-45°C, add the functional substances galangal oil, Aina sesame oil, Hainan Amomum oil, cardamom oil, glycyrrhizic acid and essence in turn, and stir them for 30 minutes at a speed of 500-600rpm. , after vacuum degassing, stand still for 24h to obtain toothpaste.

1.3.2 Sensory evaluation

Sensory indicators are the most intuitive indicators for evaluating the quality of toothpaste. According to the requirements of the new national standard for toothpaste, this experiment adopts a five-level 100-point scoring method for sensory evaluation. The evaluation method is as follows:

(1) Forming situation: Put the prepared paste into a piping bag, cut it into the diameter of the mouth of the toothpaste tube, squeeze a strip of toothpaste from the piping bag onto the filter paper that is easy to absorb water, and squeeze it out with slight force. If the force is large and it is not easy to squeeze out the paste, it means that the toothpaste is too thick; otherwise, the paste is too thin, the thickness is moderate, and the drawing is obvious; whether the extruded paste is easy to cut.

(2) Form of paste: Squeeze out two strips of toothpaste and put them on black paper, observe whether the paste is clean, uniform and delicate, whether the water is separated, whether the color is normal or whether there are impurities; whether the whole is collapsed downward; the paste is placed Whether it dries quickly for a period of time. Use a pin to mark a groove of 0.5 to 1 cm on the surface of a paste, and observe whether the groove maintains its shape within an appropriate period of time. If it is normal, it indicates that the paste is normal.

(3) Taste: Distribute the sample toothpaste for each test to 10 fixed middle-aged and elderly people for trial, and record whether the taste is fresh and comfortable, whether the cooling degree is moderate, whether there is a spicy and bitter taste, and whether the taste is moderate or moderate. Score according to the following criteria.

(4) Look at the water seepage phenomenon: squeeze some toothpaste and put it on the raw edge paper, spread it out evenly with your fingers, and check whether there is water seepage on the reverse side of the paper, and the toothpaste of good quality has little water seepage;

(5) Check whether there are too hard particles: apply a little toothpaste on the slide, press it evenly with your fingers, wash and observe whether the slide is scratched, if there is any scratches on the teeth when brushing your teeth;

(6) Determination of the amount of foam: Weigh 45 ℃, 20ml of water in advance, weigh 1g of toothpaste to be tested in a beaker, add a small amount of water to dissolve the paste, pour the dissolved paste into a stoppered measuring cylinder, and use the remaining water Clean the beaker, pour it into the measuring cylinder, close the stopper, press the stopper tightly, shake the solution in the measuring cylinder with maximum force, and stop after the paste is completely dissolved by visual inspection. The position where the foam distribution of the cylinder is most concentrated shall prevail, and the amount of foaming shall be recorded.

Table 2 Sensory evaluation criteria

1.3.3 Determination of the dosage of toothpaste formula

Among the above toothpaste ingredients, the dosage of functional substances, friction agents, humectants, thickeners, foaming agents, sweeteners and essences has a great influence on the sensory evaluation of the whole toothpaste paste. Aluminum (2.6μm): aluminum hydroxide (11μm): silicon dioxide = 2:1:1, the ratio of moisturizing agent 70% sorbitol solution and propylene glycol is 2.5:1, foaming agent K12 and lauroyl sarcosine Sodium is added in the amount of 1:1, and the functional substances are 1.1% (galangal oil 0.1%, Aina sesame oil 0.1%, Hainan Amomum oil 0.1%, cardamom oil 0.1%, glycyrrhizic acid 0.05%, citric acid 0.1%, Zinc citrate 0.55%), 2.08% (galangal oil 0.15%, Aina sesame oil 0.25%, Hainan Amomum oil 0.2%, Cardamom oil 0.2%, Glycyrrhizic acid 0.08%, Citric acid 0.2%, Zinc citrate 1% ), 2.8% (galangal oil 0.3%, aina sesame oil 0.35%, Hainan Amomum oil 0.35%, cardamom oil 0.35%, glycyrrhizic acid 0.15%, citric acid 0.3%, zinc citrate 1%), essence 0.4% (menthol 0.3%, citron oil 0.1%), 0.55% (menthol 0.4%, citron oil 0.15%), 0.8% (menthol 0.6%, citron oil 0.2%) in order to further optimize the toothpaste formula , using 7 factors and 3 levels (L ₁₈ (3 ⁷ )) orthogonal experimental design, the best formula technology was screened according to the above sensory scores. Hydroxyapatite, nipogine methyl ester and sodium pyrophosphate have little effect on the sensory evaluation of the whole toothpaste paste, and can be added to the formula in proportions of 1.5-2.5%, 0.1-0.2% and 0.2-0.5% respectively. In this experiment, the hydroxyapatite was added at 2%, the methyl naphthalene was added at 0.15%, and the sodium pyrophosphate was added at 0.3%. Each formula was made into toothpaste by the processing technology of 1.3 toothpaste formula for sensory evaluation. The result is as follows:

Table 3 Orthogonal factor level table

Table 4 Orthogonal experimental scheme and results

Experiment number	A	B	C	D	E	F	G	Sensory Score
1	1	1	1	1	1	1	1	79.4
2	1	2	2	2	2	2	2	89.8
3	1	3	3	3	3	3	3	81
4	2	1	1	2	2	3	3	86.3
5	2	2	2	3	3	1	1	86.1
6	2	3	3	1	1	2	2	84.6
7	3	1	2	1	3	2	3	81.6
8	3	2	3	2	1	3	1	86.1
9	3	3	1	3	2	1	2	85.3
10	1	1	3	3	2	2	1	87.5
11	1	2	1	1	3	3	2	86.2
12	1	3	2	2	1	1	3	86.4
13	2	1	2	3	1	3	2	88.2
14	2	2	3	1	2	1	3	82.9
15	2	3	1	2	3	2	1	91.3
16	3	1	3	2	3	1	2	86
17	3	2	1	3	1	2	3	84.8
18	3	3	2	1	2	3	1	89.5
mean 1	85.050	84.833	85.550	84.033	84.917	84.350	86.650
mean 2	86.567	85.983	86.933	87.650	86.883	88.600	86.683
mean 3	85.550	86.350	84.683	85.483	85.367	86.217	83.833
very poor	1.517	1.517	2.250	3.617	1.966	2.250	2.850

From the above test results, it can be concluded that the influence of various factors on the sense of toothpaste is D>G>C=F>E>A=B, that is, the amount of foaming agent has the greatest influence on toothpaste, followed by essence, adhesive and Sodium Saccharin. According to the intuitive analysis, the optimal composition of ingredients is A ₂ B ₃ C ₂ D ₂ E ₂ F ₂ G ₂ , that is, friction agent 40%, moisturizing agent 35%, adhesive 1.5%, foaming agent 2.5%, efficacy substance 2.08% %, sodium saccharin 0.2%, flavor 0.55%. It can be seen from variance analysis that each factor A has no significant effect on toothpaste.

1.3.4 Verification experiment

In order to examine the reproducibility of the optimal experiment, this experiment finds out the best level combination from the experiments that have been done and the optimal combination obtained through data analysis to do a comparative experiment to compare their advantages and disadvantages. For this example, the combination of the best level found by sensory scoring is Experiment No. 15, namely A ₂ B ₃ C ₁ D ₂ E ₃ F ₂ G ₁ and the best level found by range analysis A ₂ B ₃ C ₂ D ₂ E ₂ F ₂ G ₂ did a comparative experiment to further judge whether the found production process conditions were optimal. The results are as follows, the optimal level group is better than the best level group in terms of taste.

Table 5 Validation test results

1.3.5 Stability test

The stability test refers to the stability test method in "Toothpaste (GB/T 8372-2017)". Take 2 pieces of toothpaste in the optimal level group and 2 pieces of toothpaste in the best level group, store 2 samples at room temperature, and put the other 2 samples in a refrigerator at -8°C±1°C, take them out after 8 hours, and then put them at 45°C±1°C. In a constant temperature incubator at 1°C, take it out after 8 hours, return to room temperature, open the lid, and the paste does not overflow the mouth of the tube; turn the toothpaste tube upside down, and no liquid drips from the mouth within 10 seconds; compare the samples stored at room temperature after the paste is extruded , its fragrance and color are normal.

Embodiment 2 Antibacterial performance detection of compound efficacy toothpaste

2.1 Test materials and introduction

Strain: Streptococcus mutans standard strain (SM), ATCC25175; Porphyromonas gingivalis standard strain (Porphyromonas gingivalis, PG), ATCC33277; strains were provided by the molecular biology laboratory of Chengdu Lilai Biotechnology Co., Ltd. Among them, Streptococcus mutans is one of the genus Streptococcus with the largest proportion of oral cavity, and it is the main pathogenic bacteria of gingival disease; Porphyromonas gingivalis is the main cause of chronic and invasive periodontitis, gingival abscess and periodontal infection. Therefore, the antibacterial properties of these two bacteria were mainly tested.

Culture medium: rabbit blood brain heart infusion broth (BHI) medium (Shanghai Yuanye Biotechnology Co., Ltd.), anaerobic meat liver soup (Beijing Soleibo Technology Co., Ltd.).

Blank toothpaste (no added efficacy substances and flavors) and sample toothpaste 1 (functional substances 1.1%), sample toothpaste 2 (functional substances 2.08%), sample toothpaste 3 (functional substances 2.8%) and sample toothpaste 4 (functional substances do not contain Glycyrrhizic acid, other same ratio as sample toothpaste 2)

2.2 Test method

Bacterial liquid preparation: Inoculate 50 μL of the standard strains Streptococcus mutans and Porphyromonas gingivalis stored at low temperature into rabbit blood BHI medium, streak them to form a single colony, and place the inoculated plate in an anaerobic box medium (80% N ₂ , 10% H ₂ , 10% CO ₂ ) for 3d activation. Then pick the plate colonies and inoculate them into anaerobic meat liver soup for 72 hours, and the concentration of the bacteria liquid was determined by UV _{spectrophotometer} to be between 0.5 and 1.0.

Preparation of antibacterial samples: Weigh 3.0g of the four toothpastes respectively, add 10ml of deionized water and stir to obtain a sample solution, soak the sterile filter paper (d=6mm) in the prepared sample solution for 5min, and extract the It is placed flat in a sterilized plate, dried at room temperature and used for later use, to obtain sample toothpaste 1, sample toothpaste 2, sample toothpaste 3, and sample toothpaste 4.

Preparation of negative control sample 1

Weigh 3.0 g of blank toothpaste (without added efficacy substances and fragrance), add 10 ml of deionized water and stir evenly to obtain a negative control sample, soak the sterile filter paper (d=6 mm) in the prepared sample solution for 5 minutes, and propose Place flat in a sterilized plate and dry at room temperature for later use.

Preparation of negative control sample 2

The sterilized filter paper sheet (d=6mm) was soaked in 10 ml of sterile distilled water, placed flat in a sterilized plate, and dried at room temperature for later use.

Test bacteria inoculation

Use a pipette to take 50 μl of the prepared bacterial suspension and place it on the corresponding medium plate, and spread it evenly on the inner surface of the medium plate with a coating rod 3 times, rotating 60 degrees each time, and finally wrap the coating rod around the plate. Coat the edges for a week and cover the dish. Paste the soaked filter paper sheets on the bacteria-containing plate at intervals, and gently press the samples with sterile tweezers to make them close to the surface of the plate. Place 6 sheets at equal intervals on each plate, and the distance between the centers of each antibacterial sheet should not be Less than 25mm, and at the same time, the distance from the edge of the medium plate is not less than 15mm. Three parallel experiments are carried out for each sample, cover the plate, seal the bottle with sealing film, and place it in a constant temperature incubator at 37 °C for 24 hours. Observe and record the inhibition. For the presence or absence of the bacterial circle, select a uniform and completely sterile growth inhibition ring, and use a vernier caliper to accurately measure its diameter and calculate the average value.

evaluation standard

If the diameter of the antibacterial ring is greater than 7mm, it is judged to have antibacterial effect, and if it is less than or equal to 7mm, it is judged to have no antibacterial effect; if the same repeated test three times have antibacterial effect, the result of the antibacterial test is valid.

The results show that the four sample toothpastes have bacteriostatic effect on Streptococcus mutans and Poromonas gingivalis. When the amount of functional substances added is the largest, the bacteriostatic effect is more obvious. Compared with sample toothpaste 4, it shows that adding glycyrrhizic acid can improve Its antibacterial performance, combined with the effect of efficacy substances on the toothpaste paste, finally screened the sample toothpaste 2 efficacy substances as the optimal formula ratio, specifically shown in Table 6, as follows:

Table 6 Antibacterial performance test of special toothpaste for middle-aged and elderly people

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the scope of the present invention. within the scope of protection.

Claims (10)

1. A kind of south medicine compound toothpaste that is effective for middle-aged and elderly people, it is characterized in that, comprises the following raw materials by weight:

   
2. The south medicine compound toothpaste specially effective for middle-aged and elderly people according to claim 1, characterized in that, the raw material also contains 0.05%-0.15% by weight of glycyrrhizic acid.
3. According to the middle-aged and old-aged special-effect south medicine compound toothpaste of claim 1, it is characterized in that, described friction agent is aluminum hydroxide and silicon dioxide.
4. The south medicine compound toothpaste specially effective for middle-aged and elderly people according to claim 3, wherein the particle size of the aluminum hydroxide is 2.6 μm and 11 μm.
5. The compound toothpaste for middle-aged and elderly people according to claim 4, wherein the mass ratio of 2.6 μm particle size aluminum hydroxide, 11 μm particle size aluminum hydroxide and silicon dioxide is 2:1:1.
6. The south medicine compound toothpaste specially effective for middle-aged and elderly people according to claim 1, is characterized in that, described essence comprises menthol and citron fruit oil, and the weight percentage of menthol in the raw material is 0.3%-0.6%, citron fruit The weight percentage of oil in the raw material is 0.1%-0.2%.
7. According to the middle-aged and elderly people's effective south medicine compound toothpaste according to claim 1, it is characterized in that, described Amomum chinensis is Hainan Amomum chinensis.
8. The south medicine compound toothpaste specially effective for middle-aged and elderly people according to claim 1, wherein the mass concentration of the sorbitol liquid is 70%.
9. The middle-aged and old-aged special-effect south medicine compound toothpaste according to claim 1, is characterized in that, is made by the raw material of following percentage by weight:

   
10. The preparation method of the middle-aged and old-aged compound toothpaste with special effect of Chinese medicine according to any one of claims 2 to 9, characterized in that, comprising the following steps:

    S1: Take galangal oil, Aina sesame oil, Amomum oil and red cardamom oil, set aside;

    S2: Take hydroxyapatite and sodium pyrophosphate, grind, sieve, and set aside;

    S3: Glue preparation: pre-disperse CMC-Na in propylene glycol to obtain propylene glycol glue, then add sorbitol solution and water, stir until uniform without transparent particles, stir for 20- 30min, pay attention to prevent water from evaporating during the stirring process. After the end, let it stand, and wait until the glue is fully swelled for use;

    S4: Preparation of paste: Weigh mud methyl methyl ester, sodium pyrophosphate, sodium saccharin, citric acid, and zinc citrate in proportion, add water for heating, fully stir and dissolve, add to the glue solution and stir evenly; then add the remaining Add the water that has been swollen in step S2 into the glue solution swollen in step S2, and when heated to 70-75 °C, first add foaming agent K12 and sodium lauroyl sarcosinate, stir evenly; then add friction agent and hydroxyapatite in turn, stir first After fully mixing with the glue, at a temperature of 70-75°C, keep stirring at 800-1000rpm for at least 20min, then adjust the speed to 500-700rpm and stir for at least 30min to obtain a toothpaste base;

    S5: When the temperature of the toothpaste paste base drops to 40-45°C, add galangal oil, Aina sesame oil, Amomum oil, cardamom oil, glycyrrhizic acid and essence in sequence, stir fully for at least 30min under the condition of rotating speed 500-600rpm, vacuum After degassing, let it stand to get the toothpaste.

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