CN112870115B

CN112870115B - Special-effect south medicine compound toothpaste for middle-aged and elderly people and preparation method thereof

Info

Publication number: CN112870115B
Application number: CN202110210055.5A
Authority: CN
Inventors: 谢小丽; 陈振夏; 官玲亮; 于福来; 胡璇; 王凯; 黄梅
Original assignee: Tropical Crops Genetic Resources Institute CATAS
Current assignee: Tropical Crops Genetic Resources Institute CATAS
Priority date: 2021-02-25
Filing date: 2021-02-25
Publication date: 2023-04-14
Anticipated expiration: 2041-02-25
Also published as: WO2022179254A1; CN112870115A

Abstract

The invention discloses a special south medicine compound toothpaste for middle-aged and elderly people and a preparation method thereof, belonging to the technical field of toothpaste processing. Aiming at the characteristics of the oral cavity of middle-aged and old people, the invention discovers that the toothpaste added with the volatile oil of the four south medicines of galangal, amomum villosum, galangal and blumea balsamifera has better antibacterial and anti-inflammatory effects through a plurality of experimental screens, and solves the problems that the stability of the paste is poor due to high dosage required when a single Chinese herbal medicine is used, or the usability of the paste is influenced due to heavy pungent smell or medicinal taste, and the compound glycyrrhizic acid, citric acid and zinc citrate are used as compound functional substances to enhance the antibacterial performance and desensitizing effect of the toothpaste. The special south medicine compound toothpaste for the middle-aged and the elderly does not damage dentin, has good cleanliness, is antibacterial, anti-inflammatory, antiallergic, fresh and comfortable, is suitable for the characteristics of easy tooth allergy, high bacterial caries rate, and common periodontitis and periodontitis of the middle-aged and the elderly, is clean and fine, has moderate foam, is easy to extrude, has good stability, and is easy to popularize and apply.

Description

Special-effect south medicine compound toothpaste for middle-aged and elderly people and preparation method thereof

Technical Field

The invention belongs to the technical field of toothpaste processing, and particularly relates to special south medicine compound toothpaste for middle-aged and elderly people and a preparation method thereof.

Background

The oral diseases of middle-aged and old people are different from those of young people, the incidence rate is high, the third national oral health epidemiological investigation result shows that the prevalence rate of dental caries of middle-aged and old people in China is respectively up to 88.1 percent and 98.4 percent, the prevalence rate of periodontal health is respectively 14.5 percent and 14.1 percent, and the oral diseases are important public health problems threatening the health of middle-aged and old people in China. Because the middle-aged and old people gradually age due to the change of physiological aging, all tissues of the body gradually age, the organ functions gradually decline, the change of the oral cavity is also subjected to the natural development process, various oral diseases, particularly teeth, are easy to occur, the enamel on the tooth surface is greatly abraded due to the abrasion of the chewing for decades, the dentin is easy to be allergic, and because of the reasons of easy food retention in the mouth, exposure of gingiva and the like, the middle-aged and old people have a plurality of cariogenic bacteria, the periodontal diseases such as gingivitis, periodontitis and the like are common, the heart disease, the stomach disease, diabetes, cardiovascular disease, joint diseases and complications can be seriously caused or aggravated, and the whole body health is seriously damaged. The toothpaste is an oral hygiene product containing various components, can remove food residues remained between teeth and dirt attached to the surfaces of teeth, plays a role in cleaning the oral cavity, and has certain effects on preventing bacterial infection and reducing oral diseases because a proper amount of medicines are added into the paste.

At present, when a single Chinese herbal medicine is used in toothpaste in China, the required dosage is generally higher, the stability of the toothpaste is often poor, or the usability of the toothpaste is influenced because of heavy pungent smell or medicinal taste, therefore, two or more medicines are generally adopted to form compound toothpaste, the curative effect of the toothpaste is improved, but most of the Chinese herbal medicine toothpaste is added with an extracting solution or an extract, the color is darker, the toothpaste is not easily accepted by consumers, and the effect can be achieved only by adding a large amount of effective components, so that the stability of the toothpaste is influenced. In addition, the traditional Chinese herbal medicine compound toothpaste aiming at the oral problems of the middle-aged and the elderly in the market is less, so that the toothpaste which does not damage dentin, has the effects of bacteriostasis, inflammation diminishing and dentin hypersensitivity resistance and does not influence the basic performance and the sensory effect of the toothpaste is developed, and the problem to be solved is urgently solved.

Disclosure of Invention

In view of the defects of the prior art, the invention aims to solve the problems, the invention provides the special south medicine compound toothpaste for the middle-aged and the elderly, the south medicine Chinese herbal medicines which can be used for oral hygiene products are screened according to the oral characteristics of the middle-aged and the elderly, the south medicine used by the invention is added with the essential oil of the main active component, the color of the paste is not influenced, and the problem that the sensory effect of the toothpaste is influenced due to the high dosage of the single Chinese herbal medicine is solved, and the toothpaste can inhibit bacteria, diminish inflammation and resist dentin hypersensitivity by matching the glycyrrhizic acid, the citric acid and the zinc citrate as the compound effective substances. In addition, the invention also finds that aluminum hydroxide with different grain diameters is matched with silicon dioxide to be used as a toothpaste abrasive, so that the dentin is not damaged, and finally, the mint and citron fruit oil are added, so that the bad smell of the Chinese herbal medicine is covered, and the toothpaste is fresh and comfortable.

The scheme of the invention comprises the following aspects:

on one hand, the invention provides special south medicine compound toothpaste for middle-aged and elderly people, which comprises the following raw materials in percentage by weight:

preferably, the raw materials also contain 0.05 to 0.15 weight percent of glycyrrhizic acid.

Preferably, the abrasive is aluminum hydroxide and silica.

Preferably, the particle size of the aluminum hydroxide is 2.6 μm and 11 μm. Wherein the mass ratio of the 2.6 μm-diameter aluminum hydroxide to the 11 μm-diameter aluminum hydroxide to the silica is 2. Two kinds of aluminum hydroxide with different grain diameters are selected to match with silicon dioxide, and the abrasive material toothpaste which does not damage dentin is prepared according to a certain proportion, has stable chemical property, does not react with functional substances in the toothpaste, and has optimal intermiscibility.

Preferably, the essence comprises 0.3-0.6 wt% of menthol and 0.1-0.2 wt% of citron fruit oil. The menthol has strong permeation promoting effect, so that the toothpaste has the effects of refreshing taste and breath; the citron is a traditional Chinese medicine with homology of medicine and food, and the volatile oil has faint scent, can be used as an odor inhibitor, can make people comfortable and can also enhance the bacteriostatic performance.

Preferably, the fructus amomi is amomi Hainan.

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

Preferably, the special south medicine compound toothpaste for the middle-aged and the elderly is prepared from the following raw materials in percentage by weight:

in the formula of the raw materials, volatile oil of south medicine galangal, hainan villous amomum fruit, galangal and blumea balsamifera is compounded according to a certain proportion to play roles of bacteriostasis, inflammation diminishing and penetration promotion. The south medicine, the glycyrrhizic acid, the citric acid and the zinc citrate are matched and cooperated, so that the antibacterial and anti-inflammatory performance and the anti-allergic performance of the toothpaste are enhanced. Desensitizing agents citric acid and zinc citrate are added, and polyhydric alcohols (sorbitol and propylene glycol) are used as moisture retention agents, so that the citric acid anions can be promoted to permeate into dentin, and the effectiveness of the desensitizing agents is enhanced. The added volatile oil can influence the emulsification of the paste to a certain extent, and sodium pyrophosphate in the formula is used as a stabilizer to prevent the oil phase from being separated out of the paste. The added hydroxyapatite is an induction factor of bones or teeth, has better remineralization, desensitization and whitening to teeth and promotion of gingivitis healing in the field of oral health care, has better prevention and treatment effects on caries and periodontal diseases, and plays an auxiliary role. The added foaming agent is the combination of sodium dodecyl sulfate and sodium lauroyl sarcosinate, which not only can increase the fineness and fullness of the toothpaste foam, but also can further prevent the oil phase from separating out from the toothpaste body. The added sweetening agents are saccharin sodium and glycyrrhizic acid, the glycyrrhizic acid can be used as a sweetening agent besides being used as an effective substance in the formula, the sweetness of the sweetening agent is 200 times that of cane sugar, the using amount of the sweetening agent can be reduced in the formula, and the bitterness and the astringency of the effective substance can be covered.

On the other hand, the invention also provides a preparation method of the special south medicine compound toothpaste for the middle-aged and the elderly, which comprises the following steps:

s1: collecting rhizoma Alpiniae Officinarum oil, oleum Blumeae Balsamiferae, oleum Ormosiae Hosiei and fructus Galangae oil;

s2: grinding and sieving hydroxyapatite and sodium pyrophosphate for later use;

s3: preparing glue: pre-dispersing CMC-Na in propylene glycol to obtain propylene glycol glue, adding sorbitol solution and water, stirring until no transparent particles exist, stirring for 20-30min at 70-75 ℃ and 700-1000rpm, preventing water evaporation during stirring, standing after the water evaporation is finished, and fully swelling the glue solution for later use;

s4: preparing paste: weighing methyl paraben, sodium pyrophosphate, sodium saccharin, citric acid and zinc citrate according to a certain proportion, adding water, heating, fully stirring for dissolving, adding into the glue solution, and uniformly stirring; adding water into the glue solution swelled in the step S2, heating to 70-75 ℃, adding a foaming agent, and uniformly stirring; sequentially adding the friction agent and the hydroxyapatite, stirring and fully mixing with the glue solution, fully stirring at the temperature of 70-75 ℃ for at least 20min at the rotating speed of 800-1000rpm, adjusting the rotating speed to 500-700rpm, and stirring for at least 30min to obtain a toothpaste base;

s5: cooling the toothpaste base to 40-45 deg.C, sequentially adding rhizoma Alpiniae Officinarum oil, blumea balsamifera oil, oleum Amomi rotundus, fructus Galangae oil, glycyrrhizic acid and essence, stirring at 500-600rpm for at least 30min, vacuum degassing, and standing to obtain toothpaste.

The invention has the following beneficial effects:

(1) The invention adopts aluminum hydroxide (2.6 um) and aluminum hydroxide (11 um) matched with different micron-sized abrasive agents of silicon dioxide to prepare the dentin-free abrasive according to a certain proportion, and is suitable for the characteristics of severe tooth abrasion of the middle-aged and the elderly people.

(2) The invention adopts the volatile oil of four south medicines of galangal, hainan villous amomum fruit, galangal and blumea balsamifera to carry out compounding, plays the roles of bacteriostasis, inflammation diminishing and penetration promotion in toothpaste, and is suitable for the characteristics of high bacterial caries rate of middle-aged and old people, common periodontal diseases such as gingivitis, periodontitis and the like.

(3) The four south medicines are matched and cooperated with the glycyrrhizic acid, the citric acid and the zinc citrate, so that the antibacterial property and the antiallergic property of the toothpaste are improved, and the toothpaste is suitable for the characteristic that teeth of middle-aged and elderly people are allergic easily.

(4) The invention also adds hydroxyapatite as an adjuvant, enhances the effects of desensitization, reducing dental plaque in the oral cavity and promoting gingivitis healing, and can also be used as a tooth mineralization repairing agent.

(5) The toothpaste flavor type adopted by the invention is obtained by screening various essences, and the unexpected discovery that the menthol flavor and the citron fruit oil can not only cover the unpleasant odor of the drug effect substance, but also enable the toothpaste to achieve the effects of freshness and comfort.

(6) The special south medicine compound toothpaste for the middle-aged and the elderly does not damage dentin, has good cleanliness, and has the effects of bacteriostasis, inflammation diminishing, antianaphylaxis, freshness and comfort, thereby achieving the effect of preventing and treating the oral diseases of the middle-aged and the elderly.

Drawings

FIG. 1: the invention relates to a preparation process flow chart of toothpaste;

FIG. 2 is a schematic diagram: a toothpaste object graph; in the figure, (A) is a toothpaste base; (B) is the best horizontal group sample toothpaste; and (C) is the optimal level group sample toothpaste.

Detailed Description

In order that the technical contents of the invention may be better understood, specific examples are provided below to further illustrate the invention.

The raw materials of the galangal, the Hainan villous amomum fruit, the galangal and the citron fruit are collected from south medicine germplasm resource gardens of the research institute of tropical crop variety resources of the Chinese tropical agricultural academy of sciences;

the blumea balsamifera branches and leaves are collected from blumea balsamifera germplasm resource gardens of research institute of tropical crop variety resources of Chinese tropical academy of agricultural sciences;

other toothpaste accessories are purchased through on-line or off-line shops according to the quality requirements.

Example 1 preparation Process optimization experiment of toothpaste of the present application

1.1 screening of functional substances

According to the antibacterial property of volatile oil of galangal, amomum Hainan, galangal and blumea balsamifera, the volatile oil of the four south medicines is taken as a monarch medicine, glycyrrhizic acid is taken as an auxiliary medicine to enhance the antibacterial property, and according to the characteristic that the oral cavity of middle-aged and elderly people is easy to be allergic, citric acid and zinc citrate are taken as desensitizers, and hydroxyapatite is taken as a tooth mineralization repairing agent.

1.2 toothpaste base ingredient screening

The middle-aged and elderly people teeth are used for decades, the enamel on the surface is basically worn out, so that the raw material with low friction coefficient and no damage to the enamel is used for selecting the abrasive; the aluminum hydroxide has stable performance, strong tooth cleaning capability and no damage to tooth enameling, can improve the water separation phenomenon of toothpaste, and the silicon dioxide is a flexible abrasive, has stable chemical property, does not react with south medicine in the toothpaste, has better intermiscibility, has a structure of round cellular polymeric particles full of small gaps, has large contact area with tooth surface dirt, has different particle sizes, can clean teeth and does not damage tooth enameling, so that aluminum hydroxide and silicon dioxide with different micron sizes are selected as the abrasive according to the tooth characteristics of middle-aged and elderly people, and the aluminum hydroxide with the particle size of 2.6 mu m is used as the main abrasive. Because the functional substance selects citric acid and zinc citrate as desensitizers and uses polyalcohol as a moisturizing agent, the citric acid anions can be promoted to permeate into dentin, and the effectiveness of the desensitizers is enhanced, thus sorbitol and propylene glycol are selected as humectants; the adhesive agent is sodium carboxymethyl cellulose; the added essential oil can influence the emulsification of the paste to a certain extent, and sodium pyrophosphate in the formula is used as a stabilizer to prevent the oil phase from being separated out of the paste. The foaming agent is selected from sodium dodecyl sulfate and sodium lauroyl sarcosinate, so that the fineness and fullness of toothpaste foam can be improved, and the separation of an efficacy substance oil phase from the paste body can be further avoided. The sweetener is saccharin sodium, and because glycyrrhizic acid in the effective substances has high sweetness, the sweetener can also be used as the sweetener; through multiple preliminary experiments, the fact that the menthol fragrance and the citron fruit oil can not only cover up the pungent and astringent taste of the functional substance, but also enable the toothpaste to achieve the refreshing and refreshing effect is unexpectedly found, and the components of the toothpaste are obtained through screening, wherein the components are shown in table 1.

TABLE 1 toothpaste ingredient Table

1.3 toothpaste formulation process

S1: respectively taking dried rhizome of galangal, dried branches and leaves of blumea balsamifera, hainan amomum fruit and galangal fruit according to a certain amount, crushing the dried rhizome of galangal, dried branches and leaves of blumea balsamifera, dried fruits of galangal and dried fruits of galangal fruit in the shade to 40 meshes by a crusher, adding distilled water with the mass of 8-10 times of the powder, soaking the powder for 2 hours, then carrying out steam distillation extraction for 3 times, wherein the extraction time is 4 hours, 3 hours and 2 hours respectively, combining the volatile oil obtained in the three times, and respectively obtaining galangal oil, blumea balsamifera oil, hainan amomum oil and galangal oil for later use.

S2: grinding hydroxyapatite and sodium pyrophosphate into ultrafine powder, and sieving with a 150-mesh sieve;

s3: preparing glue: pre-dispersing CMC-Na in propylene glycol to obtain propylene glycol glue, adding 70% sorbitol solution and a small amount of water into a beaker, stirring until no transparent particles exist, stirring for 20-30min at the temperature of 70-75 ℃ and the rotation speed of 700-1000rpm, preventing water evaporation in the stirring process, standing for about 12h after the water evaporation is finished, and fully swelling the glue solution for later use.

S4: preparing paste: weighing methyl paraben, sodium pyrophosphate, sodium saccharin, citric acid and zinc citrate according to a certain proportion, putting into a beaker, adding water for heating, fully stirring until the sodium paraben, the sodium pyrophosphate, the sodium saccharin, the citric acid and the zinc citrate are completely dissolved, adding into a glue solution, and uniformly stirring; adding the rest deionized water into the swollen glue solution, heating to 70-75 ℃, adding a foaming agent, and stirring uniformly, wherein the foaming agent can play a defoaming role in the adding process, so that a large amount of foam is reduced in the stirring process; sequentially adding the friction agents and the hydroxyapatite with different particle sizes (the addition plays a role in defoaming again), fully mixing the mixture with the glue solution by manual stirring, fully stirring the mixture for 20min at the temperature of between 70 and 75 ℃ at the rotating speed of between 800 and 1000rpm, adjusting the rotating speed to between 500 and 700rpm, and stirring the mixture for 30min again to fully stir the mixture uniformly to obtain a toothpaste base;

s5: cooling to 40-45 deg.C, sequentially adding effective substances including rhizoma Alpiniae Officinarum oil, blumea balsamifera oil, hainan oleum Amomi, fructus Galangae oil, glycyrrhizic acid and essence, stirring at 500-600rpm for 30min, vacuum degassing, standing for 24 hr, and making into toothpaste.

1.3.2 sensory evaluation

The sensory index is the most intuitive index for evaluating the toothpaste quality, and according to the requirements of the new national standard of toothpaste on the toothpaste, the sensory evaluation is carried out by adopting a 5-grade 100-grade evaluation method, wherein the evaluation method comprises the following steps:

(1) Forming conditions are as follows: the prepared paste is put into a decorating bag, the decorating bag is cut into a caliber with the size of a toothpaste tube opening, the toothpaste is extruded out of the decorating bag on filter paper which is easy to absorb water, and the toothpaste is extruded out with slight force, if the extrusion force is large, the paste is not easy to extrude, the toothpaste is too thick, otherwise, the paste is too thin, the thickness is moderate, and the wire drawing is obvious; whether the extruded paste is easily cut or not.

(2) Paste form: extruding two strips of toothpaste and placing on black paper, and observing whether the paste is clean, uniform and fine, whether the moisture is separated, and whether the color is normal or whether impurities exist; whether the whole body collapses downwards or not; the paste is left for a period of time and is not dried quickly. A groove of 0.5-1 cm is scribed on the surface of one paste body by a pin, whether the shape of the groove is kept unchanged in proper time is observed, and if the groove is normal, the paste body is normal.

(3) The mouthfeel is as follows: the toothpaste samples tested each time are distributed to 10 fixed middle-aged and elderly people for trial, and the standards are followed to grade according to whether the mouth feel is fresh and comfortable, whether the cool degree is moderate, whether the spicy and bitter taste appears, whether the fresh and fragrant taste is moderate or not and whether the mouth feel is moderate or not.

(4) And (3) water seepage phenomenon is observed: the toothpaste is placed on the rough-edged paper, and is uniformly spread by fingers, and the reverse side of the paper is seen to have no water seepage, so that the toothpaste with good quality has little water seepage;

(5) See the presence or absence of overly hard particles: smearing a little toothpaste on a carrier, spreading with fingers, pressing, cleaning, observing whether there is scratch on the glass, and scratching teeth during brushing teeth;

(6) Measurement of foam amount: weighing 45 ℃ and 20ml of water in advance, weighing 1g of toothpaste to be measured into a beaker, adding a small amount of water to dissolve the paste, pouring the dissolved paste into a measuring cylinder with a plug, cleaning the beaker with the residual water, pouring into the measuring cylinder, covering a bottle plug, pressing the bottle plug, shaking the solution in the measuring cylinder uniformly with the maximum force, stopping after the paste is completely dissolved by visual observation, placing the measuring cylinder on an operation table, standing for 5min, and recording the foaming amount by taking the position where the foam distribution of the measuring cylinder is most concentrated by visual observation as the standard.

TABLE 2 sensory evaluation criteria

1.3.3 toothpaste formula dosage determination

In the above toothpaste components, effective substances, frictionThe amounts of abrasive aluminium hydroxide (2.6 um) aluminium hydroxide (11 um) silicon dioxide =2 um, 1, the addition ratio of 70% sorbitol solution of humectant to propylene glycol is 2.5 ₁₈ (3 ⁷ ) Orthogonal experimental design, and screening the optimal formula process according to the sensory scores. Hydroxyapatite, methyl paraben and sodium pyrophosphate have small influence on the sensory evaluation of the whole toothpaste body, and can be respectively added into the formula according to the proportion of 1.5-2.5%, 0.1-0.2% and 0.2-0.5%. In the test, 2% of hydroxyapatite, 0.15% of methyl p-hydroxybenzoate and 0.3% of sodium pyrophosphate are added, and the toothpaste is prepared by adopting a 1.3 toothpaste formula processing technology in each formula for sensory evaluation. The results are as follows:

TABLE 3 orthogonal factors horizon

TABLE 4 orthogonal experimental protocols and results

Experiment number	A	B	C	D	E	F	G	Sensory scoring
									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 value 1	85.050	84.833	85.550	84.033	84.917	84.350	86.650
Mean value 2	86.567	85.983	86.933	87.650	86.883	88.600	86.683
									Mean value 3	85.550	86.350	84.683	85.483	85.367	86.217	83.833
Extreme difference	1.517	1.517	2.250	3.617	1.966	2.250	2.850

The test results show that the influence of all factors on the sense of the toothpaste is D > G > C = F > E > A = B, namely the dosage of the foaming agent has the greatest influence on the toothpaste body, and essence, adhesive and saccharin sodium are used as the second components. The optimal composition is A according to visual analysis ₂ B ₃ C ₂ D ₂ E ₂ F ₂ G ₂ Namely 40 percent of an abrasive agent, 35 percent of a humectant, 1.5 percent of an adhesive agent, 2.5 percent of a foaming agent, 2.08 percent of an effective substance, 0.2 percent of saccharin sodium and 0.55 percent of essence. As can be seen from the analysis of variance, each factor A has no significance on the effect of toothpaste.

1.3.4 validation experiments

In order to examine the reproducibility of the optimum test, the experiment was conducted by finding the best horizontal combination from the tests conducted and comparing the best horizontal combination with the optimum combination obtained by data analysis. The best level found by sensory scoring for this example was combined as experiment No. 15, i.e. a ₂ B ₃ C ₁ D ₂ E ₃ F ₂ G ₁ Combined with the optimum level found by range analysis A ₂ B ₃ C ₂ D ₂ E ₂ F ₂ G ₂ And (4) performing a comparison experiment so as to further judge whether the found production process conditions are optimal, wherein the result is as follows, and the optimal level group is superior to the best level group in taste.

Table 5 verifies the test results

1.3.5 stability test

The stability test refers to the stability test method in toothpaste (GB/T8372-2017). Taking 2 samples of the optimal level group of sample toothpaste and the optimal level group of toothpaste respectively, storing the 2 samples at room temperature, putting the other 2 samples into a refrigerator at minus 8 +/-1 ℃, taking out after 8 hours, immediately putting into a constant temperature incubator at 45 +/-1 ℃, taking out after 8 hours, recovering the room temperature, opening the cover, and preventing the paste from overflowing out of the tube opening; inverting the toothpaste tube body, and dripping no liquid from the tube orifice within 10 s; the paste after extrusion has normal flavor and color compared with the sample stored at room temperature.

Example 2 detection of bacteriostatic Properties of Compound efficacy toothpaste

2.1 test materials and introduction

Strain: streptococcus mutans standard strain (Streptococcus mutans, SM), ATCC25175; standard strain of Porphyromonas Gingivalis (PG), ATCC33277; the strains are all provided by molecular biological laboratories of Biotech, inc., chengdu. The streptococcus mutans is one of streptococcus with the largest oral cavity proportion and is a main pathogenic bacterium for gum and tooth diseases; porphyromonas gingivalis is a main pathogenic bacterium for chronic and invasive periodontitis, gingival abscess and periodontal infection, so that the bacteriostatic properties of the two bacteria are mainly detected.

Culture medium: rabbit blood brain heart extract Broth (BHI) culture medium (Shanghai Yuan leaf Biotech Co., ltd.), and anaerobic liver soup (Beijing Soilebao Tech Co., ltd.).

Blank toothpaste (without adding functional substance and flavor type), sample toothpaste 1 (functional substance 1.1%), sample toothpaste 2 (functional substance 2.08%), sample toothpaste 3 (functional substance 2.8%), and sample toothpaste 4 (functional substance does not contain glycyrrhizic acid, and other materials are in the same proportion as sample toothpaste 2)

3.2 test methods

Preparing bacterial liquid: inoculating 50 μ L of standard strains of Streptococcus mutans and Porphyromonas gingivalis, respectively, into BHI culture medium, streaking to form single colony, placing the inoculated plate in anaerobic tank (80%N2, 10% H2, 10%) CO2) 3d activation by incubation. Then selecting a flat plate bacterial colony, inoculating the flat plate bacterial colony into anaerobic pork liver soup for culturing for 72 hours, and measuring the bacterial liquid concentration OD by using an ultraviolet spectrophotometer ₆₀₀ Is between 0.5 and 1.0.

Preparing a bacteriostatic sample: weighing 3.0g of four kinds of toothpaste samples, adding 10ml of deionized water, stirring uniformly to obtain sample solutions, soaking sterilized filter paper sheets (d =6 mm) in the prepared sample solutions for 5min, extracting, horizontally placing in a sterilized plate, and drying at room temperature for later use to obtain sample toothpaste 1, sample toothpaste 2, sample toothpaste 3 and sample toothpaste 4.

Preparation of negative control sample 1

Weighing 3.0g of blank (without adding functional substances and flavor type) toothpaste, adding 10ml of deionized water, stirring uniformly to obtain a negative control sample, soaking a sterilized filter paper sheet (d =6 mm) in the prepared sample solution for 5min, putting the sterilized filter paper sheet in a sterilized flat dish, and drying the sterilized filter paper sheet at room temperature for later use.

Preparation of negative control sample 2

A sterilized filter paper sheet (d =6 mm) was soaked in 10ml of sterile distilled water, pulled out and laid flat in a sterilized dish, and dried from room temperature for use.

Inoculation of test bacteria

Taking 50 mul of prepared bacterial suspension by using a pipette, respectively placing the prepared bacterial suspension on corresponding culture medium flat plates, uniformly coating the inner surfaces of the culture medium flat plates for 3 times by using a coating rod, rotating for 60 degrees every time of coating, finally coating the coating rod for a circle around the edges of the flat plates, and covering the flat plates. Sticking the soaked filter paper sheets on a flat plate containing bacteria at intervals, slightly pressing sample sheets by using sterile forceps to enable the filter paper sheets to be tightly attached to the surface of the flat plate, placing 6 sheets on each flat plate at equal intervals, wherein the distance between the centers of the bacteriostatic sheets is not less than 25mm, and the distance between the centers of the bacteriostatic sheets and the edge of a culture medium flat plate is not less than 15mm, performing 3 parallel experiments on each sample, covering the flat plate, sealing a bottle by using a sealing film, placing the flat plate in a constant-temperature incubator at 37 ℃ for culturing for 24 hours, observing and recording the existence of a bacteriostatic ring, selecting a uniform and completely sterile growth bacteriostatic ring, accurately measuring the diameter of the bacteriostatic ring by using a vernier caliper, and calculating an average value.

Evaluation criteria

The diameter of the antibacterial ring is more than 7mm, and the antibacterial ring is judged to have antibacterial effect, and the diameter of the antibacterial ring is less than or equal to 7mm, and the antibacterial ring is judged not to have antibacterial effect; the results of the bacteriostatic test are valid for the patients who have bacteriostatic action in the same repeated test for 3 times.

The results show that the four kinds of sample toothpaste have antibacterial effects on streptococcus mutans and porphyromonas gingivalis, wherein when the adding amount of the functional substances is the largest, the antibacterial effect is more obvious, and the antibacterial effect is compared with that of the sample toothpaste 4, which shows that the antibacterial performance of the toothpaste can be improved by adding glycyrrhizic acid, and finally the functional substances of the sample toothpaste 2 are screened as the optimal formula ratio by combining the influence of the functional substances, specifically shown in table 6 and as follows:

TABLE 6 detection of antibacterial property of special toothpaste for middle-aged and elderly people

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims

1. The special south medicine compound toothpaste for the middle-aged and the elderly is characterized by comprising the following raw materials in percentage by weight:

the preparation method of the south medicine compound toothpaste special for the middle-aged and the elderly comprises the following steps:

s2: grinding and sieving hydroxyapatite and sodium pyrophosphate for later use;

s3: preparing glue: pre-dispersing CMC-Na in propylene glycol to obtain propylene glycol glue, adding sorbitol solution and water, stirring until no transparent particles exist, stirring for 20-30min at 70-75 deg.C and 700-1000rpm, keeping the temperature at 70-75 deg.C while preventing water evaporation, standing, and swelling the glue solution;

s4: preparing paste: weighing methyl paraben, sodium pyrophosphate, sodium saccharin, citric acid and zinc citrate according to a certain proportion, adding water, heating, fully stirring for dissolving, adding into the glue solution, and uniformly stirring; adding the rest water into the glue solution swelled in the step S2, heating to 70-75 ℃, adding a foaming agent K12 and sodium lauroyl sarcosinate, and uniformly stirring; sequentially adding the friction agent and the hydroxyapatite, stirring and fully mixing with the glue solution, fully stirring at the temperature of 70-75 ℃ at the rotating speed of 800-1000rpm for at least 20min, adjusting the rotating speed to 500-700rpm, and stirring for at least 30min to obtain a toothpaste base;

s5: when the temperature of the toothpaste base is reduced to 40-45 ℃, galangal oil, blumea balsamifera oil, amomum oil, galangal oil, glycyrrhizic acid, menthol and citron fruit oil are sequentially added, fully stirred for at least 30min at the rotating speed of 500-600rpm, and then the toothpaste is obtained after vacuum degassing and standing.

2. The special south medicine compound toothpaste according to claim 1, wherein the abrasive is aluminum hydroxide and silicon dioxide.

3. The special south medicine compound toothpaste for the middle-aged and the elderly according to claim 2, wherein the particle size of the aluminum hydroxide is 2.6 μm and 11 μm.

4. The special south medicine compound toothpaste for the middle-aged and the elderly, according to claim 3, is characterized in that the mass ratio of 2.6 μm particle size aluminum hydroxide, 11 μm particle size aluminum hydroxide and silicon dioxide is 2.

5. The special south medicine compound toothpaste for the middle-aged and the elderly as claimed in claim 1, wherein the fructus amomi is amomi Hainan.

6. The special south medicine compound toothpaste for the middle-aged and the elderly as claimed in claim 1, wherein the mass concentration of the sorbitol solution is 70%.

7. The special south medicine compound toothpaste for the middle-aged and the elderly as claimed in claim 1, which is characterized by being prepared from the following raw materials by weight percent:

/>