CN110623911A

CN110623911A - Whitening toothpaste composition capable of effectively inhibiting growth of dental plaque and preparation method thereof

Info

Publication number: CN110623911A
Application number: CN201910902031.9A
Authority: CN
Inventors: 赵国盛
Original assignee: Zhejiang Ai Shang Daily Necessities Co Ltd
Current assignee: Zhejiang Ai Shang Daily Necessities Co Ltd
Priority date: 2019-09-17
Filing date: 2019-09-17
Publication date: 2019-12-31

Abstract

The invention discloses a whitening toothpaste composition capable of effectively inhibiting growth of dental plaque and a preparation method thereof. The whitening toothpaste composition is prepared from the following raw materials in percentage by weight: 10-20% of traditional Chinese medicine extracting solution, 20-30% of glycerol, 2-3% of lauroyl-N-methyl sodium aminoacetate, 30-40% of calcium hydrophosphate dihydrate, 10-20% of expanded perlite, 1-2% of sodium carboxymethylcellulose, 0.1-0.2% of saccharin, 0.5-1% of peppermint oil, 0.01-0.05% of vitamin E, 0.1-0.5% of sodium benzoate and 3-5% of purified water, wherein the sum of the weight percentages of the raw materials is equal to 100%; wherein the traditional Chinese medicine extracting solution is obtained by extracting dried buds of dried tangerine peel, pseudo-ginseng, asarum, gallnut and clove by an ultrasonic method. The whitening toothpaste has the obvious effect of inhibiting the growth of dental plaque, has obvious whitening effect and has wide application prospect.

Description

Whitening toothpaste composition capable of effectively inhibiting growth of dental plaque and preparation method thereof

Technical Field

The invention relates to a toothpaste composition and a preparation method thereof, in particular to a whitening toothpaste composition capable of effectively inhibiting the growth of dental plaque and a preparation method thereof. The invention belongs to the technical field of daily chemical articles.

Background

Residues of substances such as tobacco, tea, coffee, colored foods and the like in daily life are easy to deposit on tooth surfaces through saliva protein organic films on the surfaces of the teeth, if the teeth are not cleaned timely and effectively, the teeth can be gradually yellow or even black after long-time accumulation, exogenous stains and stains on the teeth are formed, and the oral hygiene and the tooth attractiveness are influenced.

People who have a white mouth tend to have healthy teeth that are more confident and smiling. In recent years, rapid tooth whitening techniques such as "tooth paste", "porcelain", "ultrasonic tooth washing", "plasma tooth bleaching" and the like have been developed and pursued by a few people. Despite their high cost and limited duration of effectiveness, these methods also pose varying levels of oral health risks, such as: the porcelain has great damage to the structure of the tooth, so that the texture of the tooth becomes fragile; most of the medicines used for tooth bleaching are peroxides, which have certain damage to teeth and oral soft tissues and possibly cause discomfort such as allergy.

At present, consumers have a strong demand for whitening teeth and have a high attention on whitening toothpaste. The whitening toothpaste is an oral care product aiming at exogenous staining of teeth, and can remove stains and stains on the surfaces of the teeth to a certain extent.

The traditional Chinese medicine is a treasure of Chinese nation, has rich resources, long history and huge development potential, and is widely concerned by scholars at home and abroad. At present, the traditional Chinese medicine tooth care mode is mainly to add the extract of the traditional Chinese medicine into oral care products such as toothpaste, mouthwash, chewing gum and the like.

The human mouth is filled with bacteria. Under conditions of moist heat, over 700 bacteria thrive in the oral cavity, including Streptococcus mutans (Streptococcus mutans), one of the major components of dental plaque. Streptococcus mutans adsorbs layer by layer on the teeth, forming a so-called "biofilm". They consume sugars, produce acids, attack the enamel layer of the teeth, and create cavities. Therefore, the key point of tooth whitening is to inhibit the growth of harmful bacteria such as Streptococcus mutans and prevent dental plaque formation, and currently, a plurality of traditional Chinese medicine toothpastes with antibacterial effects are available on the market, and the toothpastes can inhibit the growth of bacteria, but also inhibit the growth of other oral resident flora, such as Streptococcus salivarius (Streptococcus salivarius). Salivarius is the gram-positive coccus which can be regularly separated in human oral cavity, and the salivarius is found to prevent the formation of dental plaque and produce certain bacteriocin which has an inhibiting effect on bacteria related to oral malodor. Therefore, the ideal whitening medicinal toothpaste has good whitening effect and good bacteriostatic effect, does not generate drug resistance, and does not inhibit the growth of beneficial flora in the oral cavity.

Disclosure of Invention

The invention aims to provide whitening toothpaste capable of effectively inhibiting growth of dental plaque and a preparation method thereof. The whitening toothpaste provided by the invention can inhibit the growth of harmful bacteria in the oral cavity, prevent and treat dental plaque formation, and can maintain the flora balance of the oral cavity to the maximum extent.

In order to achieve the purpose, the invention adopts the following technical means:

the invention relates to a whitening toothpaste composition capable of effectively inhibiting growth of dental plaque, which comprises the following raw materials in percentage by weight: 10-20% of traditional Chinese medicine extracting solution, 20-30% of glycerol, 2-3% of lauroyl-N-methyl sodium aminoacetate, 30-40% of calcium hydrophosphate dihydrate, 10-20% of expanded perlite, 1-2% of sodium carboxymethylcellulose, 0.1-0.2% of saccharin, 0.5-1% of peppermint oil, 0.01-0.05% of vitamin E, 0.1-0.5% of sodium benzoate and 3-5% of purified water, wherein the sum of the weight percentages of the raw materials is equal to 100%;

the traditional Chinese medicine extracting solution is prepared by the following method:

placing 5-15 parts by weight of dried orange peel, 10-15 parts by weight of pseudo-ginseng, 5-15 parts by weight of asarum, 1-5 parts by weight of gallnut and 5-10 parts by weight of dry clove buds in an ultrasonic instrument, adding 70 w/w% ethanol solution according to the proportion of 1: 8-10, covering a cover, soaking for 20-30 minutes, then starting the ultrasonic instrument for 30-60 minutes, removing dregs of a decoction to obtain a traditional Chinese medicine extracting solution, and placing the traditional Chinese medicine extracting solution in a reduced pressure distiller to evaporate ethanol to obtain the traditional Chinese medicine extracting solution.

Preferably, the whitening toothpaste composition comprises the following raw materials in percentage by weight: 15% of traditional Chinese medicine extracting solution, 25% of glycerol, 3% of lauroyl-N-methyl sodium glycinate, 35% of calcium hydrophosphate dihydrate, 15% of expanded perlite, 1.25% of sodium carboxymethyl cellulose, 0.2% of saccharin, 1% of peppermint oil, 0.05% of vitamin E, 0.5% of sodium benzoate and 4% of purified water;

placing 5 parts by weight of dried orange peel, 15 parts by weight of pseudo-ginseng, 10 parts by weight of asarum, 7 parts by weight of gallnut and 3 parts by weight of dry bud of clove in an ultrasonic instrument, adding 70 w/w% ethanol solution according to the proportion of 1: 10, covering a cover, soaking for 30 minutes, then opening the ultrasonic instrument for 40 minutes, removing dregs of a decoction to obtain a traditional Chinese medicine extracting solution, and placing the traditional Chinese medicine extracting solution in a reduced pressure distiller to evaporate ethanol to obtain the traditional Chinese medicine extracting solution. Further, the invention also provides a method for preparing whitening toothpaste capable of effectively inhibiting the growth of dental plaque, and the whitening toothpaste is prepared by the following steps:

(1) weighing the raw materials according to the weight percentage;

(2) uniformly mixing the weighed traditional Chinese medicine extracting solution with purified water, then adding sodium carboxymethylcellulose, standing overnight, and dissolving the sodium carboxymethylcellulose after completely swelling;

(3) adding glycerol, peppermint oil, vitamin E, lauroyl-N-methyl sodium aminoacetate, saccharin and sodium benzoate into the solution obtained in the step (2), stirring to dissolve the mixture, adding calcium hydrophosphate dihydrate and expanded perlite, stirring for 24 hours in a stirrer to uniformly mix to obtain a paste with certain viscosity and proper thickness, and filling and packaging after quality inspection is qualified.

Furthermore, the invention also provides application of the whitening toothpaste composition in preparing the whitening toothpaste capable of effectively inhibiting the growth of dental plaque.

Compared with the prior art, the invention has the beneficial effects that:

1. the whitening toothpaste contains traditional Chinese medicine extract components, and the traditional Chinese medicine extract is obtained by extracting dried buds of dried tangerine peel, pseudo-ginseng, asarum, gallnut and clove by an ultrasonic extraction method. According to the invention, dried buds of dried tangerine peel, pseudo-ginseng, asarum, gallnut and clove are selected for compounding after multiple screening tests, on one hand, the compounded composition can generate a synergistic effect of inhibiting Streptococcus mutans (Streptococcus mutans), on the other hand, the screened traditional Chinese medicine extract has no significant inhibiting effect on Streptococcus salivarius (Streptococcus salivarius), and the flora balance of the oral cavity can be maintained to the maximum extent;

2. the invention adopts an ultrasonic extraction method to extract the traditional Chinese medicine, and improves the extraction rate and the extraction efficiency of the effective components of the traditional Chinese medicine because the ultrasonic waves have mechanical vibration performance and strong cavitation effect.

3. The invention adopts calcium hydrogen phosphate dihydrate and expanded perlite as an abrasive, and the calcium hydrogen phosphate dihydrate is the most common mild excellent abrasive, has affinity with the tooth enamel and has moderate friction on the tooth enamel. The use of the expanded perlite is helpful for improving the cleaning effect of the toothpaste, has better polishing effect, can polish the concave-convex surface caused by stains or fine tartar on the surface of the tooth, achieves the purpose of polishing and whitening, can reduce the abrasion of the toothpaste on the tooth, and does not damage enamel. The two can be used together to clean teeth without damaging enamel.

Detailed Description

The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.

Example 1 preparation of a whitening toothpaste effective in inhibiting the growth of dental plaque

(1) Preparation of Chinese medicinal extractive solution

Placing 10 parts by weight of dried orange peel, 15 parts by weight of pseudo-ginseng, 10 parts by weight of asarum, 3 parts by weight of gallnut and 5 parts by weight of dry bud of clove in an ultrasonic instrument, adding 70 w/w% ethanol solution according to the proportion of 1: 10, covering a cover, soaking for 30 minutes, then opening the ultrasonic instrument for 40 minutes, removing dregs of a decoction to obtain a traditional Chinese medicine extracting solution, and placing the traditional Chinese medicine extracting solution in a reduced pressure distiller to evaporate ethanol to obtain the traditional Chinese medicine extracting solution.

(2) Weighing the raw materials according to the following weight percentage;

15% of traditional Chinese medicine extracting solution, 25% of glycerol, 3% of lauroyl-N-methyl sodium glycinate, 35% of calcium hydrophosphate dihydrate, 15% of expanded perlite, 1.25% of sodium carboxymethyl cellulose, 0.2% of saccharin, 1% of peppermint oil, 0.05% of vitamin E, 0.5% of sodium benzoate and 4% of purified water;

(3) uniformly mixing the weighed traditional Chinese medicine extracting solution with purified water, then adding sodium carboxymethylcellulose, standing overnight, and dissolving the sodium carboxymethylcellulose after completely swelling;

(4) and (3) adding glycerol, peppermint oil, vitamin E, lauroyl-N-methyl sodium glycinate, saccharin and sodium benzoate into the solution obtained in the step (3), stirring to dissolve the mixture, adding calcium hydrophosphate dihydrate and expanded perlite, and stirring for 24 hours in a stirrer until the mixture is uniformly mixed to obtain a proper paste with certain viscosity and thickness.

(5) Quality detection

And (4) detecting the product quality according to the national standard of GB/T8372 and 2017 toothpaste, wherein the obtained product is qualified in quality. See tables 1 and 2.

TABLE 1 hygiene indicators for toothpaste products

Detecting items	Results
		Total number of colonies (CFU/g)	＜100
Total number of mold and yeast (CFU/g)	＜80
		Heat-resistant coliform group (g)	Not detected out
Pseudomonas aeruginosa (g)	Not detected out
		Staphylococcus aureus (g)	Not detected out
Lead content (mg/kg)	＜0.01
		Arsenic content (mg/kg)	＜0.01

TABLE 2 sensory, physicochemical indices of the toothpaste products

Experimental example 1 screening test of Chinese medicine effective in inhibiting growth of dental plaque

1. Preparation of dry powder of Chinese medicinal extract

The invention relates to a method for preparing a safe traditional Chinese medicine capable of inhibiting oral bacterial proliferation, which is prepared by primarily screening a plurality of traditional Chinese medicines with bactericidal effects, wherein the traditional Chinese medicines with bactericidal effects reported in the field comprise: rhubarb, pseudo-ginseng, scutellaria, gallnut, dried orange peel, angelica dahurica, ligusticum wallichii, asarum, clove, divaricate saposhnikovia root, cortex lycii radicis, rehmannia, lotus leaf, scandent hop, honeysuckle flower and the like. Extracting the traditional Chinese medicines respectively according to the ultrasonic extraction method described in the embodiment 1 to obtain traditional Chinese medicine extracting solution, and performing spray drying to obtain dry powder of the traditional Chinese medicine extracting solution for later use.

2. Preparation of plate containing bacteria

The test bacteria are Streptococcus mutans (ATCC 25923), Staphylococcus aureus (ATCC6538), Candida albicans (ATCC 76615), and Streptococcus salivarius (ATCC 19258).

Respectively culturing the above test bacteria, diluting with sterile normal saline to obtain test bacteria suspension with bacteria content of 1 × 10⁸cfu/ml. Respectively mixing 1ml of each bacterial suspension, 0.2ml of calf serum and 15ml of melted beef soup culture medium, making into plate containing bacteria, and condensing for use. Candida albicans was plated on sandcastle medium.

3. Bacteriostasis test

Qualitative filter paper is taken and made into 6mm diameter circular slices, and pressure steam sterilization is carried out. Then diluting the dry powder of the Chinese medicinal extract with medical normal saline respectively to obtain different concentrations (1: 10, 1: 50, 1: 100, 1: 200, 1: 400, 1: 800, 1: 1600, 1: 3200, 1: 6400). And (3) sticking filter paper sheets on the surface of the prepared bacteria-containing culture medium, wherein the distance between the paper sheets and the edges of the flat plates is 15mm, and 4-6 filter paper sheets are stuck on each flat plate. Accurately taking 10 μ l of 10 dilutions of Chinese medicinal extractive solution, and sequentially adding into each filter paper sheet. And (3) culturing the plate after adding the medicine at 37 ℃ for 24h, culturing the candida albicans plate at 37 ℃ for 48h, and accurately measuring the diameter of the bacteriostatic ring, wherein the dilution multiple corresponding to the diameter of the bacteriostatic ring being less than 7mm is considered as the minimum bacteriostatic concentration. The results are shown in table 3 below:

TABLE 3 minimum inhibitory concentration of Chinese medicinal extract

From the results, the extracts of the rhubarb, the pseudo-ginseng, the Chinese gall, the dried orange peel, the asarum, the divaricate saposhnikovia root, the cortex lycii radicis, the rehmannia root and the humulus scandens have a strong inhibiting function on streptococcus mutans, but the extracts of the rhubarb, the scutellaria baicalensis, the Chinese gall, the cortex lycii radicis and the rehmannia root and the humulus scandens also have a strong inhibiting function on streptococcus salivarius, and the extracts of the pseudo-ginseng, the dried orange peel and the asarum have a weak inhibiting function on streptococcus salivarius, so that the three traditional Chinese medicines are preliminarily screened out to serve as traditional Chinese medicine. In comprehensive consideration, clove has weak effect on streptococcus mutans, but has weaker effect on streptococcus salivarius and stronger inhibitory effect on staphylococcus aureus, so the clove is further selected as a traditional Chinese medicine component. Gallnut and cortex lycii radicis also have strong inhibiting effect on streptococcus salivarius but have strong inhibiting effect on streptococcus mutans, so the two medicines are taken as candidate medicines to carry out compound research on the medicines.

4. Bacteriostasis test of compound traditional Chinese medicine composition

1) Preparation of compound traditional Chinese medicine extract dry powder

Preparing a compound traditional Chinese medicine extract 1: placing 10 parts by weight of dried orange peel, 15 parts by weight of pseudo-ginseng, 10 parts by weight of asarum, 3 parts by weight of gallnut and 5 parts by weight of dry clove buds in an ultrasonic instrument, adding 70 w/w% ethanol solution according to the proportion of 1: 10, covering a cover, soaking for 30 minutes, then opening the ultrasonic instrument for 40 minutes, removing dregs of a decoction to obtain a traditional Chinese medicine extracting solution, placing the traditional Chinese medicine extracting solution in a reduced pressure distiller to evaporate ethanol to obtain a traditional Chinese medicine extracting solution 1, and performing spray drying to obtain dry powder of the traditional Chinese medicine extracting solution for later use.

Preparing a compound traditional Chinese medicine extract 2: placing 10 parts by weight of dried orange peel, 15 parts by weight of pseudo-ginseng, 10 parts by weight of asarum, 3 parts by weight of cortex lycii radicis and 5 parts by weight of dry clove buds in an ultrasonic instrument, adding 70 w/w% ethanol solution according to the proportion of 1: 10, covering a cover, soaking for 30 minutes, then opening the ultrasonic instrument for 40 minutes, removing dregs of a decoction to obtain a traditional Chinese medicine extracting solution, placing the traditional Chinese medicine extracting solution in a reduced pressure distiller to evaporate ethanol to obtain a traditional Chinese medicine extracting solution 2, and performing spray drying to obtain dry powder of the traditional Chinese medicine extracting solution for later use.

2) Bacteriostasis test

The bacteriostatic test was carried out according to the above method, and the results are shown in table 4:

table 4 minimum inhibitory concentration of compound traditional Chinese medicine extract

From the results in table 4, it can be seen that the inhibition effect of the compound traditional Chinese medicine extract 1 on streptococcus salivarius is lower than that of the traditional Chinese medicine extract 2, which is probably because the inhibition effect of gallnut on streptococcus salivarius is reduced by the compound traditional Chinese medicine composition, and in addition, the inhibition effect of the compound traditional Chinese medicine extract 1 on candida albicans is enhanced, which indicates that the compound traditional Chinese medicines can generate a synergistic effect.

Experimental example 2 Effect test for removing extrinsic stain from teeth

1. Test sample

Test sample 1: whitening toothpaste 1 (prepared according to example 1)

Test sample 2: whitening toothpaste 2 (prepared according to example 1, but without traditional Chinese medicine extract, the corresponding part is replaced by purified water)

Test sample 3: whitening toothpaste 3 (prepared according to example 1, but using dibasic calcium phosphate dihydrate as abrasive)

Test sample 4: whitening toothpaste 4 (commercially available)

2. Test method

The international commission on illumination (CIE) L a b standard colorimetric system is currently the most commonly used colorimetric system in oral colorimetry. In this system, L denotes lightness (also called brightness), and a and b denote hue and chroma. The value of L is 0-100, the smaller value is close to black, and the larger value is close to white. The change in L x can be used to evaluate the whitening effect of a toothpaste on removing extrinsic stains from teeth.

Taking a bovine enamel block, and carrying out embedding, polishing, cleaning, acid etching and dyeing treatment to simulate the surface of teeth which can be damaged to a certain extent and form color spots in daily life. Color of enamel was measured by a colorimeter_{Before brushing teeth}) And selecting the dentin blocks with the baseline L-value of 35-45, randomly distributing the dentin blocks to the test groups, brushing and grinding 8 blocks in each group by using the toothpaste in the test groups respectively, taking out the enamel sample from the tooth brushing machine after tooth brushing is finished, washing the enamel sample with water, and airing the enamel sample. The color L of enamel after brushing was measured.

3. Test results

The change of enamel color L (difference Δ L) before and after brushing was calculated, and the larger the Δ L value, the higher the whitening degree and the better the whitening effect. The results are shown in Table 5.

TABLE 5 Change in enamel color L-mean before and after brushing

Experimental example 3 plaque removal test

1 test drugs and groups

Test sample 1: whitening toothpaste 1 (prepared according to example 1)

Test sample 4: whitening toothpaste 4 (commercially available)

2. Study objects and groups

80 volunteers with dental plaque were selected, aged 18-50 years. 40 male cases and 40 female cases. Voluntarily participate in the study, and only use the blank nursing products provided by the study; antibiotics and hormones are not taken within 3 months; there is no systemic disease. The subjects were randomly divided into 4 groups (20 per group), and each group was brushed with a whitening toothpaste in the morning and evening each day. The subjects in group 4 required a uniform toothbrush, each time using toothpaste for a length of time to cover the brush head for 2min each time for 1 month.

3. Inspection standard

Each subject examined 6 teeth sites (16, 21, 24, 36, 41, 44), 4 sites per tooth examination: the plaque index (PLI) was recorded on the mesial, median, distal buccal and mesial lingual sides, respectively, and averaged as the clinical index for the index.

4. Results

After 30 days, the plaque index of 4 groups of patients tested is shown in table 6.

Table 6 plaque index comparison

Group of	Base line	30 days	Rate of decrease
				Test sample 1 group	1.75±0.25	0.84±0.25	52％
Test sample 2 group	1.78±1.23	1.25±2.35	29.78％
				Test sample 3 groups	1.69±2.56	1.02±1.65	39.64％
Test sample 4 groups	1.72±1.56	1.58±2.41	8.14％

As can be seen from the above results, the whitening toothpaste (whitening toothpaste 1) of the present invention has the best plaque removal effect.

Claims

1. The whitening toothpaste composition capable of effectively inhibiting the growth of dental plaque is characterized by comprising the following raw materials in percentage by weight: 10-20% of traditional Chinese medicine extracting solution, 20-30% of glycerol, 2-3% of lauroyl-N-methyl sodium aminoacetate, 30-40% of calcium hydrophosphate dihydrate, 10-20% of expanded perlite, 1-2% of sodium carboxymethylcellulose, 0.1-0.2% of saccharin, 0.5-1% of peppermint oil, 0.01-0.05% of vitamin E, 0.1-0.5% of sodium benzoate and 3-5% of purified water, wherein the sum of the weight percentages of the raw materials is equal to 100%;

2. The whitening toothpaste composition according to claim 1, wherein the whitening toothpaste composition comprises the following raw materials in percentage by weight: 15% of traditional Chinese medicine extracting solution, 25% of glycerol, 3% of lauroyl-N-methyl sodium glycinate, 35% of calcium hydrophosphate dihydrate, 15% of expanded perlite, 1.25% of sodium carboxymethyl cellulose, 0.2% of saccharin, 1% of peppermint oil, 0.05% of vitamin E, 0.5% of sodium benzoate and 4% of purified water;

3. A method for preparing whitening toothpaste capable of effectively inhibiting growth of dental plaque is characterized by comprising the following steps:

(1) weighing the raw materials according to the weight percentage of the raw materials in the claim 1 or 2;

4. Use of the whitening toothpaste composition of claim 1 or 2 for the preparation of a whitening toothpaste effective for inhibiting the growth of dental plaque.