CN113197830B

CN113197830B - Toothpaste and preparation method thereof

Info

Publication number: CN113197830B
Application number: CN202110474608.8A
Authority: CN
Inventors: 曹凤君
Original assignee: Dalian Wuyinfang Technology Co ltd
Current assignee: Heze Wuyinfang Biotechnology Group Co ltd
Priority date: 2021-04-29
Filing date: 2021-04-29
Publication date: 2022-06-14
Anticipated expiration: 2041-04-29
Also published as: CN113197830A

Abstract

The invention belongs to the technical field of daily necessities, and particularly relates to multifunctional toothpaste and a preparation method thereof. The multifunctional toothpaste comprises the following components: myrrh extract, Krameria triandra root extract, chamomile extract, propolis extract, gum mastic and lactobacillus peptide. The toothpaste has good effects of preventing dental caries and whitening teeth, and also has good effects of sterilizing, clearing pathogenic fire, and relieving inflammation.

Description

Toothpaste and preparation method thereof

Technical Field

The invention belongs to the technical field of daily necessities, and particularly relates to toothpaste and a preparation method thereof.

Background

Toothpaste is one of tooth cleaning products, generally in a gel shape, and is usually applied to a toothbrush, and the mechanical friction of the toothbrush is used for cleaning the surfaces of teeth, cleaning the teeth and the periphery of the teeth and purifying and refreshing the oral cavity. Tooth cleaning is of utmost importance for tooth aesthetics, protection of gum health and prevention of bad breath. Toothpaste has become a necessity in human daily life.

The toothpaste in the prior art is also diversified, for example, Chinese patent CN107115235A discloses a wormwood toothpaste, which comprises the following components: by mass percentage, 30-55% of an abrasive agent, 20-30% of a humectant, 1-3% of a surfactant, 1-3% of a thickening agent, 0.5-2% of a spice, 0.1-0.4% of a sweetener, 0-1% of a preservative and the balance of water; the preparation method of the wormwood toothpaste comprises the following steps: step one, preparing paste; step two, manufacturing a wormwood coating; and step three, filling. The scheme can prevent people from using the same medicinal toothpaste for a long time, and bacteria sensitive to the medicament are not easy to be inhibited for a long time to break the balance among floras.

For example, Chinese patent application CN107898695A, a preparation method of tea toothpaste, which comprises the following steps: crushing tea raw materials into tea powder of 100-500nm at low temperature to obtain nano tea powder; processing tea raw materials by a food oriented manufacturing technology to obtain a high-activity tea extract; processing the nano tea powder and/or the high-activity tea extract into nano tea particles by a microcapsule preparation technology; adding the nano tea particles into a toothpaste base material; and filling the uniformly stirred paste into a vertical pressing type package or other package forms to prepare the tea toothpaste product. The toothpaste has fresh and fine taste, and has effects of strengthening gum, protecting teeth, resisting inflammation, preventing oral bacteria breeding, etc., and especially greatly improves antibacterial effect of toothpaste.

Chinese patent application CN107412138A discloses a composition comprising sorbitol, calcium hydrogen phosphate, hydrated silica, deionized water, propylene glycol, sodium lauryl sulfate, brazilian green propolis, croscarmellose, essence, sodium pyrophosphate, saccharin sodium, carboxymethyl hydroxypropyl guar gum, methylparaben, paeonol, and cooling agent. The raw solution of Brazilian green propolis, green propolis water-soluble flavone, green beeswax and the like obtained by non-critical low-temperature extraction are mixed and emulsified according to a certain proportion and then added into the toothpaste base material, so that the toothpaste is an innovative toothpaste formula, can inhibit the growth and reproduction of pathogenic bacteria in the oral cavity, and has the effects of resisting inflammation, relieving swelling and pain, preventing gingival bleeding and swelling, and inhibiting inflammation such as oxidation-induced periodontal tissue ulcer and gall; the oral cavity health is guaranteed, and the effects of removing oral cavity peculiar smell, nourishing gum and protecting periodontal are achieved.

However, these toothpastes have a single efficacy and cannot meet the needs of different people. The invention aims to research a multifunctional toothpaste, and simultaneously satisfies the effects of whitening, sterilizing, diminishing inflammation and cleaning breath.

Disclosure of Invention

In order to overcome the technical problems, the invention provides the multifunctional toothpaste which has better effects of preventing decayed teeth and whitening teeth, and also has better effects of sterilizing, clearing heat and diminishing inflammation.

In order to realize the purpose, the technical scheme provided by the invention is as follows:

a multifunctional toothpaste comprises the following components: myrrh extract, Krameria triandra extract, chamomile extract, propolis extract, mastic gum, and lactobacillus peptide;

preferably, the multifunctional toothpaste further comprises the following components:

hydrated silica, sodium fluoride, pyridoxine HCL, tetrasodium pyrophosphate, polyethylene glycol-32, cellulose gum, glycerol, sodium lauryl sulfate, compound sweetener, compound flavoring agent, and water;

preferably, the components of the compound sweetener comprise: sodium benzoate, sorbitol, sodium saccharin and xylitol;

preferably, the composite sweetener comprises the following components in parts by weight: 0.1-0.5 part of sodium benzoate, 10-50 parts of sorbitol, 0.1-0.6 part of saccharin sodium and 0.1-0.8 part of xylitol;

preferably, the components of the composite fragrance comprise: menthol, clove leaf oil, and peppermint leaf oil.

Preferably, the composite flavoring agent comprises the following components in parts by weight: 0.01-0.01 part of menthol, 0.01-0.05 part of clove leaf oil and 0.01-0.05 part of mint leaf oil.

Preferably, the multifunctional toothpaste comprises the following components in parts by weight:

0.01-0.06 part of myrrh extract, 0.01-0.05 part of Peru tamania root extract, 0.01-0.10 part of chamomile extract, 0.01-0.08 part of propolis extract, 0.01-0.10 part of viscose mastic gum, 0.01-0.05 part of lactobacillus peptide, 10-20 parts of hydrated silica, 0.1 part of sodium fluoride, 0.1-0.5 part of pyridoxine HCL, 0.1-0.6 part of tetrasodium pyrophosphate, 320.1-0.6 part of polyethylene glycol, 0.1-0.8 part of cellulose gum, 0.1-0.5 part of glycerol, 0.1-0.6 part of sodium lauryl sulfate, 0.1-0.5 part of sodium benzoate, 10-50 parts of sorbitol, 0.1-0.6 part of saccharin sodium, 0.1-0.8 part of xylitol, 0.01-0.01 part of menthol, 0.01-0.05 part of clove leaf oil and 0.05-100 parts of water.

Preferably, the preparation method of the myrrh extract comprises the following steps:

a: reflux-extracting Myrrha with ethanol, collecting distillate, and making into ethanol extractive solution and residue;

b: drying the residue, adding water, and heating for extraction to obtain water extractive solution;

c: mixing the ethanol extractive solution and water extractive solution, adding petroleum ether, extracting, adding anhydrous sodium sulfate, dehydrating, and concentrating under reduced pressure to obtain Myrrha extract.

Preferably, in step A, the reflux extraction time is 1-2 h.

Preferably, in step B, the heating temperature is 40-60 ℃.

Preferably, in step B, the extraction time is 1-2 h.

Preferably, in the step B, an extracting agent is added in the extraction process, wherein the extracting agent is a mixture of acetic acid and sodium citrate, and the mass concentration of the acetic acid in water is 5-10%; the mass concentration of the sodium citrate water is 0.5-1%.

Preferably, the preparation method of the chamomile extract comprises the following steps:

s1: adding purified water into flos Matricariae Chamomillae, heating and extracting to obtain water extractive solution and residue;

s2: adding the residue into ethanol water solution, heating and extracting to obtain alcohol solution, and preparing alcohol extract;

s3: mixing the ethanol extractive solution and the water extractive solution, adsorbing with macroporous resin, eluting with ethyl acetate, eluting with ethanol water solution, collecting eluate, concentrating, and drying to obtain flos Matricariae Chamomillae extract.

Preferably, in step S1, the heating temperature is 70-80 deg.C, and the extraction time is 20-40 min.

Preferably, in step S2, the ethanol aqueous solution has a mass concentration of 75-95%.

Preferably, in step S3, the macroporous resin is D-101 or HPD-722.

Preferably, in the S3, the mass concentration of the ethanol aqueous solution is 30 to 45%.

The invention also aims to provide a preparation method of the multifunctional toothpaste, which comprises the following steps:

(1) taking purified water with the formula amount, adding tetrasodium pyrophosphate, polyethylene glycol-32 and sodium lauryl sulfate for dissolving, and then adding to prepare a solution 1;

(2) adding glycerol, flos Matricariae Chamomillae extract, Myrrha extract, Krameria triandra root extract, propolis extract, Olibanum gum, lactobacillus peptide, pyridoxine HCL, cellulose gum, sodium fluoride, compound sweetener, compound flavoring agent, and hydrated silica into solution 1, mixing, heating under stirring, vacuum degassing, and making into ointment.

Preferably, in the step (2), the heating temperature is 40-60 ℃.

Preferably, in the step (2), the rotation speed of the stirring is 1000-.

Compared with the prior art, the invention has the technical advantages that:

(1) the toothpaste provided by the invention has multiple effects, can better sterilize, diminish inflammation and refresh breath, and can also whiten teeth and prevent decayed teeth.

(2) The Krameria triandra root extract, the propolis extract, the myrrh extract and the chamomile extract in the toothpaste provided by the invention have good synergistic effect, and can effectively promote the whitening, anti-inflammation, internal heat-removing and sterilization effects of the toothpaste.

(3) The addition of acetic acid and sodium citrate during the preparation process of Myrrha extract is favorable for promoting the extraction of effective components of Myrrha, and enhancing its analgesic and anti-inflammatory effects.

(4) During the preparation process of the chamomile extract, D-101 or HPD-722 macroporous resin is used for extraction, and different solvents are used for elution, so that the extraction of effective components can be effectively improved, the purity of the effective components can be improved, and the effects of clearing heat, reducing internal heat and resisting dental caries can be favorably exerted.

Detailed Description

The present invention will be described below with reference to specific examples to make the technical aspects of the present invention easier to understand and grasp, but the present invention is not limited thereto. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.

Extract of Krameria triandra (Krameria triandra) or Krameria triandra (Krameria triandra, or the like: shenzhen, Rigilt Biotech, Inc.; viscose mastic gum: shanghai enzyme-linked Biotechnology, Inc.; cellulose gum: xianhao natural bioengineering, Inc.; propolis extract: xian jin Cuifang plant technology development Co., Ltd; chamomile extract: xian jin Cuifang plant technology development Co., Ltd.

Example 1

(1) The preparation method of the myrrh extract comprises the following steps:

a: adding 4 times of ethanol into myrrh, reflux-extracting for 1h, collecting fraction, and making into ethanol extract and residue;

b: drying the residue, adding 4 times of purified water by mass, and adding a mixture of acetic acid and sodium citrate, wherein the mass concentration of the acetic acid in the water is 5%; heating the sodium citrate water with the mass concentration of 0.5% to 60 ℃ for extraction for 2h to prepare water extract;

(2) The preparation method of the chamomile extract comprises the following steps:

s1: adding 3 times of purified water into flos Matricariae Chamomillae, heating to 80 deg.C, extracting for 20min to obtain water extractive solution and residue;

s2: adding the residue into an ethanol water solution with the mass concentration of 95% and the mass of 4 times of that of the residue, and heating and extracting to obtain an alcohol solution to obtain an alcohol extract;

s3: mixing the ethanol extract and the water extract, adsorbing with D-101 macroporous resin, eluting with ethyl acetate, eluting with 30% ethanol water solution, collecting eluate, concentrating, and drying to obtain flos Matricariae Chamomillae extract.

Example 2

(1) The preparation method of the myrrh extract comprises the following steps:

a: adding 6 times of ethanol into myrrh, reflux-extracting for 2h, collecting fraction, and making into ethanol extract and residue;

b: drying the residue, adding purified water 6 times the mass of the residue, and adding a mixture of acetic acid and sodium citrate, wherein the mass concentration of the acetic acid in the water is 10%; heating the sodium citrate water with the mass concentration of 1% to 40 ℃ for extraction for 1h to prepare water extract;

c: mixing the ethanol extractive solution and water extractive solution, adding petroleum ether for extraction, adding anhydrous sodium sulfate for dehydration, and concentrating under reduced pressure to obtain Myrrha extract.

s1: adding 5 times of purified water into flos Matricariae Chamomillae, heating to 70 deg.C, extracting for 40min to obtain water extractive solution and residue;

s2: adding the residue into ethanol aqueous solution with the mass concentration of 75% and the mass of 6 times of that of the residue, and heating and extracting to obtain an alcohol solution to obtain an alcohol extract;

s3: mixing the ethanol extractive solution and the water extractive solution, adsorbing with HPD-722 macroporous resin, eluting with ethyl acetate, eluting with 45% ethanol water solution, collecting eluate, concentrating, and drying to obtain flos Matricariae Chamomillae extract.

Example 3

A multifunctional toothpaste, its composition is as follows in Table 1:

table 1 example 3 formula of multifunctional toothpaste

The preparation method of the multifunctional toothpaste comprises the following steps:

(2) adding glycerol, flos Matricariae Chamomillae extract, Myrrha extract, Krameria triandra root extract, propolis extract, Olibanum gum, lactobacillus peptide, pyridoxine HCL, cellulose gum, sodium fluoride, compound sweetener, compound flavoring agent, and hydrated silica into solution 1, heating to 50 deg.C, stirring at 2000rpm, vacuum degassing, and making into ointment.

Example 4

A multifunctional toothpaste, its composition is as follows 2:

table 2 example 4 formula of multifunctional toothpaste

(2) adding glycerol, flos Matricariae Chamomillae extract, Myrrha extract, Krameria triandra root extract, propolis extract, Olibanum gum, lactobacillus peptide, pyridoxine HCL, cellulose gum, sodium fluoride, compound sweetener, compound flavoring agent, and hydrated silica into solution 1, heating to 60 deg.C, stirring at 3000rpm, vacuum degassing, and making into ointment.

Example 5

A multifunctional toothpaste, its composition is as follows 3:

table 3 example 5 formula of multifunctional toothpaste

(2) adding glycerol, flos Matricariae Chamomillae extract, Myrrha extract, Krameria triandra root extract, propolis extract, Olibanum gum, lactobacillus peptide, pyridoxine HCL, cellulose gum, sodium fluoride, compound sweetener, compound flavoring agent, and hydrated silica into solution 1, heating to 40 deg.C, stirring at 1000rpm, vacuum degassing, and making into ointment.

Comparative example 1

Compared with example 3, the difference is only the preparation method of the myrrh extract is different, and other operations are not changed.

The composition and formula of the multifunctional toothpaste are the same as those in example 3, and the preparation method of the multifunctional toothpaste is the same as that in example 3.

The preparation method of the myrrh extract comprises the following steps:

b: drying the residue, adding 4 times of purified water, heating to 60 deg.C, and extracting for 2 hr to obtain water extractive solution;

Comparative example 2

The preparation method of the myrrh extract comprises the following steps:

b: drying the residue, adding 4 times of purified water by mass, and adding acetic acid, wherein the mass concentration of the acetic acid in the water is 5%; heating to 60 deg.C, extracting for 2 hr to obtain water extractive solution;

Comparative example 3

Compared with example 3, the only difference is the preparation method of the chamomile extract, and other operations are not changed.

The preparation method of the chamomile extract comprises the following steps:

s1: adding 3 times of purified water, heating to 80 deg.C, extracting for 20min to obtain water extractive solution and residue;

s3: mixing the ethanol extractive solution and the water extractive solution, adsorbing with Diaion HP-20 macroporous resin, eluting with ethyl acetate, eluting with 30% ethanol water solution, collecting eluate, concentrating, and drying to obtain flos Matricariae Chamomillae extract.

Comparative example 4

Compared with example 3, the only difference is that propolis extract is replaced by chamomile extract with similar efficacy, and other operations are not changed.

Comparative example 5

The only difference compared to example 3 was that the viscose mastic gum was replaced with a similarly effective dipotassium glycyrrhizinate and the other operations were unchanged.

Examples of effects

1. Anti-inflammatory action

The experimental method comprises the following steps: the anti-inflammatory effect of the toothpaste is verified by adopting a xylene-induced mouse ear swelling experiment.

60 Kunming mice with the weight of 200 plus or minus 20 g; the test pieces were randomly divided into 10 groups of 6 pieces, each of which was a model group, a blank control group (physiological saline), examples 3 to 5, and comparative examples 1 to 5. Applying the medicine by smearing, wherein the dosage is 0.2ml/10g BW; wherein, the corresponding toothpaste is smeared in the examples 3-5, the model group does not need to be treated by the medicine, and the blank control group is smeared with the same amount of normal saline; 1 time every day, continuously for 5 days, smearing 50 μ L of xylene on front and back surfaces of left ear of mouse 30min after last administration, using right ear as control, removing neck of mouse after 2h, killing, cutting two ears along auricle base line, punching round ear piece at the same position with 9mm puncher, weighing, and taking difference between left and right ear pieces as swelling degree; the results of the experiment are shown in table 4 below:

TABLE 4 inhibition effect data sheet

Test group	Swelling degree (mg)
		Model set	21.3±3.1 a
Blank control group	19.7±1.9 a
		Example 3	11.8±2.5 b
Example 4	12.1±2.8 b
		Example 5	11.6±3.7 b
Comparative example 1	18.1±4.6 c
		Comparative example 2	16.3±2.8 c
Comparative example 3	14.9±5.6 c
		Comparative example 4	14.5±3.2 c
Comparative example 5	15.7±1.3 c

Remarking: in the same list, significant differences (p < 0.05) are indicated between different letters.

Therefore, the multifunctional toothpaste provided by the invention has a good anti-inflammatory effect, the components and the preparation method of the components have a great influence on the effect, and the components have a good synergistic effect.

2. Tooth whitening effect

The whitening effect of the toothpaste is evaluated by referring to an LSI (large scale integration) scoring method recorded in pages 5-6 of Shanghai-traffic university, 2009.

Selecting 90 patients meeting inclusion criteria and not belonging to exclusion criteria as study objects, wherein the age is 25-60 years. Subjects were evenly grouped by degree of tooth surface staining, gender and age. The test group was divided into 80 persons (examples 3 to 5 groups and comparative examples 1 to 5 groups, 10 persons each), and the control group was divided into 10 persons at random. The tested products were: the experimental group was the toothpaste products of the corresponding examples and comparative examples, and the control group was given a high-distillate full-effect toothpaste.

Subjects were evaluated clinically for stain index (LSI) at baseline and 8 weeks after product use using a Lobene Stain Index (LSI) scale score, with 0-3 scale for spot size and extent of stain as shown in table 5 below:

TABLE 5 LSI scoring method

Grading scoring	Size of color spot	Degree of color mottle
			0	Absence of colorless spots	Absence of colorless spots
1	1/3 for mottling up to tooth surface	Slight color spot (yellow or yellow brown)
			2	2/3 for mottling up to tooth surface	Moderate color spots (moderate brown)
3	2/3 color spot larger than tooth surface	Severe mottle (dark brown or black)

The index examines the upper anterior labial surface, the lower anterior labial surface, and the lingual surface. Each tooth surface is divided into a gum area and a tooth body area, and the teeth are respectively scored according to the area and the degree of the color spots. The score for each zone is the product of the area score and the degree score, each dentition score is the average of the dentition zone and gum zone scores, and each individual LSI score is the average of the individual dentition scores. And calculating the reduction rate = (LSI score after baseline-8 weeks)/baseline × 100%;

the test results are shown in Table 6:

TABLE 6 LSI values

Test group	Base line	LSI value after 8 weeks	Reduction rate%
				Control group	4.01±0.93	2.03±1.05	49.38
Example 3	3.97±1.01	1.22±1.22	69.27
				Example 4	4.05±1.55	1.18±1.36	70.86
Example 5	3.86±0.82	1.25±1.19	67.62
				Comparative example 1	4.03±1.67	1.93±0.67	52.11
Comparative example 2	3.80±1.22	1.57±1.05	58.68
				Comparative example 3	3.92±1.51	1.61±1.36	58.93
Comparative example 4	3.73±1.08	1.74±1.22	53.35
				Comparative example 5	3.91±1.46	1.49±1.13	61.89

Therefore, the multifunctional toothpaste provided by the invention has better effects of removing freckles and whitening teeth, and meanwhile, the components and the preparation method of the components have greater influence on the effects, and the components have better synergistic effect.

The above detailed description is directed to one of the possible embodiments of the present invention, which is not intended to limit the scope of the invention, but rather the scope of the invention is intended to include all equivalent implementations or modifications without departing from the scope of the invention.

Claims

1. The toothpaste is characterized by comprising the following components in parts by weight: 50 parts of water, 10 parts of hydrated silica, 0.1 part of sodium fluoride, 0.1 part of pyridoxine HCL, 0.1 part of tetrasodium pyrophosphate, 320.1 parts of polyethylene glycol-cellulose gum, 0.1 part of glycerol, 0.1 part of sodium lauryl sulfate, 0.01 part of myrrh extract, 0.01 part of Peru raney ni root extract, 0.01 part of chamomile extract, 0.01 part of propolis extract, 0.01 part of gum mastic, 0.01 part of lactic acid bacteria peptide, 10 parts of sorbitol, 0.1 part of sodium benzoate, 0.1 part of saccharin sodium, 0.1 part of xylitol, 0.01 part of menthol, 0.01 part of clove leaf oil and 0.01 part of mint leaf oil;

the preparation method of the myrrh extract comprises the following steps:

a: reflux-extracting Myrrha with ethanol, and collecting distillate to obtain ethanol extractive solution and residue;

c: mixing the ethanol extractive solution and water extractive solution, adding petroleum ether for extraction, adding anhydrous sodium sulfate for dehydration, and concentrating under reduced pressure to obtain Myrrha extract;

in the step B, an extracting agent is added in the extraction process, wherein the extracting agent is a mixture of acetic acid and sodium citrate, and the mass concentration of the acetic acid in water is 5-10%; the mass concentration of the sodium citrate in water is 0.5-1%.

2. The toothpaste is characterized by comprising the following components in parts by weight: 100 parts of water, 20 parts of hydrated silica, 0.5 part of sodium fluoride, 0.5 part of pyridoxine HCL, 0.6 part of tetrasodium pyrophosphate, 0.8978 parts of polyethylene glycol-320.6 parts of cellulose gum, 0.8 part of glycerol, 0.6 part of sodium lauryl sulfate, 0.06 part of myrrh extract, 0.05 part of Peru raney ni root extract, 0.1 part of chamomile extract, 0.08 part of propolis extract, 0.10 part of gum mastic, 0.05 part of lactic acid peptides, 50 parts of sorbitol, 0.5 part of sodium benzoate, 0.6 part of saccharin sodium, 0.8 part of xylitol, 0.01 part of menthol, 0.05 part of clove leaf oil and 0.05 part of mint leaf oil; the preparation method of the myrrh extract comprises the following steps:

3. The toothpaste of any one of claims 1-2, wherein said chamomile extract is prepared by a process comprising the steps of:

s2: adding the residue into ethanol water solution, and heating and extracting to obtain ethanol extract;

4. The toothpaste of claim 3, wherein in step S2, the aqueous ethanol solution has a mass concentration of 75-95%;

in step S3, the macroporous resin is D-101 or HPD-722;

in the S3, the mass concentration of the ethanol aqueous solution is 30-45%.

5. A process for preparing a toothpaste as claimed in any one of claims 1 to 4 comprising the steps of:

(1) taking water with the formula amount, adding tetrasodium pyrophosphate, polyethylene glycol-32 and sodium lauryl sulfate for dissolving to prepare a solution 1;

(2) adding glycerol, flos Matricariae Chamomillae extract, Myrrha extract, Krameria triandra root extract, propolis extract, Olibanum gum, lactobacillus peptide, pyridoxine HCL, cellulose gum, sodium fluoride, sodium benzoate, sorbitol, saccharin sodium, xylitol, menthol, clove leaf oil, peppermint leaf oil, and hydrated silica into solution 1, mixing, heating, stirring, vacuum degassing, and making into ointment.