CN111700835A - Toothpaste containing snow lotus herb and preparation method thereof - Google Patents
Toothpaste containing snow lotus herb and preparation method thereof Download PDFInfo
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- CN111700835A CN111700835A CN202010711987.3A CN202010711987A CN111700835A CN 111700835 A CN111700835 A CN 111700835A CN 202010711987 A CN202010711987 A CN 202010711987A CN 111700835 A CN111700835 A CN 111700835A
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
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- A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
- A61K8/463—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
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Abstract
The invention belongs to the technical field of oral cleaning products, and particularly relates to toothpaste containing snow lotus herb components and a preparation method thereof. The toothpaste containing the snow lotus herb component is prepared from zinc citrate, titanium dioxide, a wetting agent, an abrasive, sodium lauryl sulfate, calcium bicarbonate, a thickening agent, sodium benzoate, trichlorogalactose, sodium phytate, snow lotus herb extract, essence and water. The toothpaste containing the snow lotus herb component has good functions of cleaning, resisting bacteria, diminishing inflammation and easing pain, and can promote remineralization of enamel surfaces and enhance cariostatic capability of enamel. In addition, the preparation method of the toothpaste containing the snow lotus herb component provided by the invention is simple in process, low in cost and easy to realize industrial production.
Description
Technical Field
The invention belongs to the technical field of oral cleaning products, and particularly relates to toothpaste containing snow lotus herb components and a preparation method thereof.
Background
Toothpaste is a common cleaning product in daily life and has a long history. With the development of science and technology, the improvement and perfection of technological equipment, various types of toothpaste are brought out in succession, the quality and the grade of products are improved continuously, the variety of the existing toothpaste is developed into toothpaste with complete variety and multiple functions from single clean toothpaste, and the requirements of consumption levels of different levels are met.
With the increasing demand of people on toothpaste, the demand of people on toothpaste not only meets the requirement of cleaning the oral cavity, but also needs the toothpaste to treat and care the oral cavity problems such as oral cavity care, gingival bleeding, periodontitis and the like. Gingival bleeding is a common inflammatory condition and is generally prone to bleeding when brushing teeth, sucking and chewing hard objects. The pathogenesis of most cases of gingivitis is caused by local factors, gingival bleeding and edema are mainly caused by plaque, calculus or impaction stimulation of things on the neck of a tooth, if the treatment is not timely and thoroughly carried out, inflammation of gingival tissues can be developed into periodontitis under the action of factors inside and outside a body, so that the progressive damage to tooth parenchyma is caused, finally, teeth are loosened and fall off, and the harm to the health of the oral cavity and the whole body of a human is great.
Patent publication No. CN111388393AA discloses an antibacterial toothpaste containing bamboo mushroom triterpene and a preparation method thereof, and the components of the antibacterial toothpaste comprise bamboo mushroom triterpene, a solubilizer, an abrasive, pyrophosphate, a thickening agent, an anticarious agent, a foaming agent and the like. The toothpaste prepared by the formula has certain sterilization and anti-inflammation effects, but the treatment effect is poor, the foaming agent is sodium lauryl sulfate, and the abrasive is hydrated silica. Sodium lauryl sulfate is liable to cause rupture of oral mucosa, which leads to failure of self-healing, and then induces and aggravates oral ulcer. Hydrated silica is prone to problems with tooth sensitivity, gum bleeding, root exposure, etc. In addition, the toothpaste has single efficacy and cannot meet the use requirements of the public on the toothpaste.
In conclusion, the prior art has the technical defects of poor treatment effect, single effect, damage to gums and oral mucosa and the like in tooth maintenance and nursing.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a toothpaste containing snow lotus herb components and a preparation method thereof. The toothpaste containing the snow lotus herb component has good functions of cleaning, resisting bacteria, diminishing inflammation and easing pain, can promote remineralization of enamel surfaces, enhances the cariostatic capability of enamel, and helps supplement zinc element.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a toothpaste containing snow lotus herb comprises the following components in parts by weight:
10-18 parts of zinc citrate, 6-15 parts of titanium dioxide, 15-30 parts of wetting agent, 25-40 parts of friction agent, 2-3 parts of sodium lauryl sulfate, 1-3 parts of calcium bicarbonate, 5-15 parts of thickening agent, 5-20 parts of sodium benzoate, 10-15 parts of trichlorogalactose, 10-25 parts of sodium phytate, 15-30 parts of snow lotus herb extract, 1-1.5 parts of essence and 15-20 parts of water.
Further, the toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
Furthermore, the humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 3-5: 10-13: 9-15.
Furthermore, the abrasive in the toothpaste containing the snow lotus herb component consists of hydrated silica and hydroxyapatite according to the mass ratio of 5: 7.
Furthermore, the thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to a mass ratio of 9-15: 4-7: 3-9.
Further, the preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component comprises the following steps:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, extracting for 0.5h each time, filtering, and drying filter residues to prepare degreased snow lotus powder;
(3) adding the degreased saussurea involucrate powder prepared in the step (2) into a flask, adding 75% ethanol solution by mass, performing reflux extraction for 5 times, extracting for 1 hour each time, filtering, and combining filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 45-60 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation to obtain a supernatant.
Furthermore, in the preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component, in the step (2), the adding mass ratio of the snow lotus herb powder to the petroleum ether is 1: 7-10; the reflux extraction temperature is 60-90 ℃; the drying temperature is 90-110 ℃.
Furthermore, in the preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component, in the step (3), the adding mass ratio of the degreased snow lotus powder to the ethanol solution is 1: 12-17; the reflux extraction temperature is 60-75 ℃; in the step (5), the centrifugal speed is 4000rpm, and the centrifugal time is 15 min.
The invention also provides a preparation method of the toothpaste containing the snow lotus herb component, which comprises the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotating speed of 400-600 rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, pumping until the vacuum degree in the tank is-0.085 to-0.090 Mpa, and filling to obtain the toothpaste.
The abrasive in the toothpaste containing the snow lotus herb component consists of hydroxyapatite and hydrated silica, so that the problems of tooth sensitivity, gingival bleeding, tooth root exposure and the like caused by a large amount of hydrated silica are avoided. The hydroxyapatite has the functions of adsorbing protein, amino acid, lipid and glucan, promoting remineralization of enamel surface and enhancing anticarious ability of enamel. Meanwhile, the hydroxyapatite has good biocompatibility with the alveolar bone, can promote the repair of the defective alveolar bone and effectively prevent the alveolar bone from absorbing and shrinking. Snow lotus belongs to precious medicinal flower garden plants, has the functions of removing cold phlegm, tonifying yang, enriching blood, warming uterus and dissipating blood stasis, and also has obvious effects on lumbago caused by kidney deficiency, rheumatism removal, and meridian passage dredging. In addition, snow lotus herb has an anti-inflammatory effect, like an acute inflammation relieving effect. The beneficial substances in the snow lotus herb extract can stimulate adrenal cortical hormone to secrete substances capable of reducing swelling, thereby having the effects of resisting inflammation and easing pain.
The sodium benzoate in the formula can inhibit yeast and bacteria in the toothpaste, thereby achieving the purpose of killing the bacteria all the time. The benzoic acid is firstly dissociated from the sodium benzoate, and the benzoic acid is easy to permeate cell membranes to enter cells due to higher lipophilicity, so that the permeability of the cell membranes of microorganisms such as mould and bacteria is disturbed, and the absorption of the cell membranes to amino acid is inhibited. The benzoic acid molecules entering the cells ionize and acidify the alkali storage in the cells, can inhibit the activity of a respiratory enzyme system of the cells, has a strong effect of preventing acetyl coenzyme A condensation and reaction, and can control the growth of various microorganisms in a long time period, thereby playing a role of antisepsis. The addition of the trichlorogalactose can increase the antibacterial performance of the toothpaste, and the trichlorogalactose has no irritation to the skin, no mucosal irritation and no carcinogenic risk. The sodium phytate has good oxidation resistance, and is safe and nontoxic. Sodium phytate has high affinity with enamel surface, and can affect adsorption and desorption of stain, protein and pigment on enamel surface, prevent pigmentation, and help to remove pigment and dental calculus. Meanwhile, the sodium benzoate, the trichlorogalactose and the sodium phytate have the anti-inflammatory and bacteriostatic effects, so that the problem that the sodium lauryl sulfate is easy to cause oral mucosa rupture and further induce and aggravate oral ulcer can be effectively solved, and the snow lotus herb extract is matched with the snow lotus herb extract to play a certain inhibiting effect on gum sensitivity, redness and swelling, labor pain and the like.
In addition, the wetting agent consisting of sorbitol, glycerol and soybean lecithin in a certain ratio in the formula is uniformly dispersed in a toothpaste system under the action of the thickening agent consisting of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose, so that the toothpaste has better enzyme resistance and thermal stability, and excellent hydration capability can be provided. In addition, tetrasodium pyrophosphate can be added into toothpaste to be used as tartar control agent, and can combine calcium ions and magnesium ions to prevent the calcium ions and the magnesium ions from depositing on the surface of teeth, thereby achieving the aim of cleaning the teeth. The zinc citrate can also effectively prevent the formation of tartar and keep teeth white.
Compared with the prior art, the toothpaste containing the snow lotus herb component and the preparation method thereof provided by the invention have the following advantages:
(1) the toothpaste containing the snow lotus herb component has good effects of diminishing inflammation and relieving pain, can thoroughly clean teeth and relieve tooth sensitivity;
(2) the toothpaste containing the snow lotus herb component can help to supplement zinc element while cleaning teeth, inhibit the growth of oral microorganisms and has a good using effect;
(3) the preparation method of the toothpaste containing the snow lotus herb component provided by the invention is simple in process, low in cost and easy to realize industrial production.
Detailed Description
The present invention will be further described below by way of specific embodiments, but the present invention is not limited to only the following examples. Various modifications can be made by those skilled in the art based on the basic idea of the invention, but it is within the scope of the invention as long as it does not depart from the basic idea of the invention.
In the embodiment, the abrasive in the toothpaste containing the snow lotus herb component consists of hydrated silica and hydroxyapatite according to the mass ratio of 5: 7.
Example 1A toothpaste containing snow lotus herb ingredient
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 10 parts of zinc citrate, 6 parts of titanium dioxide, 15 parts of wetting agent, 25 parts of abrasive, 2 parts of sodium lauryl sulfate, 1 part of calcium bicarbonate, 5 parts of thickening agent, 5 parts of sodium benzoate, 10 parts of trichlorogalactose, 10 parts of sodium phytate, 15 parts of snow lotus herb extract, 1 part of essence and 15 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 3:10: 9.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 9:4: 3.
The preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component comprises the following steps:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, wherein each extraction time is 0.5h, and the adding mass ratio of the snow lotus pollen to the petroleum ether is 1: 7; the reflux extraction temperature is 60 ℃; filtering and drying the filter residue at the drying temperature of 90 ℃ to obtain degreased snow lotus powder;
(3) adding the degreased snow lotus powder prepared in the step (2) into a flask, adding the degreased snow lotus powder and an ethanol solution according to the mass ratio of 1:12, adding the ethanol solution with the mass fraction of 75% to perform reflux extraction for 5 times, wherein the reflux extraction temperature is 60 ℃, filtering, and combining the filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 45 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation at the centrifugal rotation speed of 4000rpm for 15min to prepare a supernatant, thus obtaining the high-purity liquid.
The invention also provides a preparation method of the toothpaste containing the snow lotus herb component, which comprises the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotating speed of 400rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, pumping until the vacuum degree in the tank is-0.085 Mpa, and filling to obtain the toothpaste.
Example 2A toothpaste containing snow lotus herb ingredient
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 12 parts of zinc citrate, 7 parts of titanium dioxide, 18 parts of wetting agent, 30 parts of abrasive, 2.4 parts of sodium lauryl sulfate, 1.5 parts of calcium bicarbonate, 8 parts of thickening agent, 10 parts of sodium benzoate, 11 parts of trichlorogalactose, 15 parts of sodium phytate, 20 parts of snow lotus herb extract, 1.2 parts of essence and 17 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 3:11: 10.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 9:5: 8.
The preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component comprises the following steps:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, wherein each extraction time is 0.5h, and the adding mass ratio of the snow lotus pollen to the petroleum ether is 1: 8; the reflux extraction temperature is 65 ℃; filtering and drying the filter residue at 100 ℃ to obtain defatted snow lotus powder;
(3) adding the degreased snow lotus powder prepared in the step (2) into a flask, adding the degreased snow lotus powder and an ethanol solution according to the mass ratio of 1:14, adding the ethanol solution with the mass fraction of 75% to perform reflux extraction for 5 times, wherein the reflux extraction temperature is 65 ℃, filtering, and combining the filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 50 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation at the centrifugal rotation speed of 4000rpm for 15min to prepare a supernatant, thus obtaining the high-purity liquid.
The invention also provides a preparation method of the toothpaste containing the snow lotus herb component, which comprises the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotating speed of 450rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, pumping until the vacuum degree in the tank is-0.086 Mpa, and filling to obtain the toothpaste.
Example 3A toothpaste containing snow lotus herb ingredient
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 10:5: 9.
The preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component comprises the following steps:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, wherein each extraction time is 0.5h, and the adding mass ratio of the snow lotus pollen to the petroleum ether is 1: 7.5; the reflux extraction temperature is 70 ℃; filtering and drying the filter residue at 105 ℃ to obtain degreased snow lotus powder;
(3) adding the degreased snow lotus powder prepared in the step (2) into a flask, adding the degreased snow lotus powder and an ethanol solution according to the mass ratio of 1:13, adding the ethanol solution with the mass fraction of 75% to perform reflux extraction for 5 times, wherein the reflux extraction temperature is 70 ℃, filtering, and combining the filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 55 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation at the centrifugal rotation speed of 4000rpm for 15min to prepare a supernatant, thus obtaining the high-purity liquid.
The invention also provides a preparation method of the toothpaste containing the snow lotus herb component, which comprises the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotating speed of 500rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, pumping until the vacuum degree in the tank is-0.087 Mpa, and filling to obtain the toothpaste.
Example 4A toothpaste containing snow lotus herb ingredient
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 16 parts of zinc citrate, 12 parts of titanium dioxide, 25 parts of wetting agent, 35 parts of abrasive, 2.6 parts of sodium lauryl sulfate, 2.5 parts of calcium bicarbonate, 12 parts of thickening agent, 15 parts of sodium benzoate, 13 parts of trichlorogalactose, 25 parts of sodium phytate, 25 parts of snow lotus herb extract, 1.3 parts of essence and 18 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 5:11: 15.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 15:6: 7.
The preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component comprises the following steps:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, wherein each extraction time is 0.5h, and the adding mass ratio of the snow lotus pollen to the petroleum ether is 1: 9; the reflux extraction temperature is 75 ℃; filtering and drying the filter residue at the drying temperature of 110 ℃ to obtain degreased snow lotus powder;
(3) adding the degreased snow lotus powder prepared in the step (2) into a flask, adding the degreased snow lotus powder and an ethanol solution according to the mass ratio of 1:15, adding the ethanol solution with the mass fraction of 75% to perform reflux extraction for 5 times, wherein the reflux extraction temperature is 75 ℃, filtering, and combining the filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 60 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation at the centrifugal rotation speed of 4000rpm for 15min to prepare a supernatant, thus obtaining the high-purity liquid.
The invention also provides a preparation method of the toothpaste containing the snow lotus herb component, which comprises the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotation speed of 550rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, pumping until the vacuum degree in the tank is-0.088 Mpa, and filling to obtain the toothpaste.
Example 5A toothpaste containing snow lotus herb
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 18 parts of zinc citrate, 15 parts of titanium dioxide, 30 parts of wetting agent, 40 parts of abrasive, 3 parts of sodium lauryl sulfate, 3 parts of calcium bicarbonate, 15 parts of thickening agent, 20 parts of sodium benzoate, 15 parts of trichlorogalactose, 18 parts of sodium phytate, 30 parts of snow lotus herb extract, 1.5 parts of essence and 20 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 14.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 11:6: 8.
The preparation method of the snow lotus herb extract in the toothpaste containing the snow lotus herb component comprises the following steps:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, wherein each extraction time is 0.5h, and the adding mass ratio of the snow lotus pollen to the petroleum ether is 1: 10; the reflux extraction temperature is 90 ℃; filtering and drying the filter residue at 105 ℃ to obtain degreased snow lotus powder;
(3) adding the degreased snow lotus powder prepared in the step (2) into a flask, adding the degreased snow lotus powder and an ethanol solution according to the mass ratio of 1:17, adding the ethanol solution with the mass fraction of 75% to perform reflux extraction for 5 times, wherein the reflux extraction temperature is 60 ℃, filtering, and combining the filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 55 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation at the centrifugal rotation speed of 4000rpm for 15min to prepare a supernatant, thus obtaining the high-purity liquid.
The invention also provides a preparation method of the toothpaste containing the snow lotus herb component, which comprises the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotating speed of 600rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, exhausting until the vacuum degree in the tank is-0.090 Mpa, and filling to obtain the toothpaste.
Comparative example 1, a toothpaste
The toothpaste comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11. The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 10:5: 9.
The toothpaste of this comparative example was prepared in a similar manner to example 3.
The difference between this comparative example and example 3 is: in this comparative example, snow lotus herb extract was not added.
Comparative example 2 toothpaste containing snow lotus herb component
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 10:5: 9.
The toothpaste containing the snow lotus herb ingredient in this comparative example was prepared similarly to example 3.
The difference between this comparative example and example 3 is: no zinc citrate was added in this comparative example.
Comparative example 3 toothpaste containing snow lotus herb component
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 10:5: 9.
The toothpaste containing the snow lotus herb ingredient in this comparative example was prepared similarly to example 3.
The difference between this comparative example and example 3 is: the abrasive in this comparative example was not added with hydroxyapatite.
Comparative example 4 toothpaste containing snow lotus herb component
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 10:5: 9.
The toothpaste containing the snow lotus herb ingredient in this comparative example was prepared similarly to example 3.
The difference between this comparative example and example 3 is: no sodium benzoate was added in this comparative example.
Comparative example 5 toothpaste containing snow lotus herb component
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 10:5: 9.
The toothpaste containing the snow lotus herb ingredient in this comparative example was prepared similarly to example 3.
The difference between this comparative example and example 3 is: in this comparative example, trichlorogalactose was not added.
Comparative example 6 toothpaste containing snow lotus herb component
The toothpaste containing the snow lotus herb component comprises the following components in parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
The humectant in the toothpaste containing the snow lotus herb component is prepared from sorbitol, glycerol and soybean lecithin according to the mass ratio of 4:13: 11.
The thickener in the toothpaste containing the snow lotus herb component is composed of xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose according to the mass ratio of 1:1: 1.
The toothpaste containing the snow lotus herb ingredient in this comparative example was prepared similarly to example 3.
The difference between this comparative example and example 3 is: the amount ratio of the components of the thickener in this comparative example was 1:1: 1.
Test example I, Performance test of toothpaste
Test samples: the toothpaste containing the snow lotus herb ingredient prepared in the examples 1-5 and the comparative examples 1-5;
the test method comprises the following steps: randomly selecting 100 adult volunteers with different degrees of oral diseases, averagely dividing into 10 groups, respectively using the toothpastes containing the snow lotus herb components prepared in the examples 1-5 and the comparative examples 1-5, respectively brushing teeth for 1 time in the morning and evening, lasting for 5-10 min each time, continuously using for 10 days, and not taking any other medicine for treating the oral diseases in the period;
observing changes in clinical symptoms and signs: and (3) healing: after the medicine is taken for 10 days, gingival bleeding, halitosis and toothache symptoms disappear, and the chewing function is recovered; the effect is shown: gingival bleeding, halitosis disappearance, periodontal pocket shallowing, and chewing function improvement; the improvement of gingival bleeding, halitosis and tooth looseness. No effect, no change of clinical symptoms and signs;
bacterial changes in the periodontal pocket: in all cases, the secretion in the periodontal pocket is taken for gram staining bacteria examination before and after treatment;
and (3) test results: the test results are shown in tables 1 and 2.
TABLE 1 clinical symptoms and signs
Table 2 antibacterial property test
As can be seen from tables 1 and 2, the effective rate of the toothpaste containing snow lotus herb components provided by the invention after 10 days is 90-100%, the toothpaste has an obvious bactericidal effect, bacteria in periodontal pockets are greatly reduced after 10 days, and the toothpaste containing snow lotus herb components prepared in the application example 3 has the highest effective rate and the best bactericidal effect, and is the best embodiment of the invention.
Compared with example 3, the clinical test and the antibacterial test of the toothpaste prepared in comparative example 1 are reduced, which shows that the snow lotus herb extract has the functions of anti-inflammation and analgesia. Clinical trial and antibacterial trial of the toothpaste prepared in comparative example 2 were both less effective, indicating that zinc citrate has an irreplaceable effect in the formulation of the present invention. The clinical test and antibacterial test effects of the toothpaste prepared in comparative example 3 were reduced, indicating that hydroxyapatite can effectively prevent the problems of tooth sensitivity, gingival bleeding, tooth root exposure, etc. caused by hydrated silica. The clinical test and the antibacterial test effects of the toothpastes prepared in the comparative examples 4 and 5 are reduced, which shows that the sodium benzoate, the trichlorogalactose and the sodium phytate act together to effectively relieve the problem that the sodium lauryl sulfate is easy to cause oral mucosa rupture and further induce and aggravate oral ulcer.
Test example two, toothpaste stability test
Test samples: the toothpaste containing the snow lotus herb components prepared in the examples 1-5 and the comparative example 6;
the test method comprises the following steps: enzyme resistance: fully swelling a test sample in a water bath at 40 ℃ to prepare a toothpaste suspension, then keeping the temperature constant for half an hour, transferring 1mL of cellulase solution by using a dry transfer pipette, adding the cellulase solution into the toothpaste suspension, uniformly stirring, and immediately detecting the viscosity of the suspension under the condition of keeping the temperature constant at 40 ℃, wherein the viscosity is called as 'initial viscosity'; preventing the toothpaste suspension in a 40 deg.C incubator for 80min, and detecting viscosity at 40 deg.C, which is final viscosity; enzyme resistance of the toothpaste-final viscosity/initial viscosity;
thermal stability: placing the test sample into a refrigerator at-8 + -1 deg.C, taking out after 8 hr, immediately placing into a constant temperature incubator at 45 + -1 deg.C, taking out after 8 hr, cooling to 25 deg.C, and checking toothpaste phase;
and (3) test results: the test results are shown in Table 3.
Table 3 toothpaste stability test results
Group of | Resistance to enzymes | Thermal stability |
Example 1 | 0.83 | Without water seepage, air expansion, coarse smell and off-flavor |
Example 2 | 0.79 | Without water seepage, air expansion, coarse smell and off-flavor |
Example 3 | 0.85 | Without water seepage, air expansion, coarse smell and off-flavor |
Example 4 | 0.76 | Without water seepage, air expansion, coarse smell and off-flavor |
Example 5 | 0.77 | Without water seepage, air expansion, coarse smell and off-flavor |
Comparative example 6 | 0.36 | Paste layering and small amount of water seepage |
As can be seen from table 3, the toothpaste containing snow lotus herb ingredient provided by the present invention has good enzyme resistance and thermal stability, wherein the enzyme resistance of example 3 is the best example of the present invention. Compared with example 3, comparative example 3 changes the dosage ratio of the thickener in the formula, but the prepared toothpaste containing the snow lotus herb component has reduced enzyme resistance and thermal stability, which shows that the effect of each component of the thickener in the formula of the invention under the condition of the mixture ratio of the invention is optimal, and the change of the dosage and the mixture ratio of the thickener causes uneven distribution of the wetting agent and other components in the formula, thereby influencing the enzyme resistance and the thermal stability of the toothpaste body.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art will recognize that changes may be made to the embodiments described above without departing from the spirit and scope of the invention. Therefore, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the technical spirit of the present invention are covered by the claims of the present invention.
Claims (10)
1. The toothpaste containing the snow lotus herb is characterized by comprising the following components in parts by weight:
10-18 parts of zinc citrate, 6-15 parts of titanium dioxide, 15-30 parts of wetting agent, 25-40 parts of friction agent, 2-3 parts of sodium lauryl sulfate, 1-3 parts of calcium bicarbonate, 5-15 parts of thickening agent, 5-20 parts of sodium benzoate, 10-15 parts of trichlorogalactose, 10-25 parts of sodium phytate, 15-30 parts of snow lotus herb extract, 1-1.5 parts of essence and 15-20 parts of water.
2. The toothpaste containing snow lotus herb ingredients as claimed in claim 1, which is characterized by comprising the following ingredients and parts by weight: 14 parts of zinc citrate, 9 parts of titanium dioxide, 23 parts of wetting agent, 36 parts of abrasive, 2.3 parts of sodium lauryl sulfate, 2 parts of calcium bicarbonate, 10 parts of thickening agent, 13 parts of sodium benzoate, 12 parts of trichlorogalactose, 20 parts of sodium phytate, 24 parts of snow lotus herb extract, 1.1 parts of essence and 16 parts of water.
3. The toothpaste containing snow lotus herb ingredients as claimed in claim 1 or 2, wherein the humectant is composed of sorbitol, glycerin and soybean lecithin in a mass ratio of 3-5: 10-13: 9-15.
4. The toothpaste containing snow lotus herb ingredients as claimed in claim 1 or 2, wherein the abrasive is composed of hydrated silica and hydroxyapatite at a mass ratio of 5: 7.
5. The toothpaste containing snow lotus herb ingredients as claimed in claim 1 or 2, wherein the thickener is xanthan gum, tetrasodium pyrophosphate and sodium carboxymethylcellulose in a mass ratio of 9-15: 4-7: 3-9.
6. The toothpaste containing snow lotus herb ingredients as claimed in claim 1 or 2, wherein the snow lotus herb extract is prepared by the method comprising:
(1) pulverizing dried herba Saussureae Involueratae, and sieving with 50 mesh sieve to obtain herba Saussureae Involueratae powder;
(2) adding the snow lotus pollen prepared in the step (1) into a flask, adding petroleum ether for reflux degreasing for 4 times, extracting for 0.5h each time, filtering, and drying filter residues to prepare degreased snow lotus powder;
(3) adding the degreased saussurea involucrate powder prepared in the step (2) into a flask, adding 75% ethanol solution by mass, performing reflux extraction for 5 times, extracting for 1 hour each time, filtering, and combining filtrates to prepare a crude extract;
(4) performing dynamic continuous countercurrent extraction on the crude extract prepared in the step (3), wherein the extraction temperature is 45-60 ℃, and the extraction time is 1h to prepare a refined extract;
(5) and (4) carrying out reduced pressure concentration on the refined extract prepared in the step (4), standing for 24h, and carrying out centrifugal separation to obtain a supernatant.
7. The toothpaste containing snow lotus herb ingredients as claimed in claim 6, wherein the snow lotus herb extract is prepared by adding snow lotus herb powder and petroleum ether in the step (2) in a mass ratio of 1: 7-10; the reflux extraction temperature is 60-90 ℃; the drying temperature is 90-110 ℃.
8. The toothpaste containing snow lotus herb ingredients as claimed in claim 6, wherein the snow lotus herb extract is prepared by adding the defatted snow lotus herb powder and the ethanol solution in the step (3) in a mass ratio of 1: 12-17; the reflux extraction temperature is 60-75 ℃.
9. The toothpaste containing snow lotus herb ingredients as claimed in claim 6, wherein the preparation method of snow lotus herb extract is characterized in that the centrifugation speed in step (5) is 4000rpm and the centrifugation time is 15 min.
10. A method for preparing the toothpaste containing snow lotus herb ingredients according to any one of claims 1 to 9, comprising the following steps:
s1, dissolving the wetting agent with the formula amount in water, stirring for 10min at the rotating speed of 400-600 rpm, adding sodium lauryl sulfate, zinc citrate, sodium phytate and sodium benzoate, and continuously stirring for 0.5h to obtain a mixture A;
s2, mixing the friction agent, the titanium dioxide and the calcium bicarbonate according to the formula amount, and stirring for 10min at the rotating speed of 200rpm to prepare a mixture B;
s3, adding the mixture B prepared in the step S2 into the mixture A prepared in the step S1, stirring at the rotating speed of 800rpm for 0.5h, and homogenizing for 1h to prepare a mixture C;
s4, adding the thickener, the snow lotus herb extract, the trichlorogalactose and the essence according to the formula amount into the mixture C prepared in the step S3, continuously stirring for 0.5h, and homogenizing for 1h to prepare toothpaste;
s5, adding the toothpaste body prepared in the step S4 into a paste preparation tank, pumping until the vacuum degree in the tank is-0.085 to-0.090 Mpa, and filling to obtain the toothpaste.
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CN111228185A (en) * | 2020-03-27 | 2020-06-05 | 洪雅县瓦屋山药业有限公司 | Coptis toothpaste and preparation method thereof |
CN111358724A (en) * | 2020-04-20 | 2020-07-03 | 平措绕吉 | Functional toothpaste and preparation method thereof |
CN111358725A (en) * | 2020-04-21 | 2020-07-03 | 斯耐奇(武汉)智能科技有限公司 | Toothpaste and preparation method thereof |
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2020
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CN102579305A (en) * | 2012-03-29 | 2012-07-18 | 安徽两面针·芳草日化有限公司 | Natural medicine toothpaste with saussurea involucrata as major material |
CN103462841A (en) * | 2013-09-06 | 2013-12-25 | 广州立白企业集团有限公司 | Toothpaste containing saussurea involucrate component |
CN105748377A (en) * | 2016-04-27 | 2016-07-13 | 安徽人民健康生物科技有限公司 | Chinese medicinal toothpaste and preparing method thereof |
CN105796429A (en) * | 2016-04-27 | 2016-07-27 | 安徽人民健康生物科技有限公司 | Toothpaste |
CN108113915A (en) * | 2016-11-29 | 2018-06-05 | 房世俊 | A kind of Allergy-free toothpaste and preparation method thereof |
CN111228185A (en) * | 2020-03-27 | 2020-06-05 | 洪雅县瓦屋山药业有限公司 | Coptis toothpaste and preparation method thereof |
CN111358724A (en) * | 2020-04-20 | 2020-07-03 | 平措绕吉 | Functional toothpaste and preparation method thereof |
CN111358725A (en) * | 2020-04-21 | 2020-07-03 | 斯耐奇(武汉)智能科技有限公司 | Toothpaste and preparation method thereof |
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