CN111228171A - Preparation method of toothpaste rich in tea amino acid - Google Patents
Preparation method of toothpaste rich in tea amino acid Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- 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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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- 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
- A61K8/20—Halogens; Compounds thereof
- A61K8/21—Fluorides; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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Abstract
The invention belongs to the field of daily chemicals, and provides a preparation method of toothpaste rich in tea amino acid. The method comprises the following steps: 1) micronizing fresh green tea to obtain tea powder, and sieving to obtain tea powder with particle size of 10-50 μm. 2) Ultrasonic cold extraction: adding the superfine powder into 55% ethanol extract at 5-15 deg.C, wherein the weight ratio of tea powder to extract is 1:5-1: 100. Shaking in ultrasonic oscillator for 1-180min, adjusting pH to 7-8 with sodium hydroxide, and filtering. 3) And (3) re-purification: filtering the fine filtrate with active carbon; filtering the obtained filtrate with 0.35-0.45um water phase filtering membrane to obtain folium Camelliae sinensis extract. 4) Preparing tea amino acid toothpaste: the tea extract is matched with common toothpaste raw materials to prepare the toothpaste rich in tea amino acid. The toothpaste has the effects of natural nutrition, mild care, effective prevention of decayed teeth, breath freshening and the like.
Description
Technical Field
The invention relates to a preparation method of toothpaste rich in tea amino acid, which has the effects of natural nutrition, mild care, effective prevention of decayed teeth, breath freshening and the like.
Background
China is the hometown of tea, and Chinese tea has long-term culture and great spirit. The tea contains a plurality of functional components such as tea polyphenol, alkaloid, amino acid, tea pigment, vitamin and the like, has the effects of bacteriostasis, anti-inflammation, heat clearing, detoxifying, sweet taste returning, body fluid production promoting, antiallergic, tobacco toxin removing and the like, and in addition, the tea also contains rich fluoride components, so that the caries can be effectively prevented.
The composition, content, degradation products and transformation products of amino acids in tea leaves and the content variation among these components will directly affect the aroma and taste of tea leaves. 26 amino acids are found and identified in tea at present, such as theanine, glutamic acid, arginine, serine, aspartic acid and the like, wherein the theanine accounts for more than 50% of the total amount of the amino acids and is the characteristic amino acid of the tea; a great deal of research shows that amino acid in tea not only is a main component determining the taste of tea soup, but also is a necessary nutrient substance for human body, and plays an extremely important role in preventing and recovering human diseases.
With the continuous development of the toothpaste industry, more and more consumers pay more attention to oral problems. Along with the promotion of the concept of 'health safety, nature and mildness' of people, health care products are pursued in the market in recent years. However, people focus on the research reports of tea polyphenol toothpaste, and the toothpaste added with tea amino acid is rare and rare.
The CN102764207A patent discloses a toothpaste containing pu' er tea extract, which is obtained by processes of low-temperature crushing, ultrasonic leaching, filter pressing, separation, concentration and the like, but the main functional substances are not clear, and the extract is a mixed tea extract. CN106176376A discloses a microsphere coated with a tea extract complex, which is applied to edible toothpaste, the microsphere coated with the tea extract complex is obtained by coating a complex of a tea extract and metal ions by a lactic acid/glycolic acid copolymer, but the efficacy of the microsphere is embodied in the anticaries property of tea polyphenol; CN107898695A adopts microcapsule preparation technology to process nano tea powder into nano tea particles, and the nano tea particles are directly added into a toothpaste base material, but the efficacy is difficult to exert. In the currently disclosed tea extract toothpaste patent, the care effect of tea amino acid on the oral cavity is rarely considered, and the tea amino acid toothpaste on the market is much less and less.
Disclosure of Invention
Aiming at the defects of the prior art, the invention brings natural and healthy ideas to consumers by extracting tea amino acid from fresh green tea and adding the tea amino acid to a basic formula of toothpaste, and meanwhile, the combination of the tea amino acid and fluoride plays a role in effectively caring gingiva and solving a series of problems in oral cavity. The complete technical scheme provided by the invention is as follows:
the invention provides a preparation method of toothpaste rich in tea amino acid. The method comprises the technologies of superfine grinding, 55% ethanol ultrasonic cold extraction, activated carbon adsorption and the like, can extract amino acid in tea to the maximum extent to obtain tea amino acid extracting solution with low impurity content, and successfully adds the tea amino acid extracting solution into a toothpaste formula. The method comprises the following specific steps: 1) micronizing folium Camelliae sinensis, micronizing fresh green tea to obtain folium Camelliae sinensis powder, and sieving to obtain folium Camelliae sinensis powder with particle size of 10-50 μm. 2) Ultrasonic cold extraction: adding the superfine powder into 55% ethanol extract (the temperature of the extract is 5-15 deg.C), wherein the weight ratio of the tea powder to the extract is 1:5-1: 100. Shaking in ultrasonic oscillator for 1-180min, adjusting pH of the obtained solution with sodium hydroxide to 7-8, and filtering to obtain fine filtrate of tea amino acids. 3) And (3) re-purification: filtering the fine filtrate with an active carbon filter to adsorb pigments in the tea; filtering the obtained filtrate with 0.35-0.45um water phase filtering membrane to remove macromolecular substances in the solution to obtain tea leaf extract rich in tea amino acids. 4) Preparing tea amino acid toothpaste: the tea extract is mixed with water, humectant, thickener, foaming agent, abrasive, essence, fluoride, etc. to make into toothpaste rich in tea amino acids. The toothpaste rich in tea amino acid has the effects of natural nutrition, mild care, effective prevention of decayed teeth, breath freshening and the like.
Preferably, the fresh green tea is picked fresh green tea leaves or commercially available green tea leaves, the stains on the fresh green tea leaves are cleaned by deionized water, the fresh green tea leaves are kept clean and pollution-free, and then the tea leaves are naturally dried.
Preferably, the tea leaf is subjected to superfine grinding by adopting an ultrasonic speed type superfine grinding method.
Preferably, the vibration power of the ultrasonic oscillator is 1-50W.
Preferably, the mesh number of the activated carbon in the activated carbon filter is 60-200 meshes.
Preferably, the tea amino acid toothpaste comprises the following raw material components in percentage by weight: 20-60% of humectant, 10-30% of water, 0.05-0.5% of fluoride, 0.1-2.8% of foaming agent, 10-30% of abrasive, 0.5-1.5% of thickening agent, 0.05-15% of tea amino acid-rich extract and 0.5-2.5% of essence; the preparation method of the tea amino acid toothpaste comprises the following steps: mixing and dissolving tea amino acid extract, water, humectant and fluoride, sequentially adding thickener, foaming agent and friction agent, stirring for 20min, vacuum degassing, and maintaining vacuum degree at-0.097 MPa and 20-45 deg.C. Then adding essence, and continuing stirring for 20 min. Breaking vacuum, and making into toothpaste rich in tea amino acids.
Preferably, the humectant is an ingredient that prevents the oral care composition from becoming dehydrated and hardened. Exemplary humectants include, but are not limited to, one or more of the following: sorbitol, glycerol, propylene glycol, PEG.
Preferably, the fluoride is an anticaries ingredient for oral care compositions. Exemplary fluorides include, but are not limited to, one or more of the following: sodium fluoride, stannous fluoride and sodium monofluorophosphate.
Preferably, the surfactant functions to emulsify the flavour and to lather in the oral care composition. Surfactants include, but are not limited to, anionic surfactants such as sodium dodecyl sulfate, and the like, amphoteric surfactants such as betaine, amino acid surfactants such as, or nonionic surfactants such as, polyoxyethylene and polyoxypropylene copolymers, polyethylene glycol, and the like.
Preferably, the abrasive is the primary cleaning component of the oral care composition and is selected with due regard to hardness, size, shape and amount to ensure effective cleaning without abrading the teeth. Exemplary abrasives include, but are not limited to, one or more of the following: calcium carbonate, calcium hydrogen phosphate, hydrated silicon dioxide, aluminum hydroxide, calcite, dicalcium phosphate, hydrated monocalcium phosphate, calcium pyrophosphate.
Preferably, the thickening agent is one that increases the viscosity of the solution or liquid-solid mixture. The purpose of the thickener is to provide skeleton, flow and stability to the product. Exemplary thickeners include, but are not limited to, one or more of the following: carboxymethyl cellulose, hydroxyethyl cellulose, xanthan gum, guar gum, carrageenan, xanthan gum.
Preferably, the flavour is a substance used to improve the sensory properties of the oral care composition. Exemplary flavoring agents include, but are not limited to, spearmint oil, peppermint oil, oil of wintergreen, clove oil, poplar oil, eucalyptus oil, cinnamon oil, lemon oil, and orange peel oil.
Compared with the prior art, the invention has the following advantages:
1. the tea extract is prepared by separating and extracting fresh green tea leaves, and is natural and healthy.
2. The superfine grinding technology can destroy plant cell walls, increase the contact area of water and tea leaves and accelerate the release of tea amino acid.
3. The 55% ethanol leaching solution can maximally leach out amino acids in the tea, and the leaching efficiency is high (Table 1).
4. The tea extract extracted at low temperature has the least impurity content and the best quality (table 2).
5. The activated carbon filter effectively adsorbs pigment components in the tea; filtering with 0.35-0.45um water phase filtering membrane to remove macromolecular substances in the solution. The tea polyphenol can be stably stored for a long time after being added into a formula due to the reduction of the influence of other components (such as tea polyphenol).
6. The tea amino acid-fluoride is added to make the fluorine tea component have effective effects in preventing dental caries and strengthening teeth (Table 4).
TABLE 1 extraction results of amino acids/mg "L" with different solvents-1
Note: A. extracting with boiling water at 10 deg.C for 60min, wherein the weight ratio of tea powder to extract is 1:5-1: 100. B. The data of the table are detected by high performance liquid chromatography, C18A chromatographic column.
TABLE 2 analysis of the content of various components of tea leaves/mg "L in 55% ethanol at different extraction temperatures-1
Detailed Description
The following examples are given to illustrate the present invention and it is necessary to point out here that the following examples are given for further illustration of the invention only and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims and the insubstantial modifications and adaptations of the invention by those skilled in the art from the foregoing disclosure.
Table 3 example recipe comparison table
Example 1
Fresh green tea is subjected to ultrasonic superfine grinding and then sieved to ensure that the granularity of tea powder is 20 mu m. Adding the superfine powder into 55% ethanol extract at 10 deg.C, wherein the weight ratio of tea powder to extract is 1: 50. Shaking in ultrasonic oscillator for 120min to obtain solution, adjusting pH to 7.5 with sodium hydroxide, and filtering to obtain fine filtrate of tea amino acids. Filtering the fine filtrate with an active carbon filter to adsorb pigments in the tea; filtering the obtained filtrate with 0.45um water phase filtering membrane to remove macromolecular substances in the solution to obtain tea extract rich in tea amino acids. Adding 5% of tea extract, 25% of water, 45.5% of humectant and 0.3% of fluoride according to weight percentage, mixing and dissolving, adding 1% of thickening agent, 2% of foaming agent and 20% of friction agent in sequence, stirring for 20min, and vacuum degassing, keeping the vacuum degree at-0.097 MPa and the temperature at 25 ℃. Then 1.2% essence is added and stirring is continued for 20 min. Breaking vacuum, and making into toothpaste rich in tea amino acids.
Example 2
Fresh green tea is subjected to ultrasonic superfine grinding and then sieved to ensure that the granularity of tea powder is 20 mu m. Adding the superfine powder into 55% ethanol extract at 10 deg.C, wherein the weight ratio of tea powder to extract is 1: 50. Shaking in ultrasonic oscillator for 120min to obtain solution, adjusting pH to 7.5 with sodium hydroxide, and filtering to obtain fine filtrate of tea amino acids. Filtering the fine filtrate with an active carbon filter to adsorb pigments in the tea; filtering the obtained filtrate with 0.45um water phase filtering membrane to remove macromolecular substances in the solution to obtain tea extract rich in tea amino acids. Adding 10% of tea extract, 20% of water, 45.5% of humectant and 0.3% of fluoride according to weight percentage, mixing and dissolving, adding 1% of thickening agent, 2% of foaming agent and 20% of friction agent in sequence, stirring for 20min, and vacuum degassing, keeping the vacuum degree at-0.097 MPa and the temperature at 25 ℃. Then 1.2% essence is added and stirring is continued for 20 min. Breaking vacuum, and making into toothpaste rich in tea amino acids.
Example 3
Fresh green tea is subjected to ultrasonic superfine grinding and then sieved to ensure that the granularity of tea powder is 20 mu m. Adding the superfine powder into 55% ethanol extract at 10 deg.C, wherein the weight ratio of tea powder to extract is 1: 50. Shaking in ultrasonic oscillator for 120min to obtain solution, adjusting pH to 7.5 with sodium hydroxide, and filtering to obtain fine filtrate of tea amino acids. Filtering the fine filtrate with an active carbon filter to adsorb pigments in the tea; filtering the obtained filtrate with 0.45um water phase filtering membrane to remove macromolecular substances in the solution to obtain tea extract rich in tea amino acids. Adding 15% of tea extract, 15% of water, 45.5% of humectant and 0.3% of fluoride according to weight percentage, mixing and dissolving, adding 1% of thickening agent, 2% of foaming agent and 20% of friction agent in sequence, stirring for 20min, and vacuum degassing, keeping the vacuum degree at-0.097 MPa and the temperature at 25 ℃. Then 1.2% essence is added and stirring is continued for 20 min. Breaking vacuum, and making into toothpaste rich in tea amino acids.
Comparative example:
fresh green tea is subjected to ultrasonic superfine grinding and then sieved to ensure that the granularity of tea powder is 20 mu m. Adding the superfine powder into 55% ethanol extract at 10 deg.C, wherein the weight ratio of tea powder to extract is 1: 50. Shaking in ultrasonic oscillator for 120min to obtain solution, adjusting pH to 7.5 with sodium hydroxide, and filtering to obtain fine filtrate of tea amino acids. Filtering the fine filtrate with an active carbon filter to adsorb pigments in the tea; filtering the obtained filtrate with 0.45um water phase filtering membrane to remove macromolecular substances in the solution to obtain tea extract rich in tea amino acids. Adding 30 percent of water, 45.5 percent of humectant and 0.3 percent of fluoride according to weight percentage, mixing and dissolving, then adding 1 percent of thickening agent, 2 percent of foaming agent and 20 percent of abrasive in sequence, stirring for 20min, and vacuum degassing, keeping the vacuum degree at-0.097 MPa and the temperature at 25 ℃. Then 1.2% essence is added and stirring is continued for 20 min. Breaking vacuum, and making into toothpaste rich in tea amino acids.
Table 4: toothpaste taste and antibacterial effect
+And (3) testing the anti-caries effect: control group 58; the brushing groups 174 were tested once a day, morning and evening. An oral examination was performed before starting, and the number of decayed teeth and missing teeth, as well as the number of normal deciduous teeth and permanent teeth were recorded in detail. The subjects were instructed on the correct brushing regimen. Observing for 1 year, calculating the number of newly generated teeth in one year, and calculating the incidence rate of dental caries.
*Breath freshening was determined by the concentration of volatile sulfur compounds (volatesulfur compounds) in the oral cavity of the subject before and after brushing for 0.5hFor judgment, a portable sulfide meter (model Halimeter 4710-3, Interscan, USA) was used.
Claims (12)
1. A preparation method of toothpaste rich in tea amino acid is characterized by comprising the following steps: the method comprises the following steps:
(1) micronizing folium Camelliae sinensis, wherein fresh green tea is subjected to micronization to obtain folium Camelliae sinensis powder, and sieving to obtain folium Camelliae sinensis powder with particle size of 10-50 μm;
(2) ultrasonic cold extraction: adding the superfine powder into 55% ethanol extract, soaking at 5-15 deg.C, shaking in ultrasonic oscillator for 1-180min to obtain solution, adjusting pH to 7-8 with sodium hydroxide, and filtering to obtain refined tea amino acid solution;
(3) and (3) re-purification: filtering the fine filtrate with an active carbon filter to adsorb pigments in the tea; filtering the obtained filtrate with 0.35-0.45um water phase filtering membrane to remove macromolecular substances in the solution to obtain tea leaf extract rich in tea amino acids;
(4) preparing tea amino acid toothpaste: mixing the above folium Camelliae sinensis extract with water, humectant, thickener, foaming agent, abrasive, essence, fluoride, etc. to obtain toothpaste rich in tea amino acids; the tea amino acid toothpaste comprises the following components in percentage by weight: 20-60% of humectant, 10-30% of water, 0.05-0.5% of fluoride, 0.1-2.8% of foaming agent, 10-30% of abrasive, 0.5-1.5% of thickening agent, 0.05-15% of tea extract and 0.5-2.5% of essence.
2. The preparation method according to claim 1, wherein the fresh green tea in the step (1) is fresh green tea leaves or commercially available green tea leaves, and the fresh green tea leaves are cleaned with deionized water to keep the fresh green tea leaves clean and free from contamination, and then naturally dried.
3. The method according to claim 2, wherein the micronization step (1) is ultrasonic micronization.
4. The production method according to claim 1, wherein in the step (2), the ultrasonic oscillator has a vibration power of 1-50W.
5. The preparation method according to claim 1, wherein the activated carbon filter in the step (3) has an activated carbon mesh number of 60-200 meshes.
6. The preparation method of claim 1, wherein the tea amino acid toothpaste prepared in the step (4) is prepared by the following steps: mixing and dissolving tea amino acid extract, water, humectant and fluoride, sequentially adding thickener, foaming agent and friction agent, stirring for 20min, vacuum degassing, and maintaining vacuum degree at-0.097 MPa and temperature at 20-45 deg.C; adding essence, stirring for 20min, breaking vacuum, and making into toothpaste rich in tea amino acids.
7. The preparation method according to claim 1, wherein the humectant in the step (4) is an ingredient for preventing dehydration hardening of the oral care composition, and comprises one or more of sorbitol, glycerin, propylene glycol, and PEG.
8. The method of claim 1, wherein the fluoride in step (4) is an anticaries ingredient for an oral care composition comprising one or more of sodium fluoride, stannous fluoride, sodium monofluorophosphate.
9. The preparation method according to claim 1, wherein in the step (4), the surfactant can play a role of emulsifying essence and foaming in the oral care composition, and the surfactant comprises anionic surfactant sodium dodecyl sulfate or/and sodium dodecyl sulfate; amphoteric surfactants betaine or/and amino acids; the nonionic surfactant is polyoxyethylene and polyoxypropylene copolymer or/and polyethylene glycol.
10. The production method according to claim 1, wherein the friction agent in the step (4) is: calcium carbonate, calcium hydrogen phosphate, hydrated silicon dioxide, aluminum hydroxide, calcite, dicalcium phosphate, hydrated monocalcium phosphate, calcium pyrophosphate and hydrated silicic acid.
11. The production method according to claim 1, wherein the thickener in the step (4) is: one or more of carboxymethyl cellulose, hydroxyethyl cellulose, xanthan gum, guar gum, carrageenan, and xanthan gum.
12. The preparation method according to claim 1, wherein the essence in the step (4) is: one or more of spearmint oil, peppermint oil, oil of wintergreen, clove oil, poplar oil, eucalyptus oil, cinnamon oil, lemon oil, or orange peel oil.
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| CN113350479A (en) * | 2021-06-24 | 2021-09-07 | 芭纹连锁管理(深圳)有限公司 | Ointment for removing scars and preparation method thereof |
| CN114469794A (en) * | 2020-10-28 | 2022-05-13 | 南京中科游子生物技术研究院有限公司 | Green tea active substance mouthwash composition and preparation method thereof |
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Cited By (3)
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