CN116392410A - Functional toothpaste and preparation method thereof - Google Patents

Functional toothpaste and preparation method thereof Download PDF

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Publication number
CN116392410A
CN116392410A CN202310296177.XA CN202310296177A CN116392410A CN 116392410 A CN116392410 A CN 116392410A CN 202310296177 A CN202310296177 A CN 202310296177A CN 116392410 A CN116392410 A CN 116392410A
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phase
paste
stirring
toothpaste
stirred
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段梅莉
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8158Homopolymers or copolymers of amides or imides, e.g. (meth) acrylamide; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/737Galactomannans, e.g. guar; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses

Abstract

The invention discloses functional toothpaste and a preparation method thereof. The raw materials for preparing the functional toothpaste comprise an organic cleaning agent, an abrasive, a humectant, a foaming agent, cellulose gum, guar gum and an astringent.

Description

Functional toothpaste and preparation method thereof
Technical Field
The invention relates to oral hygiene, in particular to functional toothpaste and a preparation method thereof.
Background
The disease enters from the mouth, the oral cavity is the first gateway of the alimentary canal, and the oral cavity cleaning is an important guarantee for the health of human bodies. Brushing teeth after meals, and brushing teeth with warm water, toothpaste and a toothbrush is a simple, convenient and effective method for cleaning the oral cavity of a human. The novel cleaning products such as functional toothpaste and the like which can brush and remove dental calculus and can brush and remove oral pathogenic bacteria are developed, the first gateway of oral health is maintained, and the occurrence and development of digestive tract metabolic diseases are prevented, so that the novel cleaning products are a major thing which benefits mankind and is healthy in China and cannot be ignored. Therefore, there is an urgent need in the art to provide novel cleaning products such as functional toothpaste which can achieve a comparable tooth cleaning effect without damaging the oral cavity.
Disclosure of Invention
The invention aims to provide functional toothpaste containing an organic cleaning agent and a preparation method thereof.
In a first aspect of the present invention there is provided a functional toothpaste, the raw materials used to make the functional toothpaste comprising an organic cleaning agent, an abrasive, a humectant, a foaming agent, a cellulose gum, guar gum and an astringent.
In another embodiment, the feedstock further comprises a sweetener; and/or
Essence; and/or
A pH regulator; and/or
And (3) a preservative.
In another embodiment, the feedstock also includes other active materials.
In a second aspect of the present invention, there is provided a method of preparing a functional toothpaste according to the present invention as described above, the method comprising the steps of:
(1) Mixing an organic cleaning agent and cellulose gum to form a mucus A phase;
(2) Forming a nucleus;
(3) Wrapping with guar gum phase to form paste; and
(4) The functional toothpaste provided by the invention is obtained by wrapping the cellulose gum with the outer coating phase.
In another embodiment, the step of forming the nucleus comprises:
mixing mucus A phase, humectant, abrasive, sweetener B phase and foaming agent C phase; or (b)
Mixing mucus A phase, humectant, abrasive, sweetener B phase, fiber gum inner wrapping phase and foaming agent C phase.
In another embodiment, the sweetener B phase is obtained by mixing sweetener and water.
In another embodiment, the blowing agent phase C is obtained by mixing water and blowing agent.
In another embodiment, the cellulose gum internal coating phase is obtained by mixing cellulose gum, humectant and water.
In another embodiment, step (3) comprises mixing the core body with guar gum to obtain a paste.
In another embodiment, the guar phase is obtained by mixing guar and water.
In another embodiment, the step (4) includes mixing the paste obtained in the step (3), the cellulose gum outer coating phase, and one or more of the following substances to obtain the functional toothpaste: moisturizing agents, abrasives, astringents.
In another embodiment, the cellulose gum outer phase is obtained by mixing cellulose gum, an astringent and water.
In another embodiment, the cellulose gum cover in step (4) is wrapped by 1, 2 or 3 layers.
Accordingly, the invention provides the functional toothpaste which has the equivalent tooth washing effect and does not hurt the oral cavity.
Detailed Description
The inventors have made extensive and intensive studies by layering a coating pattern of an organic cleaner core formed of an organic polyphosphate copolymer, a cellulose gum inner coating, guar gum and a cellulose gum outer coating, and performing a mixing and stirring process: firstly, preparing an aqueous solution of cellulose gel containing an organic cleaning agent into emulsion to form core microcrystal particles; then wrapping microcrystalline particles with cellulose gum, and stirring to form an inner core, namely an inner package; then adding foaming agent and essence, and then wrapping the oily matter with guar gum and the like to seal the layer; and wrapping the mixture into layers by using cellulose glue, namely, wrapping the layers; finally, the mixture is covered with an astringent, and is fully mixed and stirred into paste with certain fluidity. The paste is turned over after degassing operation to form a fine, smooth, bright, moist and well-fixed toothpaste, and the toothpaste can be filled and sealed to prepare a toothpaste product. On this basis, the present invention has been completed.
As used herein, "organic cleaner", "PM copolymer", "functional surfactant" and "organic polyphosphate" are used interchangeably and refer to a copolymer composed of phosphoenolpyruvate potassium salt PEPK and acrylamide AM, the chemical structure of the PEPK-AM copolymer being as follows:
Figure BDA0004144147390000031
wherein m and n are integers not less than 2, and the ratio of m/n is 1:0.5-50 (such as but not limited to 1:1-8). The preparation process and properties of the functional surfactants used in the present invention are described in chinese patent application 201110303110.1, the contents of which are incorporated herein by reference. As used herein, "cellulose gum" is used interchangeably with "sodium carboxymethyl cellulose (Carboxymethylcellulose sodium, CMC)" and refers to a compound having the structure shown below:
Figure BDA0004144147390000032
herein, "guar gum" refers to a hydroxypropylated galactomannan having the structure shown below:
Figure BDA0004144147390000033
guar has a molecular weight of about 22 kilodaltons, CAS accession no: 9000-30-0, einecs accession number: 232-536-8.
Herein, "PEG400" refers to a mixture of ethylene oxide and water ring-opening polymerized; molecular formula HO (CH) 2 CH 2 O) nH represents, wherein n represents the average number of oxyethylene groups; average molecular weight 380-420.
Herein, "white sugar" is a refined sugar made from molasses extracted from sugar cane and sugar beet. Also called white sugar, soft white sugar, white granulated sugar, frosting, etc.
Functional toothpaste
The invention provides functional toothpaste, which is a viscous fluid body, can be extruded by slightly extruding the wall of the toothpaste tube, is a strip-shaped viscous toothpaste body, is broken and is not drawn, and is a fine, smooth, bright and elastic paste body on a toothbrush, and the shape of the toothpaste body is kept not to collapse. After the paste is washed by water, the paste has mild taste, does not feel spicy to the tongue, does not irritate the oral tissues, is dispersed and does not agglomerate, foam is formed at the moment of brushing, the foam is easy to wash, and the breath after brushing is fresh and the oral cavity has obvious and comfortable feeling. The functional toothpaste disclosed by the invention has a taste which is especially suitable for Asian people with delicate dietary tastes. The limit of harmful substances in the functional toothpaste body of the invention and the microbial index all accord with the national standard of the sanitary index requirement in GB8372-2008 toothpaste.
Regarding rheological investigation of toothpaste, measurement of a touch-change ring (when a toothpaste system is sheared, the toothpaste is destroyed, and after shearing is stopped, the paste thickens again, but the process has hysteresis, thus being reflected as a loop on a shear rate and shear stress graph, namely, the touch-change ring. The Thixotropic properties of the toothpaste were measured by a MARS 3 rotary rheometer (test mode of Thixotropic properties of toothpaste: thixotrop loop (ramp-up, ramp-down), test conditions: CR Lin 0.1-10 s-1, time 60s, rotor #100, temperature 23 ℃ C.; CR Lin 10-0.1 s-1, time 60s, rotor #100, temperature 23 ℃ C.; shear rate control, linear point taking) and showed that the Thixotropic properties of the abrasive-free 999 vitamin soft paste, lion Wang Heibai hydrated silica toothpaste, and the functional toothpaste provided by the present invention were 374Pa/s, 1351Pa/s, 1594-4419 Pa/s, respectively, showing that the Thixotropic properties of the abrasive-free paste were minimal, the Thixotropic properties of the abrasive-containing hydrated silica paste were inferior, and the Thixotropic properties of the abrasive-containing calcium carbonate paste were optimal. The order of magnitude of the results and thixotropic properties is: calcium carbonate toothpaste > silica toothpaste, remains highly consistent with the general rule. It was also found that the thixotropic ring area between the functional toothpastes provided by the present invention was very different, probably because the total amount of the contact ring area was affected to some extent by the astringent PEG 400.
The raw materials for preparing the functional toothpaste provided by the invention comprise a functional surfactant, an abrasive, a humectant, a foaming agent, cellulose gum, guar gum and an astringent. In order to obtain the toothpaste with larger thixotropy, the composition of other raw materials is screened and examined around selecting a functional surfactant as a cleaning agent. The functional toothpaste provided by the invention is a dynamic balance system with mutually matched and mutually restricted raw material components.
The raw materials for preparing the functional toothpaste provided by the invention can be one or more than two of the following: sweetener, essence, pH regulator, preservative, etc. Other active substances can be added into the raw materials for preparing the functional toothpaste.
The raw materials used for preparing the functional toothpaste provided by the invention are as follows:
the functional surfactant may be used in an amount of 0.1 to 2 parts by weight, such as, but not limited to, 0.15 to 0.4 parts by weight, 0.2 to 0.6 parts by weight, and the like. The organic cleaning agent is typically fed in the form of a transparent glue that is blended with the cellulose gum during manufacture.
The amount of the cellulose gum used may be not less than 0.8 parts by weight, for example, but not limited to, 0.8 to 2 parts by weight, 1 to 1.5 parts by weight, and the like.
Guar gum may be used in an amount of not less than 0.1g parts by weight, such as, but not limited to, 0.1-0.5 parts by weight, 0.14-0.3 parts by weight, 0.12-0.18 parts by weight, and the like.
The astringent may be used in an amount of 0.05 to 1.2 parts by weight, such as, but not limited to, 0.1 to 1 part by weight, 0.35 to 0.7 part by weight, etc.
The amount of the abrasive may be 40 to 72 parts by weight, for example, but not limited to, 55 to 65 parts by weight, 60 to 70 parts by weight, etc.
The humectant glycerin may be used in an amount of 1 to 10 parts by weight, for example, but not limited to, 1.5 to 6.5 parts by weight, 2 to 6 parts by weight, and the like.
The humectant sorbitol may be used in an amount of 10 to 60 parts by weight, such as, but not limited to, 15 to 35 parts by weight, 12 to 17 parts by weight, 20 to 32 parts by weight, and the like.
The foaming agent (e.g., without limitation, K12) may be used in an amount of 2-4 parts by weight, such as, without limitation, 2.5 parts by weight or more, and the like.
The sweetener may be used in an amount of 9 to 11 parts by weight, such as, but not limited to, 9.5 to 10.4 parts by weight, etc.
The essence may be used in an amount of 1 to 2 parts by weight, for example, but not limited to, 1.2 to 1.7 parts by weight, 1.3 to 1.9 parts by weight, etc.
The pH adjustor can be used in an amount of 0.1 to 0.5 parts by weight, such as, but not limited to, 0.2 to 0.33 parts by weight, 0.15 to 0.25 parts by weight, and the like.
The preservative, other active ingredients may be used in an amount of not more than 1.5 parts by weight.
In one embodiment of the present invention, the organic cleaning agent, abrasive, foaming agent, cellulose gum, astringent, humectant, thickener, sweetener, flavor are used in an amount of 80-100w/w%, such as, but not limited to, 90-100w/w%, 85-98w/w%, etc., based on the total weight of the raw materials used to make the functional toothpaste provided herein.
An astringent useful in the present invention is PEG400.
The abrasive useful in the present invention is calcium carbonate.
The foaming agent useful in the present invention is sodium lauryl sulfate.
The sweetener useful in the present invention is selected from white sugar, plant sweetener, or a mixture thereof, preferably white sugar.
The humectants useful in the present invention are selected from glycerin, sorbitol, or mixtures thereof.
The essence used in the present invention is selected from artificial essence, plants with fragrance, tea, etc.; such as, but not limited to, black peppermint flavor (e.g., supplied by Shanghai Si Yuan flavor Co., ltd.), poppy peppermint flavor (e.g., produced by Guangzhou Fenhao flavor Co., ltd.), and the like.
The pH regulator which can be used in the present invention is an alkaline substance. In order to reduce dissociation of abrasive calcium carbonate and improve stability of paste, pH value of paste is regulated by alkaline substance such as sodium bicarbonate (sodium bicarbonate), herba Menthae extract, and alkaloid-containing substance such as tea water (tea soup). The result shows that the alkaline substances such as the sodium bicarbonate solution, tea water and the like can well reduce the dissociation degree of calcium carbonate, prevent the flatulence and keep the stability of the toothpaste, so that the prepared toothpaste body basically accords with various indexes. The alkaline substance is selected from sodium bicarbonate, tea, etc.
The preservative useful in the present invention is selected from sodium chloride, paraformaldehyde, or a mixture thereof, preferably sodium chloride.
Other active ingredients useful in the present invention include traditional Chinese medicine, traditional Chinese medicine extracts, plant extracts, or mixtures thereof.
In the present invention, cellulose gum, guar gum, or a mixture thereof is used as a thickener.
Preparation of functional toothpaste
The inventor finds that the organic cleaning agent cannot be placed on the outermost layer in the manufacturing process, otherwise, the taste of the toothpaste after brushing is dry, and the process of wrapping the organic cleaning agent on the inner layer core is realized through continuous improvement and breakthrough. Namely, a layered package manufacturing process for coating layers by using glue. The introduction of virtually every material was examined for its feasibility as an additive.
Specifically, the preparation method of the functional toothpaste provided by the invention comprises the following steps:
firstly, forming microcrystalline nucleus, namely mucus A phase, by using cellulose gum and an organic cleaning agent;
step two, forming a nucleus body;
thirdly, forming paste by wrapping guar gum phase;
and fourthly, wrapping the toothpaste with a cellulose gum outer wrapping phase to obtain the functional toothpaste.
The first step is to mix the PM and CMC to form a colorless mucilage A phase.
In one embodiment of the present invention, a preservative and/or a humectant may also be added thereto.
In one embodiment of the invention, PM, preservative and humectant are mixed to obtain a colorless transparent aqueous solution, then CMC powder is added and decocted (e.g., without limitation, about 140℃. For two hours, etc.) to colorless mucilage A phase.
The second step is to mix the mucus A phase, humectant, abradant, sweetener B phase and foaming agent C phase.
The second step can be obtained by mixing mucus A phase, humectant, abrasive, sweetener B phase, fiber gum inner wrapping phase and foaming agent C phase.
The sweetener B phase can be prepared by decocting sweetener and water.
The foaming agent C phase can be prepared by mixing water and the foaming agent, heating (about 130-150 ℃) and decocting.
The cellulose gum internal coating phase is prepared by forming CMC and humectant into thin paste, and then pouring aqueous solution formed by the humectant and water into the thin paste and stirring.
In one embodiment of the invention, the second step is to mix the mucous A phase, humectant and abrasive to form an emulsion, and in some embodiments other active ingredients may be added; then mixing the emulsion, the sweetener B phase, the humectant and the friction agent, and standing for 8-20 hours; adding humectant, abrasive and foaming agent C, mixing, standing for 8-20 hr to form core-coated body.
In one embodiment of the invention, the second step is to mix the mucous A phase, humectant and abrasive to form an emulsion, and in some embodiments other active ingredients may be added; mixing the emulsion, sweetener B phase, and abrasive (or humectant) and standing for 8-20 hr; then adding the humectant, the abradant and the fiber glue internal wrapping phase, continuously adding the humectant, the abradant and the foaming agent C phase, mixing, and standing for 8-20 hours to form the nucleus wrapping body.
In one embodiment of the present invention, the second step is to scrape off the possible adhesive from the inner wall of the container after the sweetener B phase is added and allowed to stand for 8-20 hours, and then to mix well.
In the second step, the liquid level is generally raised after the foaming agent C phase is added, and the liquid level is fallen after standing for 8-20 hours.
Mixing the core-coated body with guar gum to obtain paste; in one embodiment, the core, flavor and guar gum may be mixed to provide a paste.
In one embodiment of the present invention, the third step is to add the essence and guar gum phase to the core-shell and then to stand for 8 to 20 hours.
The paste obtained in the third step is bright and fine like cream and does not adhere to walls.
The guar gum phase is formed by mixing guar gum and water; in one embodiment of the present invention, one or two or more of the following may be added thereto: humectant, pH regulator and essence.
In one embodiment of the invention, guar gum and humectant are mixed and then added to an aqueous solution in which a pH adjuster is dissolved, and stirred to obtain the guar gum phase.
In one embodiment of the invention, guar gum, humectant and water infused mint are mixed to obtain a solution with pH of 6-7, and fully stirred to prepare guar gum phase.
In one embodiment of the present invention, guar gum and humectant are mixed, a solution of the humectant dispersed in tea soup is added, and an astringent is added, and the guar gum phase is obtained by stirring.
And step four, mixing the paste obtained in the step three, the cellulose gum outer coating phase and one or more than two of the following substances to obtain the toothpaste: moisturizing agents, abrasives, astringents.
The cellulose gum outer coating phase is formed by mixing CMC, astringents and water; in one embodiment of the present invention, one or a mixture of two or more of the following may be added thereto: a humectant and a pH regulator.
In one embodiment of the invention, the emulsion formed by mixing CMC, astringent and humectant is an outer cellulosic gel phase.
In one embodiment of the invention, CMC powder and humectant are mixed, an aqueous solution of pH adjuster, humectant and water is added, and after addition of astringent, the mixture is mixed to form the cellulose gum outer phase.
In one embodiment of the present invention, CMC powder and humectant are mixed and then poured into an aqueous solution of astringent, pH adjuster and humectant dispersed in water, and thoroughly stirred to make a cellulose gum outer phase.
In one embodiment of the invention, CMC powder and humectant are mixed, a solution of pH regulator dispersed in tea soup is added, and the mixture is stirred to obtain a cellulose gum coating phase.
The fourth step may be carried out using 1 to 3 layers of cellulose gum coating obtained in the same or different manner.
In one embodiment of the present invention, a round bottom stirred tank (with a round bottom frame stirrer) is used for the fabrication. Such semi-automated equipment facilitates a more visual observation of the change from emulsion to paste. By using the manual treatment of the silica gel shovel spoon, the inner wall and the stirrer can be completely treated without dead angles, and the complete and uniform mixing of materials in the kettle is ensured.
In one embodiment of the present invention, the toothpaste is removed and degassed under a low vacuum atmosphere after the toothpaste is prepared. And then the mixture is stirred evenly by hand at normal temperature and normal pressure, filled into a PE hose and subjected to tail sealing treatment by a tail sealing machine to obtain the toothpaste product.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. However, any numerical value inherently contains certain standard deviations found in their respective testing measurements. As used herein, "about" generally means that the actual value is within plus or minus 10%, 5%, 1% or 0.5% of a particular value or range. Alternatively, the term "about" means that the actual value falls within an acceptable standard error of the average value, as determined by one of ordinary skill in the art. Except in the experimental examples, or where otherwise explicitly indicated, all ranges, amounts, values, and percentages used herein (e.g., to describe amounts of materials, lengths of time, temperatures, operating conditions, ratios of amounts, and the like) are to be understood to be modified by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the present specification and attached claims are approximations that may vary depending upon the desired properties. At least these numerical parameters should be construed as the number of significant digits and by applying ordinary rounding techniques.
Unless defined otherwise herein, the meanings of scientific and technical terms used herein are the same as commonly understood and used by one of ordinary skill in the art. Furthermore, as used in this specification, the singular noun encompasses the plural version of the noun without conflict with the context; plural nouns as used also encompasses singular versions of the noun.
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The above-mentioned features of the invention, or of the embodiments, may be combined in any desired manner. All of the features disclosed in this specification may be used in combination with any combination of features, provided that the combination of features is not inconsistent and all such combinations are contemplated as falling within the scope of the present specification. The various features disclosed in the specification may be replaced by alternative features serving the same, equivalent or similar purpose. Thus, unless expressly stated otherwise, the disclosed features are merely general examples of equivalent or similar features.
The invention has the main advantages that:
1. compared with the inorganic phosphate which is a cleaning agent in the market at present, the organic cleaning agent used in the invention is organic polyphosphate, has higher biocompatibility and stronger cleaning capability, and the prepared toothpaste has the characteristics of cleaner cleaning, safety and effectiveness, can prevent stomatitis reactions such as dental ulcer and the like, brush away dental calculus on teeth and smoke stains caused by smoking, and has a certain preventing effect on osteoporosis. The functional toothpaste provided by the invention has the effects of cleaning teeth, strengthening teeth, sterilizing and diminishing inflammation, and is suitable for people of all ages.
2. The functional toothpaste provided by the invention has the advantage of brushing teeth far better than professional tooth washing, and has no harm to oral cavity.
3. The toothpaste body obtained by the layered package manufacturing process has the characteristics of easiness in extrusion, good appearance, uniform paste dispersion, rich foam and comfortable tooth brushing taste.
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. The experimental procedures, which do not address the specific conditions in the examples below, are generally carried out under conventional conditions or under conditions recommended by the manufacturer. All percentages, ratios, proportions, or parts are by weight unless otherwise indicated. The units in weight volume percent are well known to those skilled in the art and refer, for example, to the weight of solute in 100 milliliters of solution (grams). Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials described herein are presented for illustrative purposes only.
The functional toothpaste prepared in the following examples was examined for a longer period of half to three years of shelf life by examining rheological properties, appearance (rheometer test and visual observation) of the paste, and indexes such as extrusion difficulty, tooth brushing taste and use effect.
The preparation method of the traditional Chinese medicine extract used in the following examples or comparative examples is as follows, or see the description of chinese application No. cn20090035994. X:
1. weighing dried Chinese medicinal materials (cut into small pieces of 1-5 cm) according to the following formula: 10g of safflower, lithospermum, kusnezoff monkshood root, common monkshood mother root, dark plum and honeysuckle respectively;
2. placing the medicinal materials into a sterilized wide-mouth bottle, and then pouring 500-3000ml of high-alcohol white spirit with the alcohol content of more than fifty degrees into the bottle for soaking and sealing;
3. taking out after 2-3 weeks, filtering to remove residue to obtain mauve liquid medicine.
Example 1
To a colorless mucilage A phase in a 15 liter stainless steel stirred tank, 492mg of the Chinese medicinal extract was added, and the mixture was stirred to form a transparent brown mucilage. After 770g of sorbitol was added and stirred uniformly, a mixture of 200g of sorbitol and 800g of calcium carbonate powder was added and stirred for 20min to become a white emulsion. Then, adding syrup B phase, stirring uniformly, adding 200g of sorbitol and 1000g of calcium carbonate powder mixture, stirring for 30min to form white emulsion, and standing overnight. Scraping possible adhesive on the inner wall of the stainless steel kettle by using a silica gel shovel, fully stirring to uniformly mix the emulsion, adding a mixture of 300g of sorbitol and 1200g of calcium carbonate powder, adding a foaming agent ointment C, uniformly stirring for 20min, and standing overnight after the liquid level rises. After stirring, the liquid level rapidly drops, 78g of the mint essence is added, and after stirring for 30min, strong fragrance is emitted. Then slowly adding guar gum ointment D phase, stirring for 30min to lighten fragrance, and standing overnight. After stirring, the liquid level of the paste falls, is bright and fine like cream, and the paste is not sticky. Adding 285g of sorbitol and 1000g of calcium carbonate powder, stirring for 30min to make the paste uniform, adding the E phase of the external ointment, stirring for 30min, and standing overnight. The paste falls after stirring and has sticky wall, 200g of sorbitol and 120g of calcium carbonate powder are added, and then 28.0g of PEG is added and stirred uniformly for 30min. Still sticking the wall, adding 120g of sorbitol, adding 5.0g of PEG, stirring uniformly, stirring for 20min, and standing overnight. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the paste is very moist, bright, thin and white after the empty holes are removed by manual stirring, and the solid state is kept well. The paste was split into 61 toothpastes of 150 g/toothpaste, each containing 0.16mg of organic polyphosphate. The paste is bright and fine, the extrusion is easy, the paste has good slidability, no flow and solidification on a toothbrush, the mouth feel is slightly spicy, the fragrance of flowers is off, the tongue is not spicy, the foam is very rich, the mouth feel is comfortable after brushing, and the hair drying effect is good. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before. After one year, the toothpaste tube is cut off to seal, the paste is still moist as before, and the color is bright white and not dark.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] to 1085.0g of an organic cleaning agent having a water-soluble amount of 10mg of an organic polyphosphate, 6.0g of sodium chloride and 30.0g of sorbitol were respectively added, followed by stirring and dissolution to obtain colorless and transparent aqueous solutions. Then 25.0g CMC powder is added and decocted into mucus.
[ preparation of sweetener B phase ] 600.0g of white granulated sugar is weighed and put into a beaker, 360.0g of purified water is added, and the mixture is boiled into yellow transparent sugar water solution.
[ preparation of foamer ointment C phase ] to a beaker of 176.0g of pure water, 176.0g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain a colorless and transparent ointment.
[ preparation of outer guar gum D phase ] 6.0g of guar gum powder was weighed, 94.0g of glycerin was poured and stirred into a thin paste, and 147.0g of pure water solution in which 5.0g of sodium bicarbonate was dissolved was poured and stirred, and an ointment was prepared.
[ preparation of the E phase of the outer-coated cellulose gum ] 25.0g of CMC powder was weighed, and 205.0g of glycerin was poured to cover the powder and stirred into a thin paste. 15.0g of sodium bicarbonate and 15.0g of sorbitol are respectively added into 375.0g of pure water and stirred to form an aqueous solution, the aqueous solution is poured into the thin paste and stirred rapidly, and then 10.0g of PEG40010 is added and stirred fully to prepare the transparent ointment.
Experimental results show that the preparation process of the organic cleaning agent core, guar gum and CMC outer coating (CMC adding mode 25+15+10) is reasonable and feasible, and the rheological properties of the paste system prepared when the dosages of CMC and guar gum are respectively not less than 0.8 g/branch and 0.1 g/branch are stable and reliable in shelf life.
Example 2
To the mucus A phase in a 15 liter stainless steel stirred tank, 300mg of the Chinese herbal extract was added and stirred to form a clear brown mucus. After 800g of sorbitol was added and stirred uniformly, a mixture of 200g of sorbitol and 600g of calcium carbonate powder was added and stirred for 15min to give a white emulsion. Then adding syrup B phase, stirring uniformly, adding 1200g of calcium carbonate powder mixture, stirring for 30min to form white emulsion, and standing overnight. Scraping possible adhesive on the inner wall of the stainless steel kettle by using a silica gel shovel, fully stirring to ensure that the emulsion is uniformly mixed, adding a mixture of 400g of sorbitol and 800g of calcium carbonate powder, fully stirring for 15min, slowly adding the cellulose gum-coated N-phase ointment, and fully stirring to form white paste. 100g of sorbitol and 400g of calcium carbonate powder are added, and the mixture is stirred for 30min and then left to stand overnight after being stirred evenly with the foaming agent ointment C. After stirring, the liquid level rapidly drops, 86.0g of the mint essence is added, after stirring for 10min, the guar gum ointment D phase is slowly added after stirring, after stirring uniformly, stirring for 15min, and the flavor is lightened. Then 200g of sorbitol and 600g of calcium carbonate powder are added, stirred for 20min to form a cream-like bright white paste, and the mixture is left to stand for one night. After stirring, the liquid level of the paste falls. Adding cellulose gum and wrapping with W-phase ointment, stirring for 30min, adding mixture of sorbitol 150g and calcium carbonate 300g, and stirring PEG 400.0 g to uniformity to obtain bright white paste, and standing overnight. After stirring, the liquid level of the paste falls, and a mixture of 120g of sorbitol and 120g of calcium carbonate powder is added, and the mixture is fully stirred and then left to stand. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the paste is very moist, bright, thin and white after the empty holes are removed by manual stirring, and the solid state is kept well. The paste was divided into 60 toothpaste pieces of 150 g/piece, each containing 0.70mg of organic polyphosphate. The paste is bright and fine, is easy to extrude, does not flow and is good in solidification on a toothbrush, has slightly spicy and flowery flavor, does not feel spicy on the tongue, is very rich in foam, has a tooth brushing taste slightly dry compared with the example 1, but has slightly sweet mouth cavity body fluid later, and shows that the cleaning effect is better. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before. After one year, the toothpaste tube is cut off to seal, and the paste is bright white and not dark.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] 25.0g of CMC powder was weighed into a beaker, to which 75.0g of glycerol was added and stirred into a thin paste. A uniform solution was prepared by stirring with 6.0g of sodium chloride and 15.0g of sorbitol and 1100g of an organic cleaning agent having a water-soluble amount of 42mg of an organic polyphosphate, and then poured into a thin paste, stirred and decocted to give a viscous liquid.
[ preparation of sweetener B phase ] 600.0g of white granulated sugar is weighed and put into a beaker, and 370.0g of purified water is added to be decocted into a sugar water solution.
[ preparation of foamer ointment C phase ] to a beaker containing 176.0g of pure water, 15.0g of sorbitol was added, followed by stirring to dissolve, then 176.0g of sodium dodecyl sulfate was added, and the mixture was decocted to a transparent ointment.
[ preparation of N-phase of Encapsulated cellulose gum ] 10.0g of CMC powder was weighed, 50.0g of glycerol was poured and stirred into a thin paste. 15.0g of sorbitol was added to 135.0g of pure water and stirred into a transparent aqueous solution, which was poured into a thin paste and stirred into an ointment.
[ preparation of outer guar gum D phase ] 6.0g of guar gum powder was weighed, 50.0g of glycerin was poured and stirred into a thin paste, and then 113.0g of pure water solution in which 5.0g of sodium bicarbonate was dissolved was poured and stirred, and an ointment was prepared.
[ preparation of the W phase of the outer-coated cellulose gum ] 15.0g of CMC powder was weighed, and 78.0g of glycerin was poured and stirred into a thin paste. 15.0g of sodium bicarbonate and 20.0g of sorbitol are respectively added into 228.0g of pure water and stirred to form an aqueous solution, the aqueous solution is poured into the thin paste and stirred, and 27.0g of PEG400 is added and stirred fully to prepare ointment.
The results show that the coating mode (CMC adding mode 25+10+15) of the organic cleaning agent core, CMC inner bag, guar gum and CMC outer bag (multi-layer bag) has good coating effect on essence, can well keep the moisture of the paste, and the addition of PEG400 can promote the curing degree of the paste to be improved, so that the contact ring area of the paste is greatly improved, and the stability is enhanced. Compared with the toothpaste without PEG400, the toothpaste has the advantages of obviously improved wettability, more comfortable taste, better tooth brushing effect, no peculiar smell in the oral cavity after tooth brushing, no irritation to oral tissues, slightly sweet body fluid and smooth tooth surface. The organic cleaning agent inner cladding is added, so that the cleaning effect of the cleaning agent which instantaneously bursts when the cleaning agent brushes teeth, namely when the balance point is broken, can be greatly improved. The cleaning effect of the toothpaste containing CMC inner package step is obviously improved.
Example 3
By the same operation as in example 2, an enclosed white paste was obtained from the phase a mucus in a 15 liter stainless steel stirred tank. Then, a mixture of 400g and 800g of calcium carbonate powder of sorbitol and a foaming agent ointment C were added respectively, and after stirring well, the mixture was stirred well for 30 minutes, the liquid level was raised to a level lower than that without the inner core, and the mixture was left to stand overnight. Stirring to avoid sticking to wall, adding mixture of 150g sorbitol and 450g calcium carbonate powder, stirring for 20min, adding 90.0g herba Menthae essence, stirring for 10min, slowly adding guar gum ointment D phase, stirring thoroughly for 30min to form cream-like fine bright white paste, and standing overnight. After stirring, the liquid level of the paste falls down and does not adhere to the wall. Adding 200g of sorbitol and 800g of calcium carbonate powder, stirring for 30min after uniformly stirring, adding cellulose gum and coating E-phase emulsion, fully stirring for 20min after the addition is finished, and standing for one night. The stirring liquid level drops rapidly and does not adhere to the wall. Adding the mixture of 120g of sorbitol and 300g of calcium carbonate powder, fully stirring for 30min, adding the cellulose gum-coated W-phase emulsion, fully stirring for 45min after uniformly stirring, and standing. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the paste is very moist, smooth, fine, white and bright after the hollow holes are removed by manual stirring, and the solid state is kept well. The paste was divided into 59 toothpaste pieces of 150 g/piece, each containing 0.39mg of organic polyphosphate. The toothpaste is bright and fine, the extrusion is easy, the strip forming property of the toothpaste is good, the toothpaste does not flow and is good in fixation on a toothbrush, the taste is slightly spicy, the fragrance of flowers is good, the tongue is not spicy, the foam is very rich, the tooth brushing effect is good, and the mouth feel is very comfortable after tooth brushing. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] 25.0g of CMC powder was weighed into a beaker, and 93.0g of glycerol was added thereto and stirred to form a thin paste. To 1084.0g of organic cleaning agent with water-soluble amount of 23mg of organic polyphosphate, 6.0g of sodium chloride and 15.0g of sorbitol are added, and after stirring to form colorless transparent solution, the solution is poured into thin paste, and the transparent mucus is obtained by stirring while pouring.
[ preparation of foamer ointment C phase ] to a beaker of 176.0g of pure water, 176.0g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain an ointment.
[ preparation of outer guar gum D phase ] 12.0g of guar gum powder was weighed, 42.0g of glycerin was poured and stirred into a thin paste, and then 180.0g of pure water solution in which 15.0g of sodium bicarbonate was dissolved was poured and stirred, and an ointment was prepared.
[ preparation of the E phase of the outer-coated cellulose gum ] 15.0g of CMC powder was weighed, and 50.0g of glycerin and 12.0g of PEG400 were poured into the mixture and stirred well to prepare an emulsion.
[ preparation of the W phase of the outer-coated cellulose gum ] weighing 4.0g of CMC powder, pouring 15.0g of glycerol, stirring to form a thin paste, and then adding 6.0g of PEG400, and stirring fully to prepare emulsion.
The organic cleaning agent core, CMC inner bag, guar gum bag and CMC double outer bag are adopted for coating (CMC adding mode is 25+10+15+4), and a layer of outer bag is additionally arranged on the original basis, so that the core particles of the organic cleaning agent are thoroughly coated, the tension of the paste is further enhanced, and the instant explosive force during brushing is enhanced. The result shows that the paste obtained by double coating has finer appearance, better extrusion slivers, better paste dispersion and other using effects, and meets the expected presumption result.
Example 4
By the same operation as in example 2, an enclosed white paste was obtained from the phase a mucus in a 15 liter stainless steel stirred tank. Then, adding the mixture of 400g and 800g of the calcium carbonate powder and the foaming agent ointment C, stirring for 45min after uniformly stirring to form a brighter white emulsion, keeping the liquid level in a low position within 30min, indicating successful core-coating, and standing for one night. After stirring, the liquid level drops rapidly and does not adhere to the wall. A mixture of 150g of sorbitol and 450g of calcium carbonate powder was added and stirred for 20min. In order to cover the grass flavor of the peppermint water, the adding amount of the essence is increased to 98.0g of the mint essence, the mixture is stirred for 20min, the guar gum ointment D phase is slowly stirred and added, the mixture is stirred for 30min after uniform stirring, the fragrance is diluted, the paste is creamy and bright, and the mixture is left to stand for one night. The stirring drops without sticking to the wall. Adding the mixture of 250g of sorbitol and 750g of calcium carbonate powder, stirring for 20min, adding the cellulose gum-coated E-phase ointment, stirring uniformly, stirring thoroughly for 30min, and standing overnight. The stirring drops without sticking to the wall. After adding 120g of sorbitol and 400g of calcium carbonate powder and stirring for 20min, adding the emulsion of the cellulose gum outer coating W phase, fully stirring for 30min after the addition is finished, and standing for one night. After stirring, the liquid level falls down without sticking to the wall, 100g of sorbitol is added, stirring is carried out for 30min, and then 400.0 g of PEG is added, stirring is carried out for 15min, and standing is carried out. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the paste is very moist, bright, thin and white after the empty holes are removed by manual stirring, and the solid state is kept well. The paste was split into 61 toothpastes of 150 g/toothpaste, each containing 0.62mg of organic polyphosphate. The toothpaste is bright and fine, is easy to extrude, can not flow and solidify on a toothbrush, has slightly spicy and hot tooth brushing taste and grass smell, has very rich foam and good tooth brushing effect, and has sweet mouth body fluid after tooth brushing, and red and glossy gum. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before. After one year, the toothpaste tube is cut off to seal, and the paste is bright white and not dark.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] 25.0g of CMC powder was weighed into a beaker, to which 80.0g of glycerol was added and stirred to form a thin paste. A colorless transparent solution was prepared by stirring 6.0g of sodium chloride and 1084.0g of an organic cleaning agent having a water-soluble amount of 38mg of an organic polyphosphate, and then poured into a thin paste, followed by stirring and boiling to obtain a transparent mucus.
[ preparation of foamer ointment C phase ] to a beaker containing 176.0g of pure water, 176.0g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain an ointment.
Weighing 6.0g guar gum powder, pouring 30.0g glycerol, stirring to obtain a thin paste, pouring pure water at 70-80deg.C to soak herba Menthae to obtain 108.0g pale yellow solution with pH of 6-7, and stirring thoroughly to obtain pale yellow transparent ointment with slight grass smell.
[ preparation of the E phase of the outer-coated cellulose gum ] 15.0g of CMC powder was weighed, and 60.0g of glycerin was poured and stirred into a thin paste. 13.0g of PEG400, 15.0g of sodium bicarbonate and 15.0g of sorbitol were dispersed in 225.0g of pure water to prepare an aqueous solution, which was then poured into a thin paste and stirred well to prepare an ointment.
[ preparation of the W phase of the outer-coated cellulose gum ] 10.0g of CMC powder was weighed, and 15.0g of glycerol and 25.0g of PEG400 were poured into each powder, and the mixture was thoroughly stirred to prepare an emulsion.
The organic cleaning agent core, CMC inner bag, guar gum grass water bag and CMC double-layer bag are adopted for coating (CMC adding mode is 25+10+15+10), and the result shows that the paste grass water obtained by the multiple coating operation is small in water content, good in washing dispersibility, and good in gum maintenance effect besides cleaning.
Example 5
By the same operation as in example 2, an enclosed white paste was obtained from the phase a mucus in a 15 liter stainless steel stirred tank. Then, a mixture of 400g and 800g of calcium carbonate powder and foaming agent ointment C were added, and after stirring well, the mixture was stirred for 45 minutes to give a brighter white emulsion, and left to stand overnight. After stirring, the liquid level drops rapidly and does not adhere to the wall. A mixture of 200g of sorbitol and 600g of calcium carbonate powder was added and stirred for 30min. 86.0g of the mint essence for flowers is added, after stirring for 10min, the guar gum ointment D phase is slowly added after stirring, after stirring uniformly, the flavor is lightened, the ointment is creamy and bright, and the mixture is left to stand for one night. The stirring drops without sticking to the wall. Adding the mixture of 300g of sorbitol and 900g of calcium carbonate powder, stirring for 30min, adding the cellulose gum-coated E-phase ointment, stirring uniformly, stirring thoroughly for 30min, and standing overnight. The stirring liquid level does not drop basically. After adding a mixture of 120g of sorbitol and 100g of calcium carbonate powder and stirring for 20min, adding the emulsion of the cellulose gum outer coating W phase, stirring fully for 30min and standing overnight. After stirring, the liquid level falls down without sticking to the wall, and stirring is continued for 30min. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the paste is very moist, bright, thin and white after the empty holes are removed by manual stirring, and the solid state is kept well. The paste was split into 61 toothpastes of 150 g/toothpaste, each containing 0.30mg of organic polyphosphate. The paste is bright and fine, is easy to extrude, does not flow and is good in solidification on a toothbrush, the mouth feel is fragrant, sweet, warm and moist, the tongue is not hot, the mouth cavity has the feeling of promoting the production of body fluid and restoring the mind after brushing teeth, and the toothbrush is very comfortable and has good brushing effect. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] 25.0g of CMC powder was weighed into a beaker, 86.0g of glycerol was added thereto and stirred to form a thin paste. A colorless transparent solution was prepared by stirring 6.0g of sodium chloride, 15g of sorbitol and 1086.0g of an organic cleaning agent having a water-soluble amount of 18mg of an organic polyphosphate, and then poured into a thin paste, followed by stirring while pouring, and decocting to obtain a transparent mucus.
[ preparation of foamer ointment C phase ] to a beaker containing 176.0g of pure water, 176.0g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain an ointment.
[ preparation of outer guar D phase ] 9.0g of guar powder was weighed, and 33.0g of glycerin was poured and stirred into a thin paste. 15.0g of sorbitol is taken and dispersed in 105.0g of Yunnan Wei Dong tea soup to prepare an aqueous solution, the aqueous solution is poured into thin paste, 12.0g of PEG400 is added, and the mixture is fully stirred to prepare the ointment.
[ preparation of the E phase of the outer-coated cellulose gum ] 5.0g of CMC powder was weighed, and 20.0g of glycerin was poured and stirred into a thin paste. 15.0g of sodium bicarbonate is dispersed in 80.0g of Yunnan Wei Dong tea soup to prepare an aqueous solution, and then the aqueous solution is poured into the thin paste and fully stirred to prepare the ointment.
[ preparation of the W phase of the outer-coated cellulose gum ] 20.0g of CMC powder was weighed, and 60.0g of glycerin and 10.0g of PEG400 were poured into each powder, and the mixture was thoroughly stirred to prepare an emulsion.
Wei Dongcha cultivated by Yunnan ancient tree is selected, branches and leaves are large, the body fluid is produced, the mind is recovered, and the body can be heated and active after 200 milliliters of tea water is drunk. Taking drinkable tea soup with tea aroma, using the tea soup for toothpaste production, and coating by adopting the modes of organic cleaning agent core, CMC inner package, guar gum tea water package and CMC double-layer package (CMC adding mode 25+10+5+20). The result shows that the paste obtained by coating the tea has rich taste for promoting the production of body fluid and returning to mind when brushing teeth, and the oral cavity is very comfortable on the basis of sweet and warm taste.
Example 6
By the same operation as in example 2, an enclosed white paste was obtained from the phase a mucus in a 15 liter stainless steel stirred tank. Then, a mixture of 400g and 800g of calcium carbonate powder and foaming agent ointment C were added, and after stirring well, the mixture was stirred for 45 minutes to give a brighter white emulsion, and left to stand overnight. After stirring, the liquid level drops rapidly and does not adhere to the wall. A mixture of 200g of sorbitol and 600g of calcium carbonate powder was added and stirred for 30min. Adding 90.0g of the mint essence, stirring for 10min, slowly stirring, adding the guar gum ointment D phase, stirring for 30min, keeping the paste bright like cream, and standing overnight. The stirring drops without sticking to the wall. Adding the mixture of 300g of sorbitol and 600g of calcium carbonate powder, stirring for 30min, adding the cellulose gum-coated E-phase ointment, stirring uniformly, stirring thoroughly for 30min, and standing overnight. The stirring liquid level does not drop basically. After adding a mixture of 120g of sorbitol and 100g of calcium carbonate powder and stirring for 20min, adding the emulsion of the cellulose gum outer coating W phase, stirring fully for 30min and standing overnight. After stirring, the liquid level falls down without sticking to the wall, and stirring is continued for 30min. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the paste is very moist, bright, thin and white after the empty holes are removed by manual stirring, and the solid state is kept well. The paste was split into 60 toothpaste pieces of 150 g/piece, each containing 1.30mg of organic polyphosphate. The paste is bright and fine, is easy to extrude, does not flow and is good in solidification on a toothbrush, the mouth feel is fragrant, sweet, warm and moist, the tongue is not hot, the mouth cavity has the feeling of promoting the production of body fluid and restoring the mind after brushing teeth, and the toothbrush is very comfortable and has good brushing effect. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] 25.0g of CMC powder was weighed into a beaker, to which 80.0g of glycerol was added and stirred to form a thin paste. A colorless transparent solution was prepared by stirring 6.0g of sodium chloride, 15g of sorbitol and 1086.0g of an organic cleaning agent having a water-soluble amount of 78mg of an organic polyphosphate, and then poured into a thin paste, followed by stirring while pouring, and decocting to obtain a transparent mucus.
[ preparation of foamer ointment C phase ] to a beaker containing 176.0g of pure water, 176.0g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain an ointment.
[ preparation of outer guar D phase ] 9.0g of guar powder was weighed, and 41.0g of glycerin was poured and stirred into a thin paste. 10.0g of sodium bicarbonate is dispersed in 125.0g of peppermint water to prepare an aqueous solution, the aqueous solution is poured into thin paste, 12.0g of PEG400 is added, and the mixture is fully stirred to prepare the ointment.
[ preparation of the E phase of the outer-coated cellulose gum ] 10.0g of CMC powder was weighed, and 38.0g of glycerin was poured and stirred into a thin paste. 5.0g of sodium bicarbonate is dispersed in 66.0g of Yunnan Wei Dong tea soup to prepare an aqueous solution, and then the aqueous solution is poured into the thin paste and fully stirred to prepare the ointment.
[ preparation of the W phase of the outer-coated cellulose gum ] 15.0g of CMC powder was weighed, and 49.0g of glycerol and 10.0g of PEG400 were poured into each powder, and the mixture was thoroughly stirred to prepare an emulsion.
For paste with higher organic cleaning agent content, the result of coating by adopting the forms of organic cleaning agent core, CMC inner bag, guar gum herb water bag, CMC tea water bag and CMC outer bag (CMC adding mode 25+10+10+15) shows that the paste obtained by repeatedly coating grass water and tea water has better dry taste, and the mouth feel is very comfortable on the basis of sweet and warm taste after brushing teeth.
The functional toothpaste prepared by the embodiment meets the requirements of the GB8372-2008 toothpaste on the sanitary index, the content of harmful substances such as lead and arsenic is limited, and the microbial index meets the national standard, and the specific detection report content is shown as follows.
Figure BDA0004144147390000181
Comparative example 1
To a colorless mucilage A phase in a 15 liter stainless steel stirred tank, 448mg of the Chinese medicinal extract was added and stirred to form a transparent brown mucilage. 1300g of sorbitol is added, and after being stirred uniformly, 1000g of calcium carbonate powder is added, and the mixture is stirred for 30min to obtain white emulsion. Then adding the syrup B phase, stirring uniformly, adding 2000g of calcium carbonate powder, stirring for 1.0 hour, adding 92g of glycerol, stirring for 20 minutes, adding the colorless ointment C phase, and stirring thoroughly to obtain the ointment with bright white and fine oil. A mixture of 200g of sorbitol and 800g of calcium carbonate powder was added and stirred for 30min and allowed to stand overnight. After stirring uniformly, 120g of black peppermint essence in yellow liquid is added, and the mixture is stirred uniformly to give out strong fragrance. Then, 12.0g of cellulose gum powder was added with slow stirring, and after the fragrance was gradually diluted, 200g of sorbitol was added and stirred until the paste surface was bright white and fine, and left to stand overnight. The paste was stirred to be smooth but slightly refluxed, and 100g of calcium carbonate and 6.0g of cellulose gum were added, followed by stirring for 10 minutes and standing. The paste is decompressed, stored and deaerated. After the paste is restored to normal temperature and normal pressure, the white paste with bright, fine and solid good is displayed by manually stirring and removing the empty holes. The paste is divided into 64 toothpaste of 126 g/branch. The paste is bright and fine, is easy to extrude, has a little flow on a toothbrush, has mild taste, does not feel spicy on the tongue, and has good tooth brushing effect. The toothpaste extrusion is still easy for more than six months, the paste is bright, white and fine, but the color is slightly dark, and the tooth brushing effect is still good. Cut the toothpaste tube to seal, the upper part of the paste floats with a layer of yellow oily matter with flavor of essence.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] to 1500mL of organic cleaning agent with water-soluble amount of 12mg of organic polyphosphate, 6.0g of sodium chloride is added, stirred and dissolved, then 30g of CMC powder is added for dispersion and soaking, and the mixture is heated and decocted into mucus.
[ preparation of sweetener B phase ] 750g of white granulated sugar is weighed and put into a big beaker, and 440g of purified water is added to be decocted into a light yellow transparent sugar water solution.
[ preparation of foamer ointment C phase ] to a beaker containing 150g of purified water, 148g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain a colorless and transparent ointment.
In general, at least two kinds of glues are needed for preparing the toothpaste, otherwise, the stability of a paste system is difficult to ensure, and the result of comparative example 1 proves that the dynamic balance of the toothpaste body is difficult to maintain by using a single glue. Therefore, the strategy of combining CMC and hydroxypropyl guar is selected in the construction of the organic cleaning agent paste. Guar gum has a chemical structure which is distinct from streamline CMC, and has a branch-fork-like molecular structure, so that essence molecules can be encapsulated in multiple directions and angles.
Comparative example 2
320mg of the Chinese herbal extract was added to the colorless mucilage A phase in a 15 liter stainless steel stirred tank, and stirred to form a clear brown mucilage. 1000g of sorbitol is added, and after being stirred uniformly, 600g of calcium carbonate powder is added, and the mixture is stirred for 15min to obtain white emulsion. Then adding syrup B, stirring uniformly, adding 2000g of calcium carbonate and 200g of sorbitol, stirring for 50min, and standing overnight. Stirring to form uniform white emulsion, adding 200g of sorbitol and 800g of calcium carbonate powder, adding foaming agent ointment C, stirring for 15min, and standing overnight. Adding a mixture of 300g of sorbitol and 500g of calcium carbonate powder, adding 118g of black peppermint essence, stirring for 15min, and giving out strong fragrance. Then slowly stirring, adding guar gum ointment D phase, stirring for 30min, and standing overnight. The paste is bright and fine like cream after stirring, CMC glue ointment E phase is slowly added, and 100g of sorbitol, 300g of calcium carbonate powder mixture and 400 g of PEG are respectively added, and after stirring uniformly, stirring is carried out for 30min and standing is carried out for one night. After stirring, the paste was somewhat diluted, a mixture of 280g of sorbitol and 320g of calcium carbonate powder was added, and the mixture was stirred for 30min and allowed to stand overnight. The paste is stored under reduced pressure for two days. After the paste is restored to normal temperature and normal pressure, the white paste with bright, fine and soft hollow holes but good solid is obtained by manually stirring and removing the hollow holes. The paste was divided into 63 toothpaste pieces of 150 g/piece, each containing 0.51mg of organic polyphosphate. The paste is bright and fine, is easy to extrude, does not flow and solidify on a toothbrush, has good taste, is comfortable and does not feel spicy to the tongue, and has good tooth brushing effect. After more than six months, the extrusion is still easy, the tooth brushing effect is good, the toothpaste tube is cut off, the paste is bright and fine, and no yellow oily matter is found. After one and a half years, the toothpaste tube is cut off to seal, the toothpaste is slightly dark, and a trace amount of yellow oily matter floats out, and the toothpaste can still be extruded, but the taste and the tooth brushing effect are far less good than those of the examples.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] 30.0g of CMC powder was weighed into a beaker, and 120.0g of glycerin was added thereto and stirred to form a thin paste. 1100g of organic cleaning agent with water-soluble amount of 32mg of organic polyphosphate dissolved in 6.0g of sodium chloride is poured into the thin paste, and the paste is formed by stirring while pouring, and then heated and boiled into mucus.
[ preparation of sweetener B phase ] 600g of white granulated sugar is weighed and put into a beaker, 400g of purified water is added, and the mixture is boiled into a sugar water solution.
[ preparation of foamer ointment C phase ] to a beaker of 150g of pure water, 148g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain an ointment.
[ preparation of the outer guar gum D phase ] 5.0g of guar gum powder was weighed, 100.0g of glycerin was poured and stirred into a thin paste, and then 112.0g of pure water solution in which 10.0g of sodium bicarbonate was dissolved was poured and stirred, and decocted into a pale yellow ointment.
[ preparation of the E phase of the outer-coated cellulose gum ] 15.0g of CMC powder was weighed, 100.0g of glycerin was poured and stirred into a thin paste, and then 300.0g of pure water solution in which 5.0g of sodium bicarbonate was dissolved was added and stirred, and heated and decocted into an ointment.
Experimental results on the addition sequence of the two CMC gums and the hydroxypropyl guar gum and the glue input mode show that the softness of the paste obtained by coating the double glue is obviously improved compared with that of the paste obtained by coating the single CMC, and the effect of the guar gum coating essence can completely prevent oily matters from floating and dissociating according to the use amount and the cooperation of the guar gum coating essence and the CMC gum. The results show that 5.0g guar gum +15.0g CMC in the case of 60 counts, 150 g/count, is not sufficient to encapsulate the perfume. The amount of hydroxypropyl guar used should be kept at a standard of not less than 6.0g, i.e. not less than 0.1g per count.
Comparative example 3
To a colorless mucilage A phase in a 15 liter stainless steel stirred tank, 448mg of the Chinese medicinal extract was added and stirred to form a transparent brown mucilage. After adding 800g of sorbitol and stirring uniformly, a mixture of 200g of sorbitol and 800g of calcium carbonate powder is added and stirred for 20min to form white emulsion. Then, adding syrup B phase, stirring uniformly, adding 200g of sorbitol and 1000g of calcium carbonate powder mixture, stirring for 30min to form white emulsion, and standing overnight. Scraping possible adhesive on the inner wall of the stainless steel kettle by using a silica gel shovel, fully stirring to uniformly mix the emulsion, adding a mixture of 300g of sorbitol and 1200g of calcium carbonate powder, adding a foaming agent ointment C, uniformly stirring, stirring for 30min, and standing overnight. After stirring, the liquid level rapidly drops, 110g of black peppermint essence is added, after stirring for 15min, guar gum ointment D phase is slowly added, the fragrance is lightened, and after stirring uniformly, stirring for 15min is carried out for standing overnight. After stirring, the liquid level of the paste falls, the paste is not sticky and thin, a mixture of 200g of sorbitol and 600g of calcium carbonate powder is added, stirring is carried out for 20min, then the phase of the external ointment E is slowly added, stirring is carried out for 20min, and standing is carried out for one night. The stirring liquid level is slightly dropped, a mixture of 200g of sorbitol and 600g of calcium carbonate powder is added, and after being stirred uniformly, 20.0g of PEG is added, and after being stirred uniformly, the mixture is stirred for 30min and then is stood for one night. The paste drops obviously after stirring, is white and bright and fine like cream, has a little wall sticking, and is added with 60g of sorbitol and stirred for 20min for standing overnight. Stirring and dropping, no sticking to wall, fine and smooth paste, and vacuum storing. After the paste is restored to normal temperature and normal pressure, the paste is moist, bright, thin and white after the empty holes are removed by manual stirring, and the solid state is kept well. The paste was split into 61 toothpastes of 150 g/toothpaste, each containing 0.41mg of organic polyphosphate. The paste is bright and fine, the extrusion is easy, the solid on the toothbrush is good, the mouth feel is slightly sweet and not spicy, the foam is very rich, the tooth brushing effect is good, and the body fluid in the oral cavity returns sweet after tooth brushing. The toothpaste tube is cut off for sealing after more than six months, and the toothpaste is bright and moist as before. After one year, the paste was difficult to extrude, small particles with obvious touch were formed in the paste, the toothpaste tube was cut open, no oily substance was found on the surface of the paste, but the paste was darker than the paste of comparative example 1, and had darker color and more unpleasant smell.
The preparation method of various reagents comprises the following steps:
[ preparation of cellulose gum A phase ] A colorless transparent aqueous solution was obtained by adding 6.0g of sodium chloride to 1087.0g of an organic cleaning agent having a water-soluble amount of 25mg of an organic polyphosphate and stirring and dissolving the mixture. Then 25.0g CMC powder is added, stirred and dispersed, and heated and decocted into mucus.
Preparation of sweetener B phase 575.0g of white granulated sugar is weighed and put into a beaker, and 370.0g of purified water is added to be decocted into a light yellow transparent syrup solution.
[ preparation of foamer ointment C phase ] to a beaker of 176.0g of pure water, 176.0g of sodium dodecyl sulfate was added, and the mixture was heated and decocted to obtain a colorless and transparent ointment.
[ preparation of outer guar gum D phase ] 5.0g of guar gum powder was weighed, 90.0g of glycerin was poured and stirred into a thin paste, and then 118.0g of pure water solution in which 10.0g of sodium bicarbonate was dissolved was poured and stirred, and an ointment was prepared.
[ preparation of the E phase of the outer-coated cellulose gum ] 15.0g of CMC powder was weighed, and 124.0g of glycerin was poured to cover the powder and stirred into a thin paste. 275.0g of pure water solution in which 20.0g of sodium bicarbonate was dissolved was poured into the thin paste and stirred, and then 20.0g of PEG400 was added thereto and stirred well, and then decocted to an ointment.
Under the conditions of preparing 60 toothpaste and 150 g/branch, adopting CMC (CMC) coating form of 5.0g guar gum plus 15.0g, and adding PEG400, the obtained paste can also wrap essence, which indicates that the PEG400 can modify a glue layer to a certain extent. However, the shortage of glue also causes calcium ion aggregation, and hard particles with larger and smaller sizes are deposited in the paste, so that the paste is difficult to extrude. Thus, CMC should be used in an amount of at least 0.8 g/min to ensure the stability of the paste system.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, which is defined broadly in the appended claims, and any person skilled in the art to which the invention pertains will readily appreciate that many modifications, including those that fall within the metes and bounds of the claims, or equivalence of such metes and bounds thereof.

Claims (13)

1. The functional toothpaste is characterized in that raw materials for preparing the functional toothpaste comprise an organic cleaning agent, an abrasive, a humectant, a foaming agent, cellulose gum, guar gum and an astringent.
2. The functional toothpaste of claim 1, wherein the raw materials further comprise a sweetener; and/or fragrances; and/or a pH adjuster; and/or a preservative.
3. The functional toothpaste according to claim 1, wherein said material further comprises other active substances.
4. A method of preparing a functional toothpaste according to any one of claims 1 to 3, said method comprising the steps of:
(1) Mixing an organic cleaning agent and cellulose gum to form a mucus A phase;
(2) Forming a nucleus;
(3) Wrapping with guar gum phase to form paste;
(4) Use of a cellulosic gum coating phase to repack the toothpaste to provide a functional toothpaste as claimed in any one of claims 1 to 3.
5. The method of preparing of claim 4, wherein the step of forming the core-envelope comprises:
mixing mucus A phase, humectant, abrasive, sweetener B phase and foaming agent C phase; or (b)
Mixing mucus A phase, humectant, abrasive, sweetener B phase, fiber gum inner wrapping phase and foaming agent C phase.
6. The method according to claim 5, wherein the sweetener B phase is obtained by mixing a sweetener and water.
7. The process according to claim 5, wherein the foaming agent C phase is obtained by mixing water and a foaming agent.
8. The method according to claim 5, wherein the cellulose gum inclusion phase is obtained by mixing cellulose gum, humectant and water.
9. The method of claim 4, wherein step (3) comprises mixing the core body with guar gum to obtain a paste.
10. The method according to claim 4 or 9, wherein the guar phase is obtained by mixing guar with water.
11. The method of claim 4, wherein step (4) comprises mixing the paste obtained in step (3), a cellulose gum outer phase, and one or more of the following to obtain the functional toothpaste: moisturizing agents, abrasives, astringents.
12. The method according to claim 4 or 11, wherein the cellulose gum outer phase is obtained by mixing cellulose gum, an astringent agent and water.
13. The method of claim 4, wherein the cellulose gum cover in step (4) is wrapped 1, 2 or 3 layers.
CN202310296177.XA 2023-03-23 2023-03-23 Functional toothpaste and preparation method thereof Pending CN116392410A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101703596A (en) * 2009-10-15 2010-05-12 江苏华荣生物科技有限公司 Medicinal liquor for treating pains and other diseases caused by hyperosteogeny
CN102101905A (en) * 2009-12-16 2011-06-22 华东理工大学 Preparation method of organic polyphosphate
CN103998017A (en) * 2011-12-20 2014-08-20 狮王株式会社 Dentrifice composition
CN104606102A (en) * 2015-01-26 2015-05-13 柳州师范高等专科学校 Toothpaste for eliminating bad breath
CN105534866A (en) * 2016-01-25 2016-05-04 陈威宇 Preparation method of multiple-effect toothpaste capable of removing stains and conducting maintenance
CN107095827A (en) * 2017-06-30 2017-08-29 合肥卓畅农业科技有限公司 One kind is antibacterial to remove stain Chinese medicinal toothpaste and preparation method thereof
CN109528513A (en) * 2018-12-29 2019-03-29 拉芳家化股份有限公司 It is a kind of without abrasion whitening toothpaste
CN115487105A (en) * 2021-12-07 2022-12-20 象记(上海)生物科技有限公司 Chinese herbal medicine toothpaste capable of refreshing breath and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101703596A (en) * 2009-10-15 2010-05-12 江苏华荣生物科技有限公司 Medicinal liquor for treating pains and other diseases caused by hyperosteogeny
CN102101905A (en) * 2009-12-16 2011-06-22 华东理工大学 Preparation method of organic polyphosphate
CN103998017A (en) * 2011-12-20 2014-08-20 狮王株式会社 Dentrifice composition
CN104606102A (en) * 2015-01-26 2015-05-13 柳州师范高等专科学校 Toothpaste for eliminating bad breath
CN105534866A (en) * 2016-01-25 2016-05-04 陈威宇 Preparation method of multiple-effect toothpaste capable of removing stains and conducting maintenance
CN107095827A (en) * 2017-06-30 2017-08-29 合肥卓畅农业科技有限公司 One kind is antibacterial to remove stain Chinese medicinal toothpaste and preparation method thereof
CN109528513A (en) * 2018-12-29 2019-03-29 拉芳家化股份有限公司 It is a kind of without abrasion whitening toothpaste
CN115487105A (en) * 2021-12-07 2022-12-20 象记(上海)生物科技有限公司 Chinese herbal medicine toothpaste capable of refreshing breath and preparation method thereof

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