CN107184473B - Toothpaste containing spina gleditsiae extract and preparation method thereof - Google Patents

Toothpaste containing spina gleditsiae extract and preparation method thereof Download PDF

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CN107184473B
CN107184473B CN201710413997.7A CN201710413997A CN107184473B CN 107184473 B CN107184473 B CN 107184473B CN 201710413997 A CN201710413997 A CN 201710413997A CN 107184473 B CN107184473 B CN 107184473B
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toothpaste
spina gleditsiae
parts
sodium
agent
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CN107184473A (en
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牛江秀
娄新华
张岩松
王素军
陈洪
王立业
押辉远
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ZHUHAI SHANGER BIOLOGICAL TECHNOLOGY CO LTD
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Luoyang Normal University
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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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/483Gleditsia (locust)
    • 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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Abstract

A toothpaste containing spina Gleditsiae extract and its preparation method are provided. The toothpaste comprises the following components in parts by weight: 0.5-8 parts of spina gleditsiae extract; 10-30 parts of a wetting agent; 15-45 parts of a friction agent; 0.5-1.5 parts of foaming agent; 0.4-1.6 parts of adhesive; 0.15-0.3 part of stabilizer; 0.2-0.8 part of sweetening agent. The toothpaste provided by the invention has the effects of inhibiting the breeding of oral bacteria and preventing various oral diseases.

Description

Toothpaste containing spina gleditsiae extract and preparation method thereof
Technical Field
The invention belongs to the technical field of toothpaste, and particularly relates to toothpaste containing spina gleditsiae extract and having a health-care effect on tooth and oral diseases and a preparation method thereof.
Background
Toothpaste is a common oral care product for people, and has the main functions of cleaning teeth and keeping the oral cavity clean. With the acceleration of modern life rhythm, eating habits change, and the incidence rate of oral diseases is higher and higher, wherein a series of tooth and oral problems such as periodontitis, caries, dental plaque, dentinal hypersensitivity, halitosis, oral ulcer and the like caused by the breeding of bacteria attached to gingiva and oral cavity are frequently encountered diseases and common diseases in the oral diseases, and the health and the confidence of people are seriously influenced. Therefore, inhibition of growth of pathogenic bacteria in the oral cavity is an important measure for prevention and protection of teeth and prevention of oral diseases.
With the increasing awareness of environmental protection and oral health care, the demand of consumers has been far from being satisfied by common toothpaste aiming at cleaning teeth in domestic and foreign markets, and thus functional toothpaste having the effects of preventing and health care of oral diseases has been gradually developed. Most oral care products with antibacterial effect in the current market are added with chemical synthetic components, and can cause certain threat to oral health after long-term use. The Chinese herbal medicine extract has incomparable advantages of natural, environment-friendly and safe chemical synthesis medicines, and in addition to the green and natural advocation of people, the functional toothpaste taking the Chinese herbal medicine extract as the effective component gradually receives the favor of consumers, and the demand is increasing day by day, so that the functional toothpaste becomes the mainstream of the development of the toothpaste market.
Chinese honeylocust fruit, also known as Chinese honeylocust tree, is one of the unique tree species of Gleditsia of Caesalpiniaceae, grows vigorously and is a male and female variant, and the female tree has strong pod bearing capacity. The saponaria officinalis is a natural raw material of medical food, health products, cosmetics and washing products; the gleditsia sinensis seeds can eliminate food stagnation, promote digestion and stimulate appetite, and contain a vegetable gum (guar gum) which is an important strategic raw material; the gleditschia horrida (spina gleditsiae) contains flavonoid glycoside, phenols and amino acid and has high economic value. Because of the high utilization value of the saponin, the research on the saponin is more and more, for example, CN 102302435A discloses a saponin hair conditioner, CN 105063641A discloses a saponin derusting liquid, and CN 106177870A discloses a saponin thorn combined medicine and the like.
Spina Gleditsiae (also called spina Gleditsiae) is the spine of Gleditsia sinensis (L.) Abel of Leguminosae. The spina Gleditsiae extract contains flavonoids, phenols, amino acids, etc., and has antibacterial, antiinflammatory, and antiallergic effects. The prior literature reports that the saponin extract has obvious bacteriostatic action (Liujiajian et al, research on the in-vitro bacteriostatic and bactericidal action of the saponin extract [ J ], (pharmaceutical guidance, 2013, 32(3): 300-301)), which lays a foundation for the application of the saponin in oral care products and makes the saponin have the prospect of preparing the saponin toothpaste. However, no traditional Chinese medicine toothpaste taking the spina gleditsiae extract as a main functional component exists at present through search, and the extraction method of the spina gleditsiae extract is still to be further improved.
Disclosure of Invention
Therefore, an object of the present invention is to provide a toothpaste containing an extract of spina gleditsiae, which has the effects of inhibiting the growth of oral bacteria and preventing various oral diseases.
In order to achieve the purpose, the invention adopts the following technical scheme:
the toothpaste containing the spina gleditsiae extract comprises the following components in parts by weight: 0.5-8 parts of spina gleditsiae extract; 10-30 parts of a wetting agent; 15-45 parts of a friction agent; 0.5-1.5 parts of foaming agent; 0.4-1.6 parts of adhesive; 0.15-0.3 part of stabilizer; 0.2-0.8 part of sweetening agent.
Water and other conventional adjuvants such as flavors, colorants, preservatives, and the like may be added to the toothpaste of the present invention as desired.
Preferably, the toothpaste comprises the following components in parts by weight: 0.5-8 parts of spina gleditsiae extract; 10-30 parts of a wetting agent; 15-45 parts of a friction agent; 0.5-1.5 parts of foaming agent; 0.4-1.6 parts of adhesive; 0.15-0.3 part of stabilizer; 0.2-0.8 part of sweetening agent; a proper amount of water and a small amount of edible essence.
Preferably, the spina gleditsiae extract is prepared according to the following steps:
(1) drying spina Gleditsiae, pulverizing, sieving, and collecting the undersize product to obtain spina Gleditsiae coarse powder;
(2) adding ethanol into the spina gleditsiae coarse powder obtained in the step (1), soaking, heating, refluxing, extracting and concentrating;
(3) decolorizing the concentrated solution, and vacuum freeze drying to obtain spina Gleditsiae extract.
The method adopts ethanol as an extraction solvent, can effectively extract the antibacterial active ingredients in the spina gleditsiae, has simple extraction method and high efficiency, is easy to recycle the ethanol, and is beneficial to the industrial production of the spina gleditsiae extract.
Preferably, in step (1), the spina gleditsiae is cut into pieces, preferably washed in advance.
Preferably, the temperature of the drying is 50 to 70 ℃, preferably 60 ℃.
Preferably, the drying is oven drying to constant weight. Drying may be carried out in a drying oven.
Preferably, the sieve is a 50-60 mesh sieve.
Preferably, the ethanol in step (2) is aqueous ethanol, preferably 75% ethanol.
Preferably, the mass ratio of the spina gleditsiae coarse powder to the ethanol is 1:5-20, and preferably 1: 10.
Preferably, the soaking time is 6-12 h.
Preferably, the temperature of the heating reflux extraction is 80-120 ℃, preferably 100 ℃, and the time of the heating reflux extraction is more than 0.5h, preferably 1-3 h.
Preferably, extracting for 2-3 times, filtering and mixing extractive solutions.
Preferably, the concentration is carried out at 50-80 ℃, preferably 70 ℃. Concentration can be carried out using a rotary evaporator.
Preferably, the decolorization in step (3) is performed using activated carbon.
Preferably, the temperature of the cold trap of the vacuum freeze drying is-40 to-65 ℃, preferably-55 ℃, and the vacuum degree is 1500-3000Pa, preferably 2000 Pa.
Preferably, the humectant includes but is not limited to one or more of propylene glycol, sorbitol, glycerin, glycerol, and polyethylene glycol.
Preferably, the abrasive includes, but is not limited to, one or more of calcium hydrogen phosphate, silica, calcium carbonate, aluminum hydroxide, heavy calcium carbonate, light calcium carbonate, calcite powder, and chlorite.
Preferably, the foaming agent comprises one or more of sodium lauryl sulfate, sodium N-lauroyl sarcosinate and sodium methyl cocoyl taurate.
Preferably, the binding agent includes but is not limited to one or more of sodium alginate, sodium carboxymethylcellulose, xanthan gum, hydroxyethyl cellulose, guar gum, acacia gum and carrageenan.
Preferably, the stabilizer is sodium pyrophosphate.
Preferably, the sweetening agent comprises one or more of saccharin sodium, sucrose, xylitol, sodium cyclamate and sodium diaminate.
Preferably, the edible essence includes, but is not limited to, one or more of menthol, spearmint oil, perilla oil, lemon oil, orange oil, clove oil, cinnamon oil, orange oil, peppermint oil, borneol, vanillin, citral and lauraldehyde.
Preferably, the water is one or two of purified water or deionized water.
One of the purposes of the invention is also to provide a preparation method of the toothpaste, which comprises the following steps:
(1) dissolving spina Gleditsiae extract, wetting agent, foaming agent and stabilizer in water, mixing, heating to obtain gel in the form of uniform semitransparent viscous liquid, and standing to dissolve and expand;
(2) cooling the colloid obtained in the step (1) to 50-90 ℃, sequentially adding a friction agent, an adhesive and a sweetening agent, and continuously stirring to uniformly mix various materials;
(3) cooling the colloid to below 45 deg.C, adding other adjuvants such as edible essence, stirring, and making into paste with certain viscosity and proper consistency;
(4) grinding the paste, grinding the coarse and hard particles to make the paste fine, uniform and stable, vacuum degassing, standing, and sterilizing to obtain the toothpaste.
Preferably, the mixing in step (1) is carried out in a blender.
Preferably, the heating is carried out in an azeotrope kettle.
Preferably, the mixture is heated to 75-100 ℃ and left for more than 0.5h, preferably 1-2 h.
Preferably, the cooling in step (2) is to a temperature of 65 to 70 ℃.
Preferably, the adding of the abradant, the binding agent and the sweetener is carried out under stirring, and the rotation speed of the stirring is preferably 300-320 r/min.
Preferably, the stirring is continued for more than 0.5h, preferably 1-2h, at a rotation speed of 350-.
Preferably, the grinding in step (4) is performed by a grinder.
Preferably, grinding is carried out twice, the materials are naturally cooled to normal temperature after being ground for the first time and stored and aged, meanwhile, the materials are fully expanded to form homogeneous adhesive bodies, the elasticity of the materials is improved, and vacuum degassing is carried out after the grinding for the second time.
Preferably, aging is for 1 hour or more, preferably for 2 hours.
Preferably, the degassing is carried out for about 40-60min until the vacuum degree reaches-0.096 MPa or less.
Preferably, the standing time is 2-4 h.
The invention adds spina gleditsiae extract as an effective component into toothpaste, has obvious anti-inflammatory, antibacterial and antiallergic effects, can be used for preventing and treating periodontitis, gingivitis, stomatitis, oral ulcer and the like, and reduces oral diseases.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
Example 1
The traditional Chinese medicine toothpaste containing the spina gleditsiae extract comprises the following components in parts by weight: 1 part of spina gleditsiae extract; 20 parts of a wetting agent; 20 parts of a friction agent; 1.2 parts of a foaming agent; 1 part of adhesive; 0.2 part of a stabilizer; 0.5 part of a sweetening agent; a proper amount of water and a small amount of edible essence.
The spina gleditsiae extract is prepared according to the following steps:
(1) taking sliced spina gleditsiae, cleaning, drying by a drying oven at 60 ℃ to constant weight, crushing, sieving by a 40-mesh sieve, and taking undersize products to obtain spina gleditsiae coarse powder;
(2) mixing spina gleditsiae coarse powder according to the mass ratio of 1:10 soaking in 75% ethanol for 8h, heating and reflux-extracting at 100 deg.C for 3h, extracting for 3 times, filtering, mixing extractive solutions, and concentrating with rotary evaporator (70 deg.C);
(3) decolorizing the concentrated solution with active carbon, vacuum freeze drying at-55 deg.C under vacuum degree of 2000Pa, and drying to obtain spina Gleditsiae extract.
The preparation method of the traditional Chinese medicine toothpaste containing the spina gleditsiae extract comprises the following steps:
(1) dissolving spina gleditsiae extract 1 part, propylene glycol 20 parts, sodium lauryl sulfate 1.2 parts and sodium pyrophosphate 0.2 part in deionized water, stirring uniformly in a mixer, putting into an azeotropic boiler, heating to 85 ℃, so that the prepared colloid is in a uniform, semitransparent and viscous liquid state, and then standing for 2 hours to be fully dissolved and expanded for use;
(2) cooling the colloid obtained in the step (1) to 65 ℃, putting an azeotropic pot on a stirrer, sequentially adding 20 parts of calcium hydrophosphate, 1 part of sodium alginate and 0.5 part of saccharin sodium while stirring (the rotating speed is 320r/min), and continuously stirring for 2 hours (the rotating speed is 360r/min) to uniformly mix various materials;
(3) cooling the colloid to below 45 deg.C, adding a small amount of Mentholum, mechanically mixing and stirring to obtain ointment with certain viscosity and proper consistency;
(4) grinding paste by a grinder, grinding coarse and hard particles to make the paste fine, uniform and stable, grinding twice, storing and aging for 1h after the first grinding, and vacuum degassing after the second grinding until the vacuum degree reaches-0.096 MPa for 60 min;
(5) degassing the paste, standing for 4h, sterilizing, filling into a hose, and sealing to obtain the final product of spina Gleditsiae extract toothpaste.
The main quality index evaluation and bacteriostatic effect test of the toothpaste prepared in this example are as follows:
1. determination of toothpaste appearance, physicochemical index and sanitary index
Taking 4 toothpaste samples, storing 1 toothpaste sample at room temperature, putting the other 3 toothpaste samples into a refrigerator at minus 8 +/-1 ℃, taking out after 8 hours, immediately putting into a constant-temperature incubator at 45 +/-1 ℃, taking out after 8 hours, recovering to room temperature, opening a cover for observation, and enabling the toothpaste body not to overflow out of a tube opening; inverting the toothpaste tube body, and dripping no liquid from the tube orifice within 10 s; compared with the sample stored at room temperature, the paste after extrusion has normal fragrance and color. No hard particles exist, the pH value is 7.98, the foam amount is 170mm, the consistency is 26mm, the total number of bacterial colonies of the toothpaste is 71cfu/g which is less than 500cfu/g of the national standard, pathogenic bacteria are not detected, lead and arsenic do not exceed the standards, and the toothpaste quality national standard GB8372-2008 and the cosmetic hygiene standard are met.
2. The toothpaste in vitro antibacterial test is as follows
The bacteriostatic ability of the prepared toothpaste is determined by adopting a filter paper method, and the selected strains are as follows: streptococcus mutans, Lactobacillus acidophilus, Actinomyces viscosus, and Candida albicans; the specific method comprises the following steps: uniformly and crossly coating the bacterial culture solution on a culture medium of a culture dish, and placing the culture dish in a constant-temperature incubator at 37 ℃ for 24 hours; respectively taking 5 mu l of diluted toothpaste liquid medicine with different concentrations and sterilized and heat-removed raw water to soak sterile circular filter paper sheets with the diameter of 6mm, uniformly and symmetrically attaching the small circular filter paper sheets to a central area on a culture medium, placing a culture dish in a constant-temperature incubator at 37 ℃ for culturing for 24h, respectively measuring the diameters of antibacterial zones, preliminarily evaluating and analyzing the antibacterial potential of the experimental toothpaste according to the diameter of the antibacterial zones, wherein the negative indicates that the antibacterial zones are smaller than 1mm, the sample has no antibacterial ability, the dilution concentrations of the pastes are respectively 20, 40, 80, 160 and 320mg/ml, and the experimental results are shown in table 1.
TABLE 1 toothpaste in vitro antibacterial test results
3. The efficacy of the toothpaste is tested as follows
The volunteers are recruited to carry out the pharmacodynamic test of the toothpaste test, the subjects are all oral inflammation patients, the use period is 28 days, and the tooth brushing method guidance is carried out on all the subjects. The subjects used a uniform toothbrush and specified toothpaste, and required to brush their teeth 2 times per day (morning and evening) for at least 2min with horizontal tremor, using a toothpaste at a concentration of 1-1.5cm during brushing. It is desirable that the test be conducted without the use of antibiotics and any other oral hygiene product, such as other types of toothpaste, toothbrushes, mouthwashes, dental floss, etc. Diet was not restricted and the statistical results are shown in table 2.
TABLE 2 pharmacodynamic test results of toothpaste containing spina Gleditsiae extract
Figure BDA0001313153090000081
Example 2
Example 2 differs from example 1 in that: in the process of preparing the toothpaste, the types or the contents of the components are different, and certain preparation parameters are different, specifically:
(1) dissolving spina gleditsiae extract 2.5 parts, sorbitol 25 parts, sodium dodecyl sulfate 1.0 part and sodium pyrophosphate 0.3 part in deionized water, stirring uniformly in a mixer, putting into an azeotropic boiler, heating to 90 ℃, so that the prepared colloid is in a uniform, semitransparent and viscous liquid state, and then standing for 1.5 hours to be fully dissolved and expanded for use;
(2) cooling the colloid obtained in the step (1) to 70 ℃, putting an azeotropic pot on a stirrer, sequentially adding 25 parts of silicon dioxide, 1.2 parts of sodium carboxymethylcellulose and 0.6 part of xylitol while stirring (the rotating speed is 300r/min), and continuously stirring for 1.5h (the rotating speed is 350r/min) to uniformly mix various materials;
(3) cooling the colloid to below 45 deg.C, adding Mentholum and small amount of oleum Citri Tangerinae, mechanically mixing and stirring to obtain ointment with certain viscosity and proper consistency;
(4) grinding paste by a grinder, grinding coarse and hard particles to make the paste fine, uniform and stable, grinding twice, storing and aging for 2h after the first grinding, and vacuum degassing after the second grinding until the vacuum degree reaches-0.096 MPa for 50 min;
(5) degassing the paste, standing for 3h, sterilizing, filling into a hose, and sealing to obtain the final product of spina Gleditsiae extract toothpaste.
The main quality index evaluation and bacteriostatic effect test of the toothpaste prepared in this example are as follows:
1. determination of toothpaste appearance, physicochemical index and sanitary index
Taking 4 toothpaste samples, storing 1 toothpaste sample at room temperature, putting the other 3 toothpaste samples into a refrigerator at minus 8 +/-1 ℃, taking out after 8 hours, immediately putting into a constant-temperature incubator at 45 +/-1 ℃, taking out after 8 hours, recovering to room temperature, opening a cover for observation, and enabling the toothpaste body not to overflow out of a tube opening; inverting the toothpaste tube body, and dripping no liquid from the tube orifice within 10 s; compared with the sample stored at room temperature, the paste after extrusion has normal fragrance and color. No hard particles exist, the pH value is 8.05, the foam amount is 175mm, the consistency is 28mm, the total number of bacterial colonies of the toothpaste is 90cfu/g and is less than 500cfu/g of the national standard, pathogenic bacteria are not detected, lead and arsenic do not exceed the standards, and the toothpaste quality national standard GB8372-2008 and the cosmetic hygiene standard are met.
2. The toothpaste in vitro antibacterial test is as follows
The bacteriostatic ability of the prepared toothpaste is determined by adopting a filter paper method, and the selected strains are as follows: streptococcus mutans, Lactobacillus acidophilus, Actinomyces viscosus, and Candida albicans; the specific method comprises the following steps: uniformly and crossly coating the bacterial culture solution on a culture medium of a culture dish, and placing the culture dish in a constant-temperature incubator at 37 ℃ for 24 hours; respectively taking 5 mu l of diluted toothpaste liquid medicine with different concentrations and sterilized and heat-removed raw water to soak sterile circular filter paper sheets with the diameter of 6mm, uniformly and symmetrically attaching the small circular filter paper sheets to a central area on a culture medium, placing a culture dish in a constant-temperature incubator at 37 ℃ for culturing for 24h, respectively measuring the diameters of antibacterial zones, preliminarily evaluating and analyzing the antibacterial potential of the experimental toothpaste according to the diameter of the antibacterial zones, wherein the negative indicates that the antibacterial zones are smaller than 1mm, the sample has no antibacterial ability, the dilution concentrations of the pastes are respectively 20, 40, 80, 160 and 320mg/ml, and the experimental result is shown in table 3.
TABLE 3 toothpaste in vitro antibacterial test results
Figure BDA0001313153090000091
3. The efficacy of the toothpaste is tested as follows
The volunteers are recruited to carry out the pharmacodynamic test of the toothpaste test, the subjects are all oral inflammation patients, the use period is 28 days, and the tooth brushing method guidance is carried out on all the subjects. The subjects used a uniform toothbrush and specified toothpaste, and required to brush their teeth 2 times per day (morning and evening) for at least 2min with horizontal tremor, using a toothpaste at a concentration of 1-1.5cm during brushing. It is desirable that the test be conducted without the use of antibiotics and any other oral hygiene product, such as other types of toothpaste, toothbrushes, mouthwashes, dental floss, etc. Diet was not restricted and the statistical results are shown in table 4.
TABLE 4 pharmacodynamic test results of toothpaste containing spina Gleditsiae extract
Figure BDA0001313153090000102
Example 3
Example 3 differs from example 1 in that: in the process of preparing the toothpaste, the types or the contents of the components are different, and certain preparation parameters are different, specifically:
(1) dissolving 6 parts of spina gleditsiae extract, 20 parts of glycerol, 1.5 parts of methyl cocoa ester-based sodium taurate and 0.3 part of sodium pyrophosphate in deionized water, stirring uniformly in a mixer, putting into an azeotropic boiler, heating to 100 ℃, so that the prepared colloid is in a uniform, semitransparent and sticky liquid state, and then standing for 1h to be fully dissolved and expanded for use;
(2) cooling the colloid obtained in the step (1) to 65 ℃, putting an azeotropic pot on a stirrer, adding 35 parts of calcite powder, 0.8 part of guar gum and 0.7 part of sodium cyclamate in sequence while stirring (at a rotating speed of 310r/min), and continuously stirring for 1h (at a rotating speed of 350r/min) to uniformly mix various materials;
(3) cooling the colloid to below 45 deg.C, adding Mentholum and lemon sesame oil, mechanically mixing, and making into ointment with certain viscosity and proper thickness;
(4) grinding paste by a grinder, grinding coarse and hard particles to make the paste fine, uniform and stable, grinding twice, storing and aging for 3h after the first grinding, and vacuum degassing after the second grinding until the vacuum degree reaches-0.096 MPa for 40 min;
(5) degassing the paste, standing for 2.5h, sterilizing, filling into a hose, and sealing to obtain the final product of spina Gleditsiae extract toothpaste.
The main quality index evaluation and bacteriostatic effect test of the toothpaste prepared in this example are as follows:
1. determination of toothpaste appearance, physicochemical index and sanitary index
Taking 4 toothpaste samples, storing 1 toothpaste sample at room temperature, putting the other 3 toothpaste samples into a refrigerator at minus 8 +/-1 ℃, taking out after 8 hours, immediately putting into a constant-temperature incubator at 45 +/-1 ℃, taking out after 8 hours, recovering to room temperature, opening a cover for observation, and enabling the toothpaste body not to overflow out of a tube opening; inverting the toothpaste tube body, and dripping no liquid from the tube orifice within 10 s; compared with the sample stored at room temperature, the paste after extrusion has normal fragrance and color. No hard particles exist, the pH value is 8.36, the foam amount is 168mm, the consistency is 31mm, the total number of bacterial colonies of the toothpaste is 68cfu/g which is less than 500cfu/g of the national standard, pathogenic bacteria are not detected, lead and arsenic do not exceed the standards, and the toothpaste quality national standard GB8372-2008 and the cosmetic hygiene standard are met.
2. The toothpaste in vitro antibacterial test is as follows
The bacteriostatic ability of the prepared toothpaste is determined by adopting a filter paper method, and the selected strains are as follows: streptococcus mutans, Lactobacillus acidophilus, Actinomyces viscosus, and Candida albicans; the specific method comprises the following steps: uniformly and crossly coating the bacterial culture solution on a culture medium of a culture dish, and placing the culture dish in a constant-temperature incubator at 37 ℃ for 24 hours; respectively taking 5 mu l of diluted toothpaste liquid medicine with different concentrations and sterilized and heat-removed raw water to soak sterile circular filter paper sheets with the diameter of 6mm, uniformly and symmetrically attaching the small circular filter paper sheets to a central area on a culture medium, placing a culture dish in a constant-temperature incubator at 37 ℃ for culturing for 24h, respectively measuring the diameters of antibacterial zones, preliminarily evaluating and analyzing the antibacterial potential of the experimental toothpaste according to the diameter of the antibacterial zones, wherein the negative indicates that the antibacterial zones are smaller than 1mm, the sample has no antibacterial ability, the dilution concentrations of the pastes are respectively 20, 40, 80, 160 and 320mg/ml, and the experimental results are shown in Table 5.
TABLE 5 toothpaste in vitro antibacterial test results
3. The efficacy of the toothpaste is tested as follows
The volunteers are recruited to carry out the pharmacodynamic test of the toothpaste test, the subjects are all oral inflammation patients, the use period is 28 days, and the tooth brushing method guidance is carried out on all the subjects. The subjects used a uniform toothbrush and specified toothpaste, and required to brush their teeth 2 times per day (morning and evening) for at least 2min with horizontal tremor, using a toothpaste at a concentration of 1-1.5cm during brushing. It is desirable that the test be conducted without the use of antibiotics and any other oral hygiene product, such as other types of toothpaste, toothbrushes, mouthwashes, dental floss, etc. Diet was not restricted and the statistical results are shown in table 6.
TABLE 6 pharmacodynamic test results of toothpaste containing spina Gleditsiae extract
Figure BDA0001313153090000122
Therefore, the toothpaste prepared by the invention has obvious improvement effect on dental plaque, gum swelling and pain and oral peculiar smell. Therefore, the toothpaste of the invention can be used for preventing and treating periodontitis, gingivitis, stomatitis, oral ulcer and the like, thereby reducing oral diseases.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (9)

1. The toothpaste containing the spina gleditsiae extract is characterized by comprising the following components in parts by weight: 0.5-8 parts of spina gleditsiae extract; 10-30 parts of a wetting agent; 15-45 parts of a friction agent; 0.5-1.5 parts of foaming agent; 0.4-1.6 parts of adhesive; 0.15-0.3 part of stabilizer; 0.2-0.8 part of sweetening agent;
the spina gleditsiae extract is prepared according to the following steps:
(1) drying spina Gleditsiae, pulverizing, sieving, and collecting the undersize product to obtain spina Gleditsiae coarse powder;
(2) adding ethanol into the spina gleditsiae coarse powder obtained in the step (1), soaking, heating, refluxing, extracting and concentrating;
(3) decolorizing the concentrated solution, and vacuum freeze drying to obtain spina Gleditsiae extract;
in the step (1), the spina gleditsiae is cut into sheets and is cleaned in advance; the drying temperature is 50-70 ℃;
the ethanol in the step (2) is hydrous ethanol; the mass ratio of the spina gleditsiae coarse powder to the ethanol is 1: 5-20; heating reflux extraction at 80-120 deg.C;
decoloring in the step (3) by using activated carbon; the temperature of the cold trap for vacuum freeze drying is-40 to-65 ℃, and the vacuum degree is 1500-3000 Pa.
2. The toothpaste of claim 1, wherein the drying in step (1) is oven drying to constant weight; the sieve is a 50-60 mesh sieve.
3. The toothpaste according to claim 1 or 2, wherein the ethanol in step (2) is 75% ethanol; the mass ratio of the spina gleditsiae coarse powder to the ethanol is 1: 10;
the soaking time is 6-12 h; the temperature of heating reflux extraction is 100 ℃, and the time of heating reflux extraction is 1-3 h; extracting for 2-3 times; concentrating at 50-80 deg.C; the decolorization in the step (3) is performed by using activated carbon.
4. The toothpaste according to claim 1 or 2, wherein the humectant is one or more of propylene glycol, sorbitol, glycerin, polyethylene glycol;
the friction agent is one or more of calcium hydrophosphate, silicon dioxide, calcium carbonate, aluminum hydroxide, calcite powder and chlorite;
the foaming agent is one or more of sodium lauryl sulfate, N-lauroyl sarcosine sodium and methyl cocoyl sodium taurate;
the adhesive comprises one or more of sodium alginate, sodium carboxymethylcellulose, xanthan gum, hydroxyethyl cellulose, guar gum, Arabic gum and carrageenan.
5. The toothpaste according to claim 1 or 2, wherein the stabilizer is sodium pyrophosphate;
the sweetener is one or more of saccharin sodium, sucrose, xylitol, sodium cyclamate and sodium diaminate;
the toothpaste also contains edible essence and water;
the edible essence is one or more of menthol, spearmint oil, perilla oil, lemon oil, orange oil, clove oil, cinnamon oil, orange oil, peppermint oil, borneol, vanillin, citral and lauraldehyde;
the water is one or two of purified water or deionized water.
6. A method of preparing a toothpaste as claimed in any one of claims 1 to 5 comprising the steps of:
(1) dissolving spina Gleditsiae extract, wetting agent, foaming agent and stabilizer in water, mixing, heating to obtain gel in uniform semitransparent viscous liquid state, and standing to allow it to melt and expand;
(2) cooling the colloid obtained in the step (1) to 50-90 ℃, sequentially adding a friction agent, an adhesive and a sweetening agent, and continuously stirring;
(3) cooling the colloid to below 45 deg.C, adding other adjuvants, and stirring to obtain paste;
(4) grinding the paste, then vacuum degassing, standing and sterilizing to obtain the toothpaste.
7. The production method according to claim 6, wherein the mixing in the step (1) is performed in a blender;
heating is carried out in an azeotropic boiler;
heating to 75-100 deg.C, and standing for 1-2 h.
8. The method according to claim 6 or 7, wherein the cooling in the step (2) is to a temperature of 65 to 70 ℃;
adding the friction agent, the adhesive and the sweetener while stirring, wherein the stirring speed is 300-320 r/min;
the continuous stirring time is 1-2h, and the rotating speed is 350-360 r/min.
9. The production method according to claim 6 or 7, wherein the grinding in the step (4) is performed by a grinder;
grinding is carried out twice, the grinding is carried out for the first time and then stored, and the vacuum degassing is carried out after the grinding for the second time;
degassing until the vacuum degree reaches below-0.096 MPa;
standing for 2-4 h.
CN201710413997.7A 2017-06-05 2017-06-05 Toothpaste containing spina gleditsiae extract and preparation method thereof Active CN107184473B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106265368A (en) * 2016-09-30 2017-01-04 中科漠霖科技(北京)有限公司 A kind of medicated toothpaste containing Francolini pintadeani leaf extract and preparation method thereof

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN106265368A (en) * 2016-09-30 2017-01-04 中科漠霖科技(北京)有限公司 A kind of medicated toothpaste containing Francolini pintadeani leaf extract and preparation method thereof

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口腔炎喷雾剂治疗慢性牙周炎的临床观察;封帅;《中国民间疗法》;20161231;第24卷(第12期);第62-64页 *
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