CN108852909B - Toothpaste for preventing dental caries and preparation method thereof - Google Patents

Toothpaste for preventing dental caries and preparation method thereof Download PDF

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CN108852909B
CN108852909B CN201810864891.3A CN201810864891A CN108852909B CN 108852909 B CN108852909 B CN 108852909B CN 201810864891 A CN201810864891 A CN 201810864891A CN 108852909 B CN108852909 B CN 108852909B
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toothpaste
stirring
chitosan
volatile oil
sodium
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CN108852909A (en
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易国辉
何小稳
姚孟霞
张菁芸
陈锦萍
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Hainan Medical College
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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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • 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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • 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
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • 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
    • A61K8/736Chitin; Chitosan; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • 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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
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  • Oral & Maxillofacial Surgery (AREA)
  • Emergency Medicine (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to a toothpaste for preventing dental caries and a preparation method thereof, belonging to the technical field of toothpaste. The papaya seed volatile oil and the chitosan are added at the same time, the two components are compatible with each other to play a synergistic role in mutually promoting the anti-caries effect, and meanwhile, the problem that the chitosan is difficult to dissolve is solved, and the stability of the papaya seed volatile oil is improved. The toothpaste has stable performance, and has fresh and cool taste, and can improve breath and effectively prevent dental caries.

Description

Toothpaste for preventing dental caries and preparation method thereof
Technical Field
The invention relates to a dental caries prevention toothpaste and a preparation method thereof, belonging to the technical field of skin care.
Background
Dental caries is a common oral disease with a combination of multiple factors, and researches for many years prove that Streptococcus mutans (Streptococcus mutans) is a main cariogenic bacterium for human, the cariogenic virulence of the Streptococcus mutans is mainly reflected in the adhesion, the colonization, the acidity and the acid resistance of the tooth surface, and the process of forming dental plaque biofilm by the adhesion and the aggregation of the Streptococcus mutans on the tooth surface is the basis of the dental caries, so that the control of the formation of the dental plaque biofilm is the key for preventing and controlling the dental caries. It has been found that bacteria with biofilms have a resistance to antibiotics that is more than 1000 times higher than that of free bacteria and are difficult to remove by conventional sterilization methods. The plant volatile oil is also called essential oil, has various biological activities such as oxidation resistance, virus resistance, bacteria resistance and the like, and the main component of the papaya seed volatile oil is Benzyl Isothiocyanate (BITC), accounting for 99.36 percent. The research on the cancer prevention and inhibition of benzyl isothiocyanate has made great progress and has strong biological activity, and the research on the inhibition of the growth of oral bacteria has not been reported.
Disclosure of Invention
Aiming at the problems, the invention aims to provide the toothpaste for preventing the decayed tooth, which has the synergistic effect of mutually promoting the effect of preventing the decayed tooth by using the two components of the papaya seed volatile oil and the chitosan which are mutually compatible, and simultaneously, not only solves the problem that the chitosan is difficult to dissolve, but also improves the stability of the papaya seed volatile oil. The toothpaste has stable performance, and has fresh and cool taste, and can improve breath and effectively prevent dental caries.
The technical solution of the invention is that:
the dental caries prevention toothpaste is prepared from the following raw materials in percentage by weight: 0.004-0.008% of papaya seed volatile oil, 0.846-1.272% of chitosan, 35-45% of calcium bicarbonate, 0.60-1.50% of glycerol, 18-20% of sorbitol, 0.50-1.00% of sodium carboxymethylcellulose, 2.00-4.00% of sodium lauryl sulfate, 0.14-0.20% of sodium alginate, 3.50-4.80% of sodium hyaluronate, 0.10-0.20% of methyl p-hydroxybenzoate, 0.01-0.02% of xylitol and 22-39.3% of deionized water.
Furthermore, the papaya seed volatile oil is obtained by extracting papaya seeds, wherein the content of benzyl isothiocyanate is 99.36%.
The extraction method is described in patent application 20141018682.
Further, the content of the chitosan is 99%, and the pH value is 5-6.
Furthermore, the content of the calcium bicarbonate is 99%, and the granularity is 80 meshes.
Furthermore, the content of the sodium hyaluronate is 95%, and the content of heavy metal is less than or equal to 10 ppm.
The invention also provides a preparation method of the toothpaste for preventing dental caries, which comprises the following steps:
firstly, putting 22-39.3% of deionized water into a reaction kettle, starting a stirrer, setting the stirring speed to be 50rpm, sequentially adding 35-45% of calcium bicarbonate and 18-20% of sorbitol, after the calcium bicarbonate and the sorbitol are completely dissolved, increasing the stirring speed to 80rpm, sequentially adding 0.60-1.50% of glycerol, 0.50-1.00% of sodium carboxymethylcellulose, 0.14-0.20% of sodium alginate and 0.10-0.20% of methyl p-hydroxybenzoate into the reaction kettle, keeping stirring for 30min, and carrying out premixing and dispersion treatment;
then, opening a heating device, setting the temperature to be 70-85 ℃, slowly adding 0.004-0.008% of papaya seed volatile oil, 0.846-1.272% of chitosan and 3.50-4.80% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1h after the addition is finished, and then keeping the temperature for 30min to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.01-0.02% of xylitol and 2.00-4.00% of sodium lauryl sulfate, continuing stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, and discharging.
Papaya seed volatile oil plays a very good role in preventing dental caries in the scheme, which is not disclosed in the prior art and the literature at present. In addition, chitosan has good effect of inhibiting bacterial activity and is applied to the fields of cosmetics, agriculture and tobacco, but the chitosan is difficult to dissolve, so the chitosan cannot be well applied to toothpaste, and in some technologies, water-soluble chitosan is added into toothpaste in a modified mode, but the antibacterial effect of the chitosan is greatly reduced. According to the invention, the papaya seed volatile oil and the chitosan are combined for use, the two are found to have a mutual dissolution effect, the problem that the chitosan is difficult to dissolve is solved by perfectly matching the papaya seed volatile oil and the chitosan in a reasonable proportion, and the chitosan also ensures the stability of the papaya seed volatile oil in the toothpaste composition.
TABLE 1 comparison of the Performance of the caries-preventive toothpaste of the present invention with other types of caries-preventive toothpastes or drugs
Dental caries preventing toothpaste 1 Toothpaste for preventing dental caries 2 The invention provides toothpaste for preventing decayed teeth Medicine for preventing dental caries
Appearance of the product Milk white and bright luster Milky white color Milk white with bright luster /
Taste of the product Fresh and sweet Fresh and sweet Fresh and sweet /
Dental caries preventing effect 90.5%~94.2% 66.5%~70.6% 93.2%~95.4% 95.0%~96.3%
Stability of Demixing after 1 month Demixing after 15 days No delamination in 1 year /
Remarking: 1. the caries prevention toothpaste 1 and the caries prevention toothpaste 2 are respectively toothpaste prepared by removing the papaya seed volatile oil and the chitosan in the formula of the caries prevention toothpaste and still keeping the same content proportion and the same preparation process as the invention;
2. the anti-caries medicine is chlorhexidine, and the drug effect of the anti-caries medicine is in the conventional use range compared with the 3 tooth pastes;
3. the cariogenic effect is characterized by the percentage of inhibition of laboratory-cultured S.mutans in the same environment.
Referring to table 1, it can be seen that the toothpaste 1 prepared by separately adding the papaya seed volatile oil has relatively obvious effect of preventing dental caries, but has poor stability, and the papaya seed volatile oil, glycerin and other oil phases and other water phase components of the toothpaste are layered after 1 month, so that the stability is not satisfactory; if the papaya seed volatile oil is not added, the toothpaste 2 prepared by only adding the chitosan also has a partial caries prevention effect, but is only 66.5-70.6 percent, which is reduced by 40 percent compared with the toothpaste prepared by only adding the papaya seed volatile oil, and the caries prevention effect is provided by xylitol and chitosan through analysis, and meanwhile, the toothpaste has oil layer delamination after 15 days, and has poorer stability. Compared with toothpaste 1 and toothpaste 2, the invention has the advantages that the carious tooth prevention effect is higher than that generated by using two components separately because the papaya seed volatile oil and the chitosan are added, and the stability is improved to more than 1 year. Therefore, in the scheme of the invention, the mutual compatibility of the two components plays a synergistic role of mutual promotion, and simultaneously, the problem that chitosan is difficult to dissolve is solved, and the stability of the papaya seed volatile oil is improved. In addition, due to the addition of the sodium hyaluronate, the prepared toothpaste product is particularly fresh and delicious and is suitable for children and adults in different age groups. The stability of the prepared anti-caries toothpaste can reach more than 1 year by combining with other components such as reasonably selected abrasives, and the anti-caries toothpaste plays a role in preventing caries and basically reaches the efficacy level of an anti-caries medicament when being used as a health-care product in daily life.
Detailed Description
To further illustrate the technical means and advantages of the present invention, the following detailed description is given to the embodiments of the present invention with reference to the preferred embodiments:
example one
Firstly, putting 39.3% of deionized water into a reaction kettle, starting a stirrer, setting the stirring speed to be 50rpm, sequentially adding 35% of calcium bicarbonate and 18% of sorbitol, increasing the stirring speed to 80rpm after the calcium bicarbonate and the sorbitol are completely dissolved, then sequentially adding 0.60% of glycerol, 0.50% of sodium carboxymethylcellulose, 0.14% of sodium alginate and 0.10% of methyl p-hydroxybenzoate into the reaction kettle, keeping stirring for 30min, and carrying out premixing and dispersion treatment;
then, opening a heating device, setting the temperature to be 70 ℃, slowly adding 0.004% of papaya seed volatile oil, 0.846% of chitosan and 3.50% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1h after the addition is finished, and then keeping the temperature for 30min to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.01% of xylitol and 2.00% of sodium lauryl sulfate, continuously stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, discharging, and preparing the dental caries preventing toothpaste.
Tests show that the toothpaste has an anti-caries effect of 93.5% and can keep the stability for more than 1 year.
Example two
Firstly, putting 33.55% of deionized water into a reaction kettle, starting a stirrer, setting the stirring speed to be 50rpm, sequentially adding 38% of calcium bicarbonate and 19% of sorbitol, increasing the stirring speed to 80rpm after the calcium bicarbonate and the sorbitol are completely dissolved, then sequentially adding 0.80% of glycerol, 0.60% of sodium carboxymethylcellulose, 0.16% of sodium alginate and 0.20% of methyl p-hydroxybenzoate into the reaction kettle, keeping stirring for 30min, and carrying out premixing and dispersion treatment;
then, opening a heating device, setting the temperature to be 78 ℃, slowly adding 0.006% of papaya seed volatile oil, 0.864% of chitosan and 3.80% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1h after the addition is finished, and keeping the temperature for 30min to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.02% of xylitol and 3.00% of sodium lauryl sulfate, continuing stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, and discharging.
Tests show that the toothpaste has an anti-caries effect of 93.2% and stability of more than 1 year.
EXAMPLE III
Firstly, putting 31.04% of deionized water into a reaction kettle, starting a stirrer, setting the stirring speed to be 50rpm, sequentially adding 40% of calcium bicarbonate and 18% of sorbitol, increasing the stirring speed to 80rpm after the calcium bicarbonate and the sorbitol are completely dissolved, sequentially adding 1.00% of glycerol, 0.70% of sodium carboxymethylcellulose, 0.18% of sodium alginate and 0.10% of methyl p-hydroxybenzoate into the reaction kettle, keeping stirring for 30min, and carrying out premixing and dispersion treatment;
then, opening a heating device, setting the temperature to be 75 ℃, slowly adding 0.007% of papaya seed volatile oil, 0.963% of chitosan and 4.00% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1h after the addition is finished, and keeping the temperature for 30min to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.01% of xylitol and 4.00% of sodium lauryl sulfate, continuing stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, and discharging.
Tests show that the toothpaste has a caries prevention effect of 94.6% and can keep the stability for more than 1 year.
Example four
Firstly, putting 28.02% of deionized water into a reaction kettle, starting a stirrer, setting the stirring speed to be 50rpm, sequentially adding 42% of calcium bicarbonate and 19% of sorbitol, increasing the stirring speed to 80rpm after the calcium bicarbonate and the sorbitol are completely dissolved, sequentially adding 1.20% of glycerol, 0.80% of sodium carboxymethylcellulose, 0.15% of sodium alginate and 0.20% of methyl p-hydroxybenzoate into the reaction kettle, keeping stirring for 30min, and carrying out premixing and dispersion treatment;
then, opening a heating device, setting the temperature to be 80 ℃, slowly adding 0.008% of papaya seed volatile oil, 1.112% of chitosan and 4.50% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1h after the addition is finished, and keeping the temperature for 30min to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.01% of xylitol and 3.00% of sodium lauryl sulfate, continuing stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, and discharging.
Tests show that the toothpaste has a caries prevention effect of 94.9% and can keep the stability for more than 1 year.
EXAMPLE five
Firstly, putting 22% of deionized water into a reaction kettle, starting a stirrer, setting the stirring speed to be 50rpm, sequentially adding 45% of calcium bicarbonate and 20% of sorbitol, increasing the stirring speed to 80rpm after the calcium bicarbonate and the sorbitol are completely dissolved, sequentially adding 1.50% of glycerol, 1.00% of sodium carboxymethylcellulose, 0.20% of sodium alginate and 0.20% of methyl p-hydroxybenzoate into the reaction kettle, keeping stirring for 30min, and carrying out premixing and dispersion treatment;
then, opening a heating device, setting the temperature to be 85 ℃, slowly adding 0.008% of papaya seed volatile oil, 1.272% of chitosan and 4.80% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1h after the addition is finished, and keeping the temperature for 30min to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.02% of xylitol and 4.00% of sodium lauryl sulfate, continuing stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, and discharging.
Tests show that the toothpaste has a caries prevention effect of 95.4% and can keep the stability for more than 1 year.

Claims (4)

1. The dental caries prevention toothpaste is characterized by being prepared from the following raw materials in parts by weight: 0.004-0.008% of papaya seed volatile oil, 0.846-1.272% of chitosan, 35-45% of calcium bicarbonate, 0.60-1.50% of glycerol, 18-20% of sorbitol, 0.50-1.00% of sodium carboxymethylcellulose, 2.00-4.00% of sodium lauryl sulfate, 0.14-0.20% of sodium alginate, 3.50-4.80% of sodium hyaluronate, 0.10-0.20% of methyl p-hydroxybenzoate, 0.01-0.02% of xylitol and 22-39.3% of deionized water;
the papaya seed volatile oil is obtained by extracting papaya seeds, wherein the content of benzyl isothiocyanate is 99.36%;
the chitosan has the purity of 99% and the pH value of 5-6.
2. The toothpaste according to claim 1, wherein said calcium bicarbonate has a purity of 99% and a particle size of 80 mesh.
3. The toothpaste according to claim 1, wherein the sodium hyaluronate has a purity of 95% and a heavy metal content of less than 10 ppm.
4. The method for preparing a toothpaste for preventing dental caries according to claim 1, comprising the steps of:
firstly, 22-39.3% of deionized water is put into a reaction kettle, a stirrer is started, the stirring speed is set to be 50rpm, 35-45% of calcium bicarbonate and 18-20% of sorbitol are sequentially added, after the calcium bicarbonate and the sorbitol are completely dissolved, the stirring speed is increased to 80rpm, then 0.60-1.50% of glycerol, 0.50-1.00% of sodium carboxymethylcellulose, 0.14-0.20% of sodium alginate and 0.10-0.20% of methyl p-hydroxybenzoate are sequentially added into the reaction kettle, stirring is kept for 30min, and premixing and dispersion treatment are carried out;
then, opening a heating device, setting the temperature to be 70-85 ℃, slowly adding 0.004-0.008% of papaya seed volatile oil, 0.846-1.272% of chitosan and 3.50-4.80% of sodium hyaluronate into the reaction kettle in sequence, continuously stirring for 1 hour after the addition is finished, and keeping the temperature for 30 minutes to ensure uniform stirring;
and finally, reducing the stirring speed to 30rpm, adding 0.01-0.02% of xylitol and 2.00-4.00% of sodium lauryl sulfate, continuing stirring for 1h, closing the heating device and the stirring device, slowly cooling to room temperature, standing for 1h, and discharging.
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