CN108079013A - A kind of preparation method and application for relieving pain bioactivity glass powder - Google Patents

A kind of preparation method and application for relieving pain bioactivity glass powder Download PDF

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CN108079013A
CN108079013A CN201711457498.4A CN201711457498A CN108079013A CN 108079013 A CN108079013 A CN 108079013A CN 201711457498 A CN201711457498 A CN 201711457498A CN 108079013 A CN108079013 A CN 108079013A
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glass powder
bioactivity glass
analgesic
preparation
deionized water
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CN108079013B (en
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李祥永
李雨丝
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DONGGUAN HONGYUAN MEDICAL TECHNOLOGY Co Ltd
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DONGGUAN HONGYUAN MEDICAL TECHNOLOGY Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/141Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/143Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with inorganic compounds

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  • Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a kind of preparation methods for relieving pain bioactivity glass powder, are reacted and are made using raw materials such as concentrated nitric acid, ethyl orthosilicate, triethyl phosphate, calcium nitrate tetrahydrate, sodium nitrate, potassium nitrate, potassium-containing compound aqueous solutions.The present invention also discloses a kind of applications for relieving pain bioactivity glass powder, are applied in oral preparation.Analgesic bioactivity glass powder produced by the present invention plays an important role of good anti-sensitivity of tooth, slows down dental pain, especially suitable for bleeding gums, the targeted therapy of dental pain.Potassium ion slowly discharges after bioactivity glass powder demeanour dentinal tubule, blocks the neural traffic in dentinal tubule, reduces dental pain immediately;And bioactivity glass has long-acting tooth antiallergic effect, the two complements each other, and can effectively alleviate sensitivity of tooth pain, and 3 months visible positive effects are used continuously, can effectively avoid the recurrent exerbation of gingivitis.

Description

A kind of preparation method and application for relieving pain bioactivity glass powder
Technical field
The present invention relates to a kind of bioactivity glass preparing technical field more particularly to a kind of analgesic bioactivity glass powder The preparation method and application at end.
Background technology
Biomaterial is a kind of new and high technology material, is mainly used for the diagnosis of tissue or organ, repairs.The first generation is given birth to Object material does not have bioactivity, such as medical metal, inactive ceramic, and this kind of material belongs to bio-inert material;Second generation biology Material, such as bioactive ceramics, hydroxyapatite can provide the ability of tissue conduction for cambium, i.e. tissue conducts Biomaterial has bioactivity;In the 1990s, the concept of third generation biomaterial is suggested, on a molecular scale Activated cell responds, and belongs to tissue induction biomaterial.While this kind of material has bioactivity and degradability, and have Gene activation acts on, and cell can be stimulated to generate responsing reaction on a molecular scale, promotes cell Proliferation, differentiation, and passes through secretion Extracellular matrix and self assembling process form new tissue, the regeneration and reparation of induced tissue, suitable in situ tissue regeneration and Organizational project regenerates.Bioactivity glass has good bioactivity, and hydroxyapatite is induced in body fluid or simulated body fluid Deposition, play the role of osteoacusis;Secondly, bioactivity glass has good degradable characteristic, and by adjusting its group Into and preparation process, its microstructure can be adjusted so as to adjusting control its degradation speed, be allowed to and tissue growth speeds match; Meanwhile the released ion of bioactivity glass can promote multiplication and the differentiation of cell, activate the expression of osteogenesis gene;Therefore, Bioactivity glass is looked at as typical third generation biomaterial.In addition, bioactivity glass as bioactivity without unit Point it is added in tissue engineering bracket material, natural macromolecular material can be made up in terms of degradability and cell compatibility not Foot.
Bioactivity glass is a kind of special glass material with tissue repair, initially by University of Florida Hench professors develop out in 19 century 70s, belong to silicate systems and with specific chemical composition.It is being planted Bonding action can be generated after entering in vivo so as to closely combine bone tissue, while does not generate the adverse effects such as inflammation, is had good Good biocompatibility and bioactivity, thus the highest attention of bio-medical material circle is caused, and with material preparation The development of technology, preparation process, chemical composition, institutional framework and the physicochemical property of bioactivity glass are also being continuously improved, Continuous forward development is obtained, application prospect is also more and more extensive.
Patient with gingivitis, red and swollen usually with bleeding gums, the symptoms such as distending pain are, it is necessary to long-acting anti-using having Sensitive drug progressively alleviates gingivitis to recovery from illness.But existing oral preparation, active ingredient are difficult to be attached in lesion, rise Effect speed is slow, and specific aim is poor, and the pain of gingivitis patients is made to be difficult to alleviate immediately;And agents area is in oral cavity, Huan Zherong Easily preparation is swallowed together with saliva, the poor taste of the medicament, the drug use feeling for making patient is poor, is unwilling to receive to make for a long time With, it is difficult to reach the required course for the treatment of and curative effect;Meanwhile active ingredient is difficult to be attached to lesions position for a long time so that Huan Zhexu Regular frequent supplement medication is wanted, but also patient is difficult to adhere to using drug so that gingivitis is repeatedly, it is difficult to thoroughly fully recover from an illness More.
The content of the invention
Against the above deficiency, it is an object of the invention to provide it is a kind of relieve pain bioactivity glass powder preparation method and Using there is good instant alleviation dental pain, and the effect of long-acting antiallergic can also repair damaged tooth, and it is thin to inhibit oral cavity Bacterium.
The used in order to achieve the above objectives technical solution of the present invention is:
A kind of preparation method for relieving pain bioactivity glass powder, comprises the following steps:
(1) concentrated nitric acid is scattered in deionized water, stirred evenly, obtain dust technology;
(2) ethyl orthosilicate is taken to be dissolved in dust technology, when stirring hydrolysis 0.5~2 is small;
(3) triethyl phosphate is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.5~1 is small;
(4) calcium nitrate tetrahydrate is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 5~15 minutes;
(5) one or both of sodium nitrate, potassium nitrate are taken, is dissolved in step (4) acquired solution, stirring hydrolysis 5~30 Minute;
(6) when by the placement of step (5) acquired solution, ageing 6~24 is small at room temperature, solution gradually forms gel, this is coagulated Glue continue at 60~70 DEG C ageing 24~72 it is small when;
(7) when by gel obtained by step (6), drying 6~24 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 650~750 DEG C 1~4 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder that step (9) obtains and potassium-containing compound aqueous solution are carried out under ultrasound environments Mixing, obtains mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
As a further improvement on the present invention, the step (5) is further comprising the steps of:
(5.1) citric acid is taken to be dissolved in step (5) acquired solution, stirring hydrolysis 5~15 minutes;
As a further improvement on the present invention, concentrated nitric acid and the volume ratio of deionized water are 1 in the step (1):8~ 1:45。
As a further improvement on the present invention, the ratio of ethyl orthosilicate and deionized water is 1g in the step (2):(1 ~2) ml.
As a further improvement on the present invention, the ratio of triethyl phosphate and deionized water is 1g in the step (3): (10~25) ml.
As a further improvement on the present invention, the ratio of calcium nitrate tetrahydrate and deionized water is 1g in the step (4): (1.7~4) ml.
As a further improvement on the present invention, the ratio of sodium nitrate and deionized water is (0~2.8) in the step (5) g:The ratio of 1ml, sodium nitrate and deionized water is (0~1.6) g:1ml.
As a further improvement on the present invention, in the step (10) potassium-containing compound aqueous solution for potassium nitrate aqueous solution, One kind in potassium chloride solution, aqueous dibasic potassium phosphate solution, potassium bicarbonate aqueous solution, wet chemical;The biology glass The ratio of glass reactive powder and 5% potassium-containing compound aqueous solution is (0.5~2) g:1g.
As a further improvement on the present invention, the ratio of citric acid deionized water is (0~0.06) in the step (5.1) g:1ml。
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For:
Wherein, the rubbing agent includes analgesic bioactivity glass powder.
As a further improvement on the present invention, the moisturizer is propylene glycol, glycerine, polyethylene glycol, deionized water, sorb The combination of one or more of alcohol.
As a further improvement on the present invention, the rubbing agent further includes one or both of calcium carbonate or calcium monohydrogen phosphate Combination.
As a further improvement on the present invention, the surfactant is sodium lauryl sulfate, sodium cocoyl glutamate, coconut palm The combination of one or more of oleamide propyl betaine, lauryl sodium sulfate, cocoyl sarcosine sodium.
As a further improvement on the present invention, the thickener for carboxymethyl cellulose, hydroxyethyl cellulose, guar gum, The combination of one or more of Arabic gum, xanthans.
As a further improvement on the present invention, the preservative is ethylparaben, in methyl hydroxybenzoate, propylben One or more of combinations.
Beneficial effects of the present invention are:
Preparation method provided by the invention, using unique formula and technique, industrialization production easy to implement, and each batch Product quality stablize, obtained powder diameter be nanoscale, and shape be the ellipsoid with capillary structure, be conducive to by Thickener, pain management drug ingedient (potassium ion) are placed in inside its capillary structure, and make thickener, pain management drug Ingredient from capillary structure internal stretch to surface on so that its surface possesses stronger viscosity and certain density controls Treat drug (potassium ion) ingredient.
Analgesic bioactivity glass powder produced by the present invention, using the ellipsoid sprills with capillary structure as core, When being made into oral preparation, due to its unique ingredient, structure and nano level grain size, preparation is made to be glued with excellent surface Property, accommodated inside, thickener, pain management drug ingedient (potassium ion) are placed in inside its capillary structure and extended to Surface, and with preferable sustained release, long lasting benefits;Powder can go directly lesion, and can adsorb for a long time in lesion, rise To anti-sensitivity of tooth, slow down the effect of dental pain, the targeting especially suitable for oral conditions such as bleeding gums, dental pains is controlled It treats.Its potassium ion carried is slowly discharged after the dentinal tubule of lesions position is reached inside bioactivity glass powder, hindered Neural traffic in snaggletooth tubules reduces dental pain, while the growth that can effectively inhibit bacteria immediately;It is and biological Activity glass has long-acting tooth antiallergic effect, the mutually auxiliary phase of the two by repairing, blocking tooth chips gap or groove position Into, can adsorb the affected site in oral cavity for a long time, and due to its stronger viscosity, will not with swallowing for saliva and by Patient eats, because without regular supplement drug, convenient for patient's long-time service, reaching the effect of required and the course for the treatment of, effectively Alleviate sensitivity of tooth pain in ground.By actual test, general oral condition patient, it is visible apparent to be used continuously 3 months Therapeutic effect;After 3 months, the patient of most gingivitis recurrent exerbations is no longer recurred.
Above-mentioned is the general introduction of inventive technique scheme, and below in conjunction with specific embodiment, the present invention will be further described.
Specific embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined purpose is taken, below in conjunction with preferable The specific embodiment of the present invention is described in detail in embodiment.
Ratio in each embodiment unless otherwise instructed, is weight percentage.
Embodiment 1
A kind of preparation method for relieving pain bioactivity glass powder provided in this embodiment, comprises the following steps:
(1) concentrated nitric acid of 6ml 69wt.% is scattered in 250ml deionized waters, stirred evenly, obtain dust technology;
(2) 125g ethyl orthosilicates is taken to be dissolved in dust technology, when stirring hydrolysis 1.5 is small;
(3) 10g triethyl phosphates is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.8 is small;
(4) 62.5g calcium nitrate tetrahydrates is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 15 minutes;
(5) 700g sodium nitrate is taken, is dissolved in step (4) acquired solution, stirring hydrolysis 30 minutes;
(6) when by the placement of step (5) acquired solution, ageing 20 is small at room temperature, solution gradually forms gel, by the gel Continue at 60~70 DEG C ageing 20 it is small when;
(7) when by gel obtained by step (6), drying 10 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 750 DEG C 1 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder for obtaining step (9) and 5wt.% potassium nitrate aqueous solutions are according to mass ratio 0.5: 1 ratio is mixed under ultrasound environments, obtains mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
Embodiment 2
A kind of preparation method for relieving pain bioactivity glass powder provided in this embodiment, comprises the following steps:
(1) concentrated nitric acid of 8ml 69wt.% is scattered in 250ml deionized waters, stirred evenly, obtain dust technology;
(2) 160g ethyl orthosilicates is taken to be dissolved in dust technology, when stirring hydrolysis 0.5 is small;
(3) 14g triethyl phosphates is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.6 is small;
(4) 54g calcium nitrate tetrahydrates is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 5 minutes;
(5) 300g sodium nitrate and 300g potassium nitrate are taken, is dissolved in step (4) acquired solution, stirring hydrolysis 20 minutes;
(5.1) 15g citric acids is taken to be dissolved in step (5) acquired solution, stirring hydrolysis 15 minutes;
(6) when by the placement of step (5) acquired solution, ageing 15 is small at room temperature, solution gradually forms gel, by the gel Continue at 60~70 DEG C ageing 15 it is small when;
(7) when by gel obtained by step (6), drying 15 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 725 DEG C 1.75 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder for obtaining step (9) and 5wt.% potassium chloride solutions are according to mass ratio 0.8: 1 ratio is mixed under ultrasound environments, obtains mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
Embodiment 3
The present embodiment provides a kind of preparation methods for relieving pain bioactivity glass powder, comprise the following steps:
(1) concentrated nitric acid of 10ml 69wt.% is scattered in 250ml deionized waters, stirred evenly, obtain dust technology;
(2) 195g ethyl orthosilicates is taken to be dissolved in dust technology, when stirring hydrolysis 2 is small;
(3) 18g triethyl phosphates is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.7 is small;
(4) 105.5g calcium nitrate tetrahydrates is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 12 minutes;
(5) 500g sodium nitrate and 100g potassium nitrate are taken, is dissolved in step (4) acquired solution, stirring hydrolysis 5 minutes;
(6) when by the placement of step (5) acquired solution, ageing 24 is small at room temperature, solution gradually forms gel, by the gel Continue at 60~70 DEG C ageing 24 it is small when;
(7) when by gel obtained by step (6), drying 15 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 725 DEG C 1.75 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder and the potassium dihydrogen phosphate aqueous solution of 5%wt. obtained step (9) is according to quality Than 1.2:1 ratio is mixed under ultrasound environments, obtains mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
Embodiment 4
The present embodiment provides a kind of preparation methods for relieving pain bioactivity glass powder, comprise the following steps:
(1) concentrated nitric acid of 12ml 69wt.% is scattered in 250ml deionized waters, stirred evenly, obtain dust technology;
(2) 220g ethyl orthosilicates is taken to be dissolved in dust technology, when stirring hydrolysis 1 is small;
(3) 22g triethyl phosphates is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.9 is small;
(4) 130g calcium nitrate tetrahydrates is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 8 minutes;
(5) 400g sodium nitrate and 200g potassium nitrate are taken, is dissolved in step (4) acquired solution, stirring hydrolysis 15 minutes;
(5.1) 5g citric acids is taken to be dissolved in step (5) acquired solution, stirring hydrolysis 5 minutes;
(6) when by the placement of step (5) acquired solution, ageing 10 is small at room temperature, solution gradually forms gel, by the gel Continue at 60~70 DEG C ageing 10 it is small when;
(7) when by gel obtained by step (6), drying 20 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 675 DEG C 3.25 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder for obtaining step (9) and 5%wt. potassium bicarbonate aqueous solutions are according to mass ratio 1.6:1 ratio is mixed under ultrasound environments, obtains mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
Embodiment 5
The present embodiment provides a kind of preparation methods for relieving pain bioactivity glass powder, comprise the following steps:
(1) concentrated nitric acid of 13.5ml 69wt.% is scattered in 250ml deionized waters, stirred evenly, obtain dust technology;
(2) 250g ethyl orthosilicates is taken to be dissolved in dust technology, when stirring hydrolysis 1.5 is small;
(3) 25g triethyl phosphates is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.5 is small;
(4) 147g calcium nitrate tetrahydrates is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 10 minutes;
(5) 400g potassium nitrate is taken, is dissolved in step (4) acquired solution, stirring hydrolysis 10 minutes;
(5.1) 10g citric acids is taken to be dissolved in step (5) acquired solution, stirring hydrolysis 10 minutes;
(6) by step (5) acquired solution place at room temperature ageing 6 it is small when, solution gradually forms gel, by the gel after Continue at 60~70 DEG C ageing 6 it is small when;
(7) when by gel obtained by step (6), drying 24 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 650 DEG C 4 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder for obtaining step (9) and 5wt.% wet chemicals are according to mass ratio 2:1 Ratio mixed under ultrasound environments, obtain mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
Application Example 1
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For (by mass percentage):
Wherein bioactivity glass powder is using the analgesic bioactivity glass powder obtained of embodiment 1.
Manufacture craft is:Thickener is scattered in the moisturizer in addition to deionized water, by sweetener, rubbing agent, surface Activating agent is added in deionized water, and preceding liquid is poured into rear liquid, through storing, being aged, adding in preservative, after stirring evenly, then is passed through Grinding, vacuum outgas are made.
Application Example 2
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For (by mass percentage):
Wherein bioactivity glass powder is using the analgesic bioactivity glass powder obtained of embodiment 2.
Manufacture craft is:Thickener is scattered in the moisturizer in addition to deionized water, by sweetener, rubbing agent, surface Activating agent is added in deionized water, and preceding liquid is poured into rear liquid, through storing, being aged, adding in preservative, after stirring evenly, then is passed through Grinding, vacuum outgas are made.
Application Example 3
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For (by mass percentage):
Wherein bioactivity glass powder is using the analgesic bioactivity glass powder obtained of embodiment 3.
Manufacture craft is:Thickener is scattered in the moisturizer in addition to deionized water, by sweetener, rubbing agent, surface Activating agent is added in deionized water, and preceding liquid is poured into rear liquid, through storing, being aged, adding in preservative, after stirring evenly, then is passed through Grinding, vacuum outgas are made.
Application Example 4
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For (by mass percentage):
Wherein bioactivity glass powder is using the analgesic bioactivity glass powder obtained of embodiment 3.
Manufacture craft is:Thickener is scattered in the moisturizer in addition to deionized water, by sweetener, rubbing agent, surface Activating agent is added in deionized water, and preceding liquid is poured into rear liquid, through storing, being aged, adding in preservative, after stirring evenly, then is passed through Grinding, vacuum outgas are made.
Application Example 5
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For (by mass percentage):
Wherein bioactivity glass powder is using the analgesic bioactivity glass powder obtained of embodiment 4.
Manufacture craft is:Thickener is scattered in the moisturizer in addition to deionized water, by sweetener, rubbing agent, surface Activating agent is added in deionized water, and preceding liquid is poured into rear liquid, through storing, being aged, adding in preservative, after stirring evenly, then is passed through Grinding, vacuum outgas are made.
Application Example 6
A kind of application for relieving pain bioactivity glass powder, is used it in oral preparation, the formula of the oral preparation For (by mass percentage):
Wherein bioactivity glass powder is using the analgesic bioactivity glass powder obtained of embodiment 4.
Manufacture craft is:Thickener is scattered in the moisturizer in addition to deionized water, by sweetener, rubbing agent, surface Activating agent is added in deionized water, and preceding liquid is poured into rear liquid, through storing, being aged, adding in preservative, after stirring evenly, then is passed through Grinding, vacuum outgas are made.
Application Example 7
Oral preparation made from above application embodiment is used for the inhibition for testing to sensitivity of tooth pain.It surveys Method for testing is:The patient of 210 sensitivity of tooth pain of adult is chosen, is divided into 7 groups at random, is respectively experimental group 1~6 and right According to group, for experimental group 1~6 using oral preparation made from Application Example 1~6, control group, which uses, biology is relieved pain in embodiment 3 Activity glass powder replaces with the oral preparation of regular silica particles, every group all using identical identical style toothbrush into Row is brushed teeth, and the alleviation situation of sensitivity of tooth pain is recorded after 3 months, obtains that the results are shown in table below:
Symptom Experimental group 1 Experimental group 2 Experimental group 3 Experimental group 4 Experimental group 5 Control group
It is clearly better 15 13 13 14 15 0
It take a favorable turn 10 11 10 12 12 0
Slightly slow down 2 3 2 2 2 3
It is invalid 3 3 4 2 1 27
It can be seen that the analgesic bioactivity glass powder of the application has the effect of good alleviation sensitivity of tooth pain.It uses It can substantially take effect within 3 months.
The emphasis of the present invention essentially consists in, and the present invention is by relieving pain bioactivity glass powder made from unique formula and technique End and the oral preparation using its preparation, play an important role of good anti-sensitivity of tooth, slow down dental pain, particularly suitable In bleeding gums, the targeted therapy of dental pain.Potassium ion is slowly released after bioactivity glass powder demeanour dentinal tubule It puts, blocks the neural traffic in dentinal tubule, reduce dental pain immediately;And bioactivity glass has long-acting tooth Antiallergic acts on, and the two complements each other, and can effectively alleviate sensitivity of tooth pain, can be effective using 3 months visible positive effects Avoid the recurrent exerbation of gingivitis.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention, Therefore identical with the above embodiment of the present invention or approximate technical characteristic is used, within protection scope of the present invention.

Claims (10)

1. a kind of preparation method for relieving pain bioactivity glass powder, which is characterized in that comprise the following steps:
(1) concentrated nitric acid is scattered in deionized water, stirred evenly, obtain dust technology;
(2) ethyl orthosilicate is taken to be dissolved in dust technology, when stirring hydrolysis 0.5~2 is small;
(3) triethyl phosphate is taken to be dissolved in step (2) acquired solution, when stirring hydrolysis 0.5~1 is small;
(4) calcium nitrate tetrahydrate is taken to be dissolved in step (3) acquired solution, stirring hydrolysis 5~15 minutes;
(5) one or both of sodium nitrate, potassium nitrate are taken, is dissolved in step (4) acquired solution, stirring hydrolysis 5~30 minutes;
(6) by step (5) acquired solution place at room temperature ageing 6~24 it is small when, solution gradually forms gel, by the gel after Continue at 60~70 DEG C ageing 24~72 it is small when;
(7) when by gel obtained by step (6), drying 6~24 is small at 110~130 DEG C, gel is gradually dry for solid;
(8) step (7) obtained solid is calcined at 650~750 DEG C 1~4 it is small when;
(9) solid that step (8) obtains is placed in ball mill ball milling, obtains bio-vitric reactive powder;
(10) the bio-vitric reactive powder that step (9) obtains and potassium-containing compound aqueous solution are mixed under ultrasound environments It closes, obtains mixed liquor;
(11) abandoning supernatant after the mixed liquor for obtaining step (10) is stood retains precipitation;
(12) precipitation that step (11) obtains is spontaneously dried at normal temperatures, obtains analgesic bioactivity glass powder.
2. the preparation method of analgesic bioactivity glass powder as described in claim 1, which is characterized in that the step (5) It is further comprising the steps of:
(5.1) citric acid is taken to be dissolved in step (5) acquired solution, stirring hydrolysis 5~15 minutes.
3. the preparation method of analgesic bioactivity glass powder as described in claim 1, which is characterized in that the step (1) Middle concentrated nitric acid and the volume ratio of deionized water are 1:8~1:45;Ethyl orthosilicate and the ratio of deionized water in the step (2) Example is 1g:(1~2) ml;It is characterized in that, the ratio of triethyl phosphate and deionized water is 1g in the step (3):(10~ 25)ml;The ratio of calcium nitrate tetrahydrate and deionized water is 1g in the step (4):(1.7~4) ml.
4. the preparation method of analgesic bioactivity glass powder as described in claim 1, which is characterized in that the step (5) The ratio of middle sodium nitrate and deionized water is (0~2.8) g:The ratio of 1ml, sodium nitrate and deionized water is (0~1.6) g: 1ml。
5. the preparation method of analgesic bioactivity glass powder as described in claim 1, which is characterized in that the step (10) Middle potassium-containing compound aqueous solution is potassium nitrate aqueous solution, potassium chloride solution, aqueous dibasic potassium phosphate solution, saleratus are water-soluble One kind in liquid, wet chemical;The ratio of the bio-vitric reactive powder and 5% potassium-containing compound aqueous solution is (0.5 ~2) g:1g.
6. the preparation method of analgesic bioactivity glass powder as claimed in claim 2, which is characterized in that the step (5.1) ratio of citric acid deionized water is (0~0.06) g in:1ml.
7. a kind of application for relieving pain bioactivity glass powder, which is characterized in that use it in oral preparation, the oral cavity system The formula of agent is:
Wherein, the rubbing agent includes analgesic bioactivity glass powder.
8. the application of analgesic bioactivity glass powder as claimed in claim 7, which is characterized in that the moisturizer is the third two Several combinations in alcohol, glycerine, polyethylene glycol, deionized water, sorbierite;The surfactant for sodium lauryl sulfate, One or more of sodium cocoyl glutamate, Cocoamidopropyl betaine, lauryl sodium sulfate, cocoyl sarcosine sodium Combination.
9. the application of analgesic bioactivity glass powder as claimed in claim 7, which is characterized in that the rubbing agent further includes The combination of one or both of calcium carbonate, calcium monohydrogen phosphate.
10. the application of analgesic bioactivity glass powder as claimed in claim 7, which is characterized in that the thickener is carboxylic The combination of one or more of methylcellulose, hydroxyethyl cellulose, guar gum, Arabic gum, xanthans;The preservative For the combination of one or more of ethylparaben, methyl hydroxybenzoate, propylben.
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CN108542832A (en) * 2018-07-11 2018-09-18 佛山皖阳生物科技有限公司 A kind of antibacterial liquid tooth paste
CN113975185A (en) * 2021-09-27 2022-01-28 深圳芳新悦享品牌管理有限公司 Toothpaste containing bioactive glass particles and preparation method thereof

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WO2010115039A2 (en) * 2009-04-01 2010-10-07 Colgate-Palmolive Company Dual action dentifrice compositions to prevent hypersensitivity and promote remineralization
CN103340896A (en) * 2013-07-10 2013-10-09 山东赛克赛斯药业科技有限公司 Duplex dentin hypersensitivity resistant composition and application thereof
CN104490608A (en) * 2014-12-26 2015-04-08 东莞市鸿元医药科技有限公司 Multiple composition for oral treatment

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WO2010115039A2 (en) * 2009-04-01 2010-10-07 Colgate-Palmolive Company Dual action dentifrice compositions to prevent hypersensitivity and promote remineralization
CN103340896A (en) * 2013-07-10 2013-10-09 山东赛克赛斯药业科技有限公司 Duplex dentin hypersensitivity resistant composition and application thereof
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Publication number Priority date Publication date Assignee Title
CN108542832A (en) * 2018-07-11 2018-09-18 佛山皖阳生物科技有限公司 A kind of antibacterial liquid tooth paste
CN113975185A (en) * 2021-09-27 2022-01-28 深圳芳新悦享品牌管理有限公司 Toothpaste containing bioactive glass particles and preparation method thereof
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