CN107095795A - A kind of sodium azulenesulfonate composition, oral-cavity article and preparation method thereof - Google Patents
A kind of sodium azulenesulfonate composition, oral-cavity article and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
- A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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Abstract
The invention discloses a kind of sodium azulenesulfonate composition, its raw material is mainly made up of sodium azulenesulfonate, zinc citrate, and the mass fraction of its raw material is respectively：0.001~3 part of sodium azulenesulfonate, 0.01~8 part of zinc citrate.The technical problem to be solved in the present invention is to provide a kind of optimal sodium azulenesulfonate composition of a kind of antibacterial and anti-sensitizing effect, oral-cavity article and preparation method thereof.
Description
Technical field
The present invention relates to dentistry configure product technical field, and in particular to a kind of sodium azulenesulfonate composition, oral-cavity article and its
Preparation method.
Background technology
Swelling and aching of gum, canker sore and the tip of the tongue erosion and pain are commonly known as oral cavity " excessive internal heat " symptom.The hair of canker sore
Life is the result of many factors comprehensive function, and it includes local trauma, stress, food, medicine, malnutrition, hormone water
It is flat to change and vitamin or microelement deficiencies, wherein, systemic disease, heredity, immune and microorganism canker sore hair
It may be played an important role in raw, development, such as lack trace element zinc, iron, lack folic acid, vitamin B12 and malnutrition etc.,
Immunologic function, the possibility of increase canker sore morbidity can be reduced；Streptococcus, helicobacter pylori, Candida albicans etc. also with mouth
Chamber ulcer is in close relations.
Gingivitis refers to acute, the chronic inflammation for occurring in gingiva tissue, and common manifestation is bleeding gums, red and swollen, distending pain,
The recurrent exerbation of canker sore is also resulted in, both interact, form vicious circle, if be possible to without effectively treatment
Cause periodontitis to Deep Development, cause the problem of tooth mobility, loss of tooth etc. are more serious.
Periodontitis is to invade the chronic inflammation of gum and periodontium, is a kind of destructive disease, many because bacterial plaque, tooth
Stone, food impaction, ill fitting prosthesis, sting wound etc. and cause and a large amount of larger teeth of virulence are grown in various focusing depths represented swelling, bacterial plaque
All pathogenic bacteria, the increased inflammation and expansion for making gum prolongs, and causes periodontal bag formation and absorption of alveolar bone, causes periodontitis.
Sodium azulenesulfonate is the abbreviation of Kessazulen sodium sulfonate, and its chemistry is entitled：1.4-dimethyl-7-isopropyl Azulene-
3-sodium sulfonate.Its parent compound is Azulene, and Kessazulen is its alkyl-substituted derivative.Azulene and its derivative are non-benzene carbon
Cyclophane aroma compounds, though it is weak compared with benzene series aromatic compound armaticity, but still electrophilic substitution reaction can occur on ring.Alkyl takes
For Azulene, especially 1.4 are methyl, and 7 are that the compound of ethyl or isopropyl has stronger bioactivity, with anti-inflammatory, are promoted
The effects such as granulation regeneration.It is water insoluble because it is a kind of blue grease, limit its application again pharmaceutically.It is carried out
Chemical constitution is transformed, and introduces chemical group, and increase is water-soluble, and the activity of this purple is obtained during water-soluble Azulene is prepared
Composition.The composition has the effect such as antibacterial, antiallergy and function of tissue regeneration, and security is again high, thus be applied to medicine,
Health products and cosmetics, and in developed countries such as Japan, Europe, sodium azulenesulfonate has started to use in oral care product.
Publication number CN101062005 patent discloses a kind of medicated toothpaste containing sodium azulenesulfonate.Publication number
CN102283949A patent discloses a kind of spraying agent for ulcer of oral cavity containing sodium azulenesulfonate, including：Sodium azulenesulfonate, benzene assistant card
Cause, Chinese medical extract, purified water, ethanol and sweetener.Publication number CN102160886A patent is disclosed containing sodium azulenesulfonate
With the compound buccal tablet of herbal mixture, the treatment for inflammation in oral cavity.Publication number CN102600122A patent discloses one
Plant the mouth paster containing Glu and sodium azulenesulfonate.The A of publication number CN 103550102 patent discloses a kind of containing field
The Chinese herbal toothpaste of seven total saposins and Kessazulen sodium sulfonate.Publication number CN 104983844A patent is disclosed with mucous membrane
The composite formula of repair function and its preparation process of preparation, composition include sodium azulenesulfonate, chitosan, Rosa roxburghii fruit powder.It is public
The number of opening CN 105748385A patent discloses a kind of improvement gum blood circulation, safeguards the tooth of periodontal and mucous membrane of mouth health
Cream, including Radix Sophorae Flavescentis extractive liquid, rhizoma imperatae extract solution, French yellow chamomile extract solution, sodium azulenesulfonate etc..Publication number CN105123353A
Patent disclose compound oral film and preparation method containing sodium azulenesulfonate.Publication number CN104644460A patent is disclosed
A kind of medicated toothpaste composition and its production and use, including Kessazulen sodium sulfonate, Paeonol, allantoin and ammonia first
Naphthenic acid.Publication number CN101590005 patent discloses biological nursing composition toothpaste, including sodium azulenesulfonate, radix notoginseng are extracted
Liquid, SOD organized enzymes and biological lysozyme.Publication number CN105031614A patent discloses a kind of Anhydroalkannin and alleviates ulcer
Oral care composition and its application, including sodium azulenesulfonate and EGF.
Sodium azulenesulfonate is pure plant extracts, with Nonsteroidal anti-inflammatory effect and anti-mucosal ulcer effect, can promote mucous membrane
Metabolism, promotes epidermal growth, enjoys modern to favor.But study and find according to inventor, it is anti-that sodium azulenesulfonate is used alone
Bacterium ability is weaker and without the effect of anti-sensitivity of tooth, and therefore, sodium azulenesulfonate, which is individually added into, can not effectively suppress to cause oral cavity disease
The bacterium of disease, alleviation a variety of oral problems such as gingivitis and sensitivity of tooth, it is many equal in this problem, the patent of the above in order to solve
It is the toothpaste with good anti-bacterial effect that toothpaste and various Chinese herbal medicines are cooperatively formed to compounding.
Zinc citrate has preferably bacteriostasis, to pathogenic bacteria such as streptococcus, Candida albicans etc. of canker sore
There is good inhibiting effect, and with control gingivitis, destroy the formation of bacterial plaque, the work of the deposition of pre- dental calculus preventing and pigment
With, and zinc ion can participate in epithelial tissue differentiation, can further promote wound healing.But, zinc citrate is single in the oral cavity
Only use can cause oral-cavity article poor taste, it is such as sour and astringent, the problems such as stimulate.
Although sodium azulenesulfonate and zinc citrate are the raw materials commonly used in toothpaste, at present not sodium azulenesulfonate with
The oral cavity composition of zinc citrate combination, therefore, inventor is during research and development, the combination to sodium azulenesulfonate, zinc citrate
Proportioning is studied, and has reached prevention and treatment canker sore, the effect of gingivitis, and improve the mouthfeel of oral-cavity article.
The content of the invention
In good taste prevent that canker sore and gingivitis can be treated the technical problem to be solved in the present invention is to provide a kind of
A kind of sodium azulenesulfonate composition, oral-cavity article and preparation method thereof.
In order to solve the above-mentioned technical problem, the present invention provides following technical scheme：A kind of sodium azulenesulfonate composition, its raw material
Mainly it is made up of sodium azulenesulfonate, zinc citrate, and the mass fraction of its raw material is respectively：0.001~3 part of sodium azulenesulfonate, lemon
Sour 0.01~8 part of zinc.
Using a kind of sodium azulenesulfonate composition of technical solution of the present invention, inventor has found under study for action, sodium azulenesulfonate with
The exclusive use of zinc citrate, it is impossible to reach the optimum efficiency that both use cooperatively, and its optimal proportion relation is in non-linear
Trend, therefore, after inventor has done substantial amounts of experimental study, has obtained proportion relation as above, compared to sodium azulenesulfonate, lemon
For the comparative example oral-cavity article that sour zinc is used alone, with more excellent antibacterial, antiallergic sense, prophylactic treatment periodontitis, gingivitis
Effect, and the soft taste of oral-cavity article do not stimulate, and Experience Degree is good.
Further, its product is toothpaste.
Further, its product is mouthwash.
Further, its product is tooth powder.
Further, the mass fraction of the raw material of its toothpaste is：0.03 part of sodium azulenesulfonate, 0.5 part of zinc citrate；
Or 0.03 part of sodium azulenesulfonate, 0.1 part of zinc citrate；
Or 0.1 part of sodium azulenesulfonate, 0.5 part of zinc citrate.
Further, the mass fraction of the raw material of its mouthwash is：0.01 part of sodium azulenesulfonate, 0.1 part of zinc citrate；
Or 0.01 part of sodium azulenesulfonate, 0.3 part of zinc citrate；
Or 0.08 part of sodium azulenesulfonate, 0.3 part of zinc citrate.
Further, the mass fraction of the raw material of its tooth powder is：0.03 part of sodium azulenesulfonate, 0.3 part of zinc citrate；Or Azulene sulphur
Sour 0.1 part of sodium, 0.3 part of zinc citrate.
Further, the purity of described sodium azulenesulfonate is more than 98%.
Further, its product also includes tooth gel or chewing gum.
The preparation method of toothpaste in sodium azulenesulfonate oral-cavity article, its operating procedure includes：
The first step, adds NMF, adds adhesive, stirs homogeneous, sequentially adds sweetener, sodium azulenesulfonate, lemon
Lemon acid zinc, surfactant, preservative, and uniform stirring；
Second step, vacuumizes addition rubbing agent, stirs homogeneous；
3rd step, adds essence, stirs homogeneous, and degassing, toothpaste completes.
Embodiment
First, a kind of sodium azulenesulfonate oral-cavity article toothpaste of the invention, the raw material and its quality of each embodiment are as shown in table 1, single
Position：G,
Table 1
A kind of sodium azulenesulfonate composition toothpaste of the present invention, the raw material and its quality of comparative example is as shown in table 2, unit：g：
Table 2
By taking embodiment 1 as an example, a kind of specifically preparation method of bright sodium azulenesulfonate oral-cavity article toothpaste：
Embodiment 1：
The first step, adds NMF glycerine 10g, adds adhesive sodium carboxymethylcellulose 0.7g, quickly stir homogeneous,
Sequentially add sweetener sorbierite 35g, saccharin sodium 0.4g, sodium azulenesulfonate 0.001g, zinc citrate 0.01g, surfactant
Lauryl sodium sulfate 2g, preservative sodium benzoate 0.3g, and uniform stirring；
Second step, vacuumizes addition rubbing agent silica 24g, stirs homogeneous；
3rd step, adds essence Mint Essence 1g, stirs homogeneous, and degassing, toothpaste completes.
2~embodiment of embodiment 7,1~comparative example of comparative example 7, its preparation method in addition to table 1, the difference of table 2, its
It is remaining consistent.
Experiment one：Bacteriostatic test
Candida albicans (C.a) can cause thrush, canker sore etc., and porphyromonas gingivalis (P.g) is to trigger periodontal
Scorching main bacteria, using disk diffusion method assess table 1,1~embodiment of embodiment 7 of table 2,1~comparative example of comparative example 7 tooth
Antibacterial potentiality of the cream to Candida albicans and porphyromonas gingivalis.Operating procedure is as follows：To cultivate has P.g concentration to be 1.5
×106CFU/mL bacteria suspensions are applied on BHIA with oese picking uniform crossover, totally 14.To cultivate has C.a concentration to be 1.0
×107Cells/mL bacteria suspensions are applied on Sabouraud glucose agar with oese picking uniform crossover, totally 14.Respectively
14 kinds of experiment toothpaste are spread evenly across on a diameter of 6mm roundlet filter paper with paste about 50mg, every kind of 6, toothpaste.It will apply
A kind of roundlet filter paper of toothpaste of cloth is divided into two groups, and each flat board pastes 3 of same toothpaste, then pastes negative control and the positive is right
According to each a piece of, every group of middle section (every kind of each culture medium of bacterium) for being attached at symmetrically respectively on culture medium.Most
Culture dish is placed in 37 DEG C of constant temperature incubator afterwards result is observed after 24h, determine antibacterial circle diameter.3 repeated experiments, with 3
Secondary average value is bacteriostatic diameter.As a result it is as shown in table 3：
Table 3
As shown in Table 3, first, 1~embodiment of embodiment 7, the consumption with sodium azulenesulfonate, zinc citrate gradually increases,
Fungistatic effect is incremented by；Second, 1~comparative example of comparative example 5, without sodium azulenesulfonate, zinc citrate any one raw material, its is antibacterial
Effect under embodiment 4, and fungistatic effect is substantially reduced；3rd, either embodiment or comparative example, in embodiment
Continue to increase any of which raw material on 4 sodium azulenesulfonate and zinc citrate consumption, the change of its fungistatic effect is no longer notable, by
This is visible, and the raw material proportioning of the present embodiment 4 is most appropriate.
Experiment two：Clinical test
1st, canker sore clinical test
Clinical oral test, choosing are carried out to the toothpaste of table 1,1~embodiment of embodiment 7 of table 2,1~comparative example of comparative example 7
Take with canker sore, the red and swollen bleeding of gum, the people of sensitivity of tooth, every group of 20 people.By physician guidance, patient uses, user
Method is completely the same, it is desirable to which patient is brushed teeth 2 times using toothpaste daily, more than 3 minutes every time, and coordinates in canker sore partial smearing
Toothpaste 2 times, during using toothpaste, other unmated any whole bodies and local application use 1~embodiment of embodiment 7 and contrast
After toothpaste in 1~comparative example of example 7, the 3rd day, further consultation inspection in 5 days, 7 days, 9 days and 12 weeks was simultaneously recorded.It is medical for the first time and subsequent
Check record content includes canker sore number, size, pain degree etc. each time, as a result as shown in table 4：
Table 4
2nd, the clinical test of gingivitis
Tooth is carried out before clinical trial in terms of carrying out gingivitis to the toothpaste shown in Tables 1 and 2, every group of 20 people, treatment
Weekly check, and record grow permanent teeth position, subjective symptoms, gingival index and plaque index.Person under inspection above does conventional clean one's teeth.Disable
Antibiotic, external used medicine and other toothpaste.Brush teeth once in the morning and once at night, more than 3 minutes every time.Check once within 7-14 days, by above-mentioned
Index is filled in a form.Observed content：Subjective sensation, including bleeding of brushing teeth, hematostaxis, excitant pain, gingival index, bacterial plaque refer to
Number, observing time is three months, as a result such as table 5：
Table 5
From table 4 and table 5 it will be seen that the proportion relation of first, composition determines therapeutic effect, embodiment 1~reality
The therapeutic effect for applying example 7 is significantly better than the therapeutic effect of 1~comparative example of comparative example 7；Secondth, the therapeutic effect of embodiment 1 is better than
2~comparative example of comparative example 4, illustrates to add a small amount of composition all than adding single sodium azulenesulfonate or zinc citrate effect good；The
3rd, 1~comparative example of comparative example, 3 pairs for the treatment of gingivitis is efficient relatively low, and the sodium azulenesulfonate of instruction sheet one is in treatment gingivitis
Effect is not protruded, and the addition of zinc citrate can be made to have complementary advantages；4th, preferably, this is just for the effect of 2~embodiment of embodiment 5
Illustrate sodium azulenesulfonate, zinc citrate only can effectively treat canker sore and gingivitis in specific proportioning, and zinc citrate
Addition can play synergy, hence it is evident that shorten canker sore healing time.
Therefore, sodium azulenesulfonate and zinc citrate are when certain proportion is used cooperatively, best results, and three months recurrence frequencies
It is low.And find that comparative example 6 and comparative example 7 have astringent taste and excitement, and zinc citrate addition is bigger, mouth by group on probation
Sense is poorer, but has added mouthfeel after sodium azulenesulfonate to be obviously improved, and good dispersion, does not stimulate gently.
2nd, a kind of sodium azulenesulfonate composition mouthwash of the invention, the raw material and its quality of each embodiment are as shown in table 6, single
Position：G,
Table 6
A kind of sodium azulenesulfonate composition mouthwash of the present invention, the raw material and its quality of its comparative example is as shown in table 7, unit：
G,
Table 7
| Comparative example 8 | Comparative example 9 | Comparative example 10 | Comparative example 11 | Comparative example 12 | |
| Sodium azulenesulfonate | 0 | 0.08 | 0 | 0.08 | 3.1 |
| Zinc citrate | 0 | 0 | 0.3 | 8.1 | 0.3 |
| Glycerine | 5.5 | 5.5 | 5.5 | 5.5 | 5.5 |
| Sorbierite | 12 | 12 | 12 | 12 | 12 |
| Poloxamer | 2 | 2 | 2 | 2 | 2 |
| Neotame | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Mint Essence | 1 | 1 | 1 | 1 | 1 |
| Water | Surplus | Surplus | Surplus | Surplus | Surplus |
| It is total | 100 | 100 | 100 | 100 | 100 |
Now illustrated with a kind of embodiment 8 of sodium azulenesulfonate composition mouthwash of the invention, illustrate the preparation method of the present invention：
Preparation process is：
The first step：NMF glycerine 5.5g, water 79.289g, sweetener neotame 0.2g are first mixed into aqueous phase,
Second step：Still further add sodium azulenesulfonate 0.001g, zinc citrate 0.01g, Mint Essence 1g, sorbierite 12g, pool
Luo Shamu 2g are mixed to after without muddy shape, and aqueous phase is slowly added to during stirring, and filtering packing, mouthwash prepares completion.
Experiment one：Bacteriostatic test
Select Candida albicans and porphyromonas gingivalis to table 6,8~embodiment of embodiment 14 of table 7, comparative example 8~
The mouthwash of comparative example 12 carries out bacteriostatic experiment, experimental method according to《Disinfection technology standard》2.1.8.2 operated, taken three times
Repeating experiment has the average value of inhibition zone diameter of bacteriostasis, as a result as shown in table 8：
Table 8
As shown in Table 8, first, 8~embodiment of embodiment 14, the consumption with sodium azulenesulfonate, zinc citrate gradually increases,
Fungistatic effect is incremented by；Second, 8~comparative example of comparative example 10, without sodium azulenesulfonate, zinc citrate any one raw material, it presses down
Bacterium effect is under embodiment 11；3rd, either embodiment or comparative example, sodium azulenesulfonate and lemon in embodiment 11
Continue to increase any of which raw material on sour zinc consumption, the change of its fungistatic effect is no longer notable, it can be seen that, the present embodiment 11
Raw material proportioning it is most appropriate.
Experiment two：Clinical test
1st, canker sore clinical test
Canker sore side is carried out to the mouthwash of table 6,8~embodiment of embodiment 14 of table 7 and 8~comparative example of comparative example 12
The clinical trial in face, every group of 20 people, by physician guidance, patient uses, and application method is completely the same, it is desirable to which patient gargles 3 daily
It is secondary, during using mouthwash, other unmated any whole bodies and local application, the 3rd day, the inspection of further consultation in 5 days, 7 days, 9 days and 12 weeks
Look into and record.The medical for the first time and subsequent record content of check each time includes canker sore number, size, pain degree etc.,
As a result it is as shown in table 9：
Table 9
2nd, the clinical test of gingivitis
In terms of gingivitis being carried out to the mouthwash shown in 8~embodiment of embodiment 14 and 8~comparative example of comparative example 12
Periodontal inspection is carried out before clinical trial, every group of 20 people, treatment, and records position of growing permanent teeth, subjective symptoms, gingival index and bacterial plaque refer to
Number.Person under inspection above does conventional clean one's teeth.Disable antibiotic, external used medicine and other effect type toothpaste.Patient gargles 3 daily
It is secondary.Check in 7-14 days once, is filled in a form by These parameters.Observed content：Subjective sensation, including bleeding of brushing teeth, hematostaxis, thorn
Swash property pain, gingival index, plaque index, observing time is three months.
As a result such as table 10：
Table 10
From table 9 and table 10 it will be seen that the proportion relation of composition determines therapeutic effect, 8~embodiment of embodiment
14 therapeutic effect is significantly better than the therapeutic effect of 8~comparative example of comparative example 12, and the therapeutic effect of embodiment 1 is better than comparative example 9
~comparative example 10, illustrates to add a small amount of composition all than adding single sodium azulenesulfonate or zinc citrate effect good, the He of comparative example 8
9 pairs of comparative example treats the efficient relatively low of gingivitis, illustrates the addition of zinc citrate and can improve the effective percentage for the treatment of gingivitis,
Have complementary advantages with sodium azulenesulfonate.Wherein preferably, this just illustrates sodium azulenesulfonate, zinc citrate to the effect of 9~embodiment of embodiment 12
Composition can effectively treat canker sore and gingivitis, and the addition of zinc citrate can play synergy, hence it is evident that shorten mouth
Chamber healing.So, sodium azulenesulfonate and zinc citrate are when certain proportion is used cooperatively, best results, and three months
Recurrence frequency is low.
It can be drawn from table 9,1. the proportion relation of composition determines therapeutic effect, 8~embodiment of embodiment 14 controls curative effect
Fruit is significantly better than the therapeutic effect of 8~comparative example of comparative example 12, and 2. the effect of 9~embodiment of embodiment 12 is best；3. by implementing
The result of example 11 and comparative example 9, comparative example 10 shows that the addition of zinc citrate can preferably alleviate canker sore and gum
Scorching symptom, under same ratio, even if only adding a kind of component less in mouthwash, effect also differs greatly, and this just illustrates Azulene
Sodium sulfonate, zinc citrate composition can effectively treat the symptom of canker sore and gingivitis, the two only with the use of when, effect
Fruit is optimal, and is not recurred substantially after three months；4. it can be seen that from the proportion relation and experimental result of embodiment 10,11,12,13,
The cooperation of the two, is not that the bigger effect of dosage is more excellent, but has mutual matching relationship, is increased although excessively adding fungistatic effect
By force, but oral mucosa is stimulated, therapeutic effect is influenceed on the contrary, for example, embodiment 10,11, although the addition of sodium azulenesulfonate is different,
But identical effect can be reached, and embodiment 12,13, the amount of three's raw material is added, but effect is but substantially reduced.
3rd, in each embodiment of the tooth powder of the composition containing sodium azulenesulfonate raw material composition and quality, unit is g, such as the He of table 11
Shown in table 12：
Table 11
Table 12
Illustrated with embodiment 15, illustrate the preparation method of tooth powder, preparation process is：First by calcium carbonate 79.979g, carbon
Sour hydrogen sodium 8g, saccharin sodium 0.5g, Herba Menthae powder essence 0.5g, Natural menthol 1g grind to form fine powder and cross 250 mesh sieves, then by Azulene sulfonic acid
Sodium powder 0.001g, zinc citrate 0.01g are made powder and crossed after 300 mesh sieves, are mixed with aforementioned mixture and lauryl sodium sulfate 10g
Uniformly, finally, every part of 10g~50g is dispensed, prepared by tooth powder completes.
Experiment one：Bacteriostatic test
Candida albicans and porphyromonas gingivalis are selected to 15~embodiment of embodiment 21, the comparative example of table 11, table 12
The toothpaste of 13~comparative example 17 carries out bacteriostatic experiment, and experimental method is:Weigh respectively after 5g tooth powder, mortar grinder add 50mL without
Bacterium distilled water, is made uniform dispersion；To cultivate has P.g concentration to be 1.5 × 106CFU/mL bacteria suspensions are equal with oese picking
Even intersection is applied on BHIA, totally 12.To cultivate has C.a concentration to be 1.0 × 107Cells/mL bacteria suspensions oese picking
Uniform crossover is applied on Sabouraud glucose agar, totally 12.Aseptic nipper gripping filter paper immerses above-mentioned tooth powder respectively
In dispersion liquid, surplus liquid is removed in beaker inwall, the scraps of paper are checked the number to be pasted into and are inoculated with the flat board for examination bacterium by sterile working, then
Paste negative control and positive control is each a piece of, every group of middle section being attached at symmetrically respectively on culture medium is (every kind of thin
Each culture medium of bacterium).Finally culture dish is placed in 37 DEG C of constant temperature incubator result is observed after 24h, determine inhibition zone straight
Footpath.3 repeated experiments, using 3 average values as bacteriostatic diameter.As a result it is as shown in table 13：
Table 13
As shown in Table 13, first, 15~embodiment of embodiment 21, the consumption with sodium azulenesulfonate, zinc citrate gradually increases
Plus, fungistatic effect is incremental；Second, 13~comparative example of comparative example 17, without sodium azulenesulfonate, zinc citrate any one raw material,
Its fungistatic effect is under embodiment 18；3rd, either embodiment or comparative example, embodiment 18 sodium azulenesulfonate and
Continue to increase any of which raw material on zinc citrate consumption, the change of its fungistatic effect is no longer notable, it can be seen that, this implementation
The raw material proportioning of example 18 is most appropriate.
Experiment two：Clinical test
1st, to the clinical test of canker sore
Oral cavity is carried out to the tooth powder shown in table 11,15~embodiment of embodiment 21 of table 12 and 13~comparative example of comparative example 17
Clinical trial in terms of ulcer, every group of 20 people, by physician guidance, patient uses, and application method is completely the same, it is desirable to which patient is daily
Gargle 3 times, during using tooth powder, other unmated any whole bodies and local application, the 3rd day, further consultation in 5 days, 7 days, 9 days and 12 weeks
Check and record.The medical for the first time and subsequent record content of check each time includes canker sore number, size, pain degree
Deng.
As a result such as table 14：
Table 14
2nd, to the clinical test of gingivitis
Carried out before clinical trial in terms of carrying out gingivitis to the tooth powder shown in table 11 and table 12, every group of 20 people, treatment
Periodontal is checked, and records grow permanent teeth position, subjective symptoms, gingival index and plaque index.Person under inspection above does conventional clean one's teeth.Stop
With antibiotic, external used medicine and other toothpaste.Brush teeth once in the morning and once at night, more than 3 minutes every time.Check once within 7-14 days, by upper
Index is stated to fill in a form.Observed content：Subjective sensation, including bleeding of brushing teeth, hematostaxis, excitant pain, gingival index, bacterial plaque refer to
Number, observing time is three months.
As a result such as table 15：
Table 15
From table 14 and table 15 it will be seen that the proportion relation of composition determines therapeutic effect, embodiment 15~implementation
The therapeutic effect of example 21 is significantly better than the therapeutic effect of 13~comparative example of comparative example 17, and the therapeutic effect of embodiment 15 is better than contrast
14~comparative example of example 15, illustrates to add a small amount of composition all than adding single sodium azulenesulfonate or zinc citrate effect good, contrast
14 pairs of example 13 and comparative example treat the efficient relatively low of gingivitis, illustrate the addition of zinc citrate and can improve treatment gingivitis
Effective percentage, has complementary advantages with sodium azulenesulfonate.Wherein 16~embodiment of embodiment 17 effect preferably, this just illustrate sodium azulenesulfonate,
Zinc citrate composition can effectively treat canker sore and gingivitis, and the addition of zinc citrate can play synergy, bright
It is aobvious to shorten canker sore healing time.So, sodium azulenesulfonate and zinc citrate are when certain proportion is used cooperatively, best results,
And three months recurrence frequencies are low.
It can be drawn from table 14,1. the proportion relation of composition determines therapeutic effect, the treatment of 15~embodiment of embodiment 21
Effect is significantly better than the therapeutic effect of 13~comparative example of comparative example 17；2. the effect of 16~embodiment of embodiment 20 is best；3. pass through
The result of embodiment 18 and 14~comparative example of comparative example 16 shows that the addition of zinc citrate can preferably alleviate canker sore
With the symptom of gingivitis, under same ratio, even if only adding a kind of component less in tooth powder, effect also differs greatly, and this just says
Bright sodium azulenesulfonate powder, zinc citrate composition can effectively treat the symptom of canker sore and gingivitis, and the two only makes in cooperation
Do not recurred substantially after used time, best results, and three months；4. from the proportion relation and experimental result of embodiment 17,18,19,20
It can be seen that, the cooperation of the two, be not that the bigger effect of dosage is more excellent, but have mutual matching relationship, although excessive add suppression
Bacterium effect strengthen, but stimulate oral mucosa, therapeutic effect is influenceed on the contrary, for example, embodiment 17,18, although sodium azulenesulfonate plus
Enter amount different, but identical effect can be reached, embodiment 19,20, the amount of three's raw material is added, but effect is bright
Aobvious reduction.
From a kind of secondary, of the invention sodium azulenesulfonate composition, toothpaste, mouthwash, tooth powder are in sodium azulenesulfonate, citric acid
Zinc is coordinated with suitable ratio, can reach the effect of optimal treatment canker sore and gingivitis.
For those skilled in the art, toothpaste, mouthwash, tooth powder are considered technical solution of the present invention and are relatively applicable
Oral-cavity article, but the present invention is not limited in being added into toothpaste, mouthwash, tooth powder, tooth gel, chewing gum etc. other
Oral-cavity article is equally applicable.Without departing from the inventive concept of the premise, several modifications and improvements can also be made, these
Protection scope of the present invention should be considered as, these effects and practical applicability for implementing all without the influence present invention.
Claims (10)
1. a kind of sodium azulenesulfonate composition, it is characterised in that its raw material is mainly made up of sodium azulenesulfonate, zinc citrate, and it is former
The mass fraction of material is respectively：0.001~3 part of sodium azulenesulfonate, 0.01~8 part of zinc citrate.
2. sodium azulenesulfonate oral-cavity article according to claim 1, it is characterised in that：Its product is toothpaste.
3. sodium azulenesulfonate oral-cavity article according to claim 1, it is characterised in that：Its product is mouthwash.
4. sodium azulenesulfonate oral-cavity article according to claim 1, it is characterised in that：Its product is tooth powder.
5. sodium azulenesulfonate oral-cavity article according to claim 2, it is characterised in that：The primary raw material mass fraction of its toothpaste
For：0.03 part of sodium azulenesulfonate, 0.5 part of zinc citrate；
Or 0.03 part of sodium azulenesulfonate, 0.1 part of zinc citrate；
Or 0.1 part of sodium azulenesulfonate, 0.5 part of zinc citrate.
6. sodium azulenesulfonate oral-cavity article according to claim 3, it is characterised in that：The primary raw material mass parts of its mouthwash
Number is：0.01 part of sodium azulenesulfonate, 0.1 part of zinc citrate；
Or 0.01 part of sodium azulenesulfonate, 0.3 part of zinc citrate；
Or 0.08 part of sodium azulenesulfonate, 0.3 part of zinc citrate.
7. sodium azulenesulfonate oral-cavity article according to claim 4, it is characterised in that：The mass parts of the primary raw material of its tooth powder
Number is：0.03 part of sodium azulenesulfonate, 0.3 part of zinc citrate；
Or 0.1 part of sodium azulenesulfonate, 0.3 part of zinc citrate.
8. the sodium azulenesulfonate oral-cavity article according to claim 5 ~ 7 any one, it is characterised in that：Described sodium azulenesulfonate
Purity be more than 98%.
9. sodium azulenesulfonate oral-cavity article according to claim 8, it is characterised in that：Its product also include tooth gel or
Chewing gum.
10. the preparation method of toothpaste in sodium azulenesulfonate oral-cavity article according to claim 2, it is characterised in that：It is operated
Step includes：
The first step, adds NMF, adds adhesive, stirs homogeneous, sequentially adds sweetener, sodium azulenesulfonate, citric acid
Zinc, surfactant, preservative, and uniform stirring；
Second step, vacuumizes addition rubbing agent, stirs homogeneous；
3rd step, adds essence, stirs homogeneous, and degassing, toothpaste completes.
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| CN108743442A (en) * | 2018-07-17 | 2018-11-06 | 天津中鼎生物医学科技有限公司 | Sodium azulenesulfonate, Cetylpyridinium Chloride and zinc ion compound formula mouth wash and preparation method |
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| CN106265423A (en) * | 2016-08-23 | 2017-01-04 | 广州立白企业集团有限公司 | Having relieves inflammation or internal heat disappear pain effect oral care composition |
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| CN106265423A (en) * | 2016-08-23 | 2017-01-04 | 广州立白企业集团有限公司 | Having relieves inflammation or internal heat disappear pain effect oral care composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108743442A (en) * | 2018-07-17 | 2018-11-06 | 天津中鼎生物医学科技有限公司 | Sodium azulenesulfonate, Cetylpyridinium Chloride and zinc ion compound formula mouth wash and preparation method |
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