CN105902407A - Lysozyme hydrochloride toothpaste and preparation method thereof - Google Patents
Lysozyme hydrochloride toothpaste and preparation method thereof Download PDFInfo
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- CN105902407A CN105902407A CN201610308798.5A CN201610308798A CN105902407A CN 105902407 A CN105902407 A CN 105902407A CN 201610308798 A CN201610308798 A CN 201610308798A CN 105902407 A CN105902407 A CN 105902407A
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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
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/66—Enzymes
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- A—HUMAN NECESSITIES
- 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
Abstract
The invention discloses a lysozyme hydrochloride toothpaste and a preparation method thereof. The lysozyme hydrochloride toothpaste comprises an active ingredient and auxiliary materials, wherein the active ingredient is lysozyme hydrochloride, and the weight percentage of lysozyme hydrochloride in toothpaste is 0.3-4.6 percent; the auxiliary materials are any acceptable auxiliary materials for preparing the toothpaste, and comprise a humectant, a thickener, a foaming agent, a protective agent, an abrasive, a flavoring agent and other additives. The lysozyme hydrochloride toothpaste has the advantages that the cleaning capability is strong, the mouth feel of tooth brushing is excellent, the effect of treating periodontal diseases, such as inhibiting of dental plaque and/or relieving of gingivitis and periodontitis, are realized, and more safety in use is realized.
Description
Technical field
The present invention relates to a kind of toothpaste and preparation method thereof, particularly to a kind of lisozima toothpaste and preparation method thereof, belong to
Daily chemical products field.
Background technology
Oral cavity is actually the environment of an opening, there is the normal of a large amount of antibacterial, the most mostly non-pathogenic in oral cavity
In bacterium.They are maintaining the balance of Oral health behaviours environment, assist oral cavity function, keep the health in oral cavity, have important work
With.The microecological balance mainly human mouth maintaining oral cavity has many Immunity active factors in action at normal condition.Certain is different
In the case of Chang, occurring the unbalance of Tiny ecosystem to cause disease to occur at certain position in oral cavity, external antibiotic substance can suppress antibacterial
Undue growth, is but difficult to maintain rightly the microecological balance in oral cavity.Unsuitable medicament selection can not only suppress or kill
Oral cavity pathogen, also kills oral cavity simultaneously and resides commensalism bacterium, thus be likely to form and affect the long-term slow of Oral health behaviours environment
Property stimulating factor, it is also possible to make conditioned pathogen in oral cavity produce drug resistance, and reduce oral cavity and respectively organize damage
Self-healing ability.Therefore, it is suggested that various medicated toothpaste should be all short-period used, exploitation can control rather than eliminate pathogenic bacterium or elimination
The medicated toothpaste of special mechanism of causing a disease is significant.
Toothpaste is cleaning supplies conventional in daily life, has the longest history.Along with the development of science and technology, work
Updating and perfect of skill equipment, various types of toothpaste are come out one after another, and quality and the class of product improve constantly, present tooth
Cream kind, by single clean type toothpaste, develops into great variety of goods, diverse in function, the Mobyneb toothpaste of up to a hundred brands,
Meet the needs of different levels level of consumption.Toothpaste quality quality, directly affects the healthy of people.At present, China
The toothpaste produced has following several；Acid-proof antiallergic effective type toothpaste, anti-tartar oral cavity cleaning, alleviate gingivitis Chinese medicinal toothpaste,
Anticarious IgY and IgY toothpaste, mica filled polypropylene etc., function above toothpaste is all to add on the basis of lotion of toothpaste substrate
External functional chemical or Chinese herbal medicine etc..Oral cavity is the common site of anaerobic infection, and Clinical Laboratory finds, periodontitis
Pathogenic bacterium 75% are anaerobe.Owing to position, oral cavity lacuna is more, beneficially bacterial growth.Research display, adult's periodontal is sent out
Time scorching, the ratio shared by gram-negative anaerobic bacteria is about 75%, when treating some infectious disease such as oral cavity, and life-time service
The chemical substance of external interpolation is as antibacterial, and effect is the most bad, instead results in dysbacteriosis, increases the weight of the state of an illness.The annual tooth of China
Being in great demand of cream, is badly in need of finding a kind of pure natural, has again the additive of fine antibiotic effect.Therefore, in this respect
Carry out studying important in inhibiting.
Chinese patent document CN104382762A discloses a kind of deodorization and sterilization dentifrice composition, and it is mainly with containing weight hundred
Proportion by subtraction is the mixture of Folium Baeckeae extract and zinc ion of 0.1～5%, and Folium Baeckeae extract with zinc ion is by weight percentage
5:1.Above patent well provides the compositions of a kind of deodorization and sterilization toothpaste, is disadvantageous in that, because toothpaste is life-time service,
The mixture of the zinc ion that upper patent is used can produce zinc poisoning phenomenon.
Chinese patent document CN101342140A discloses a kind of silver-zinc powder toothpaste, described toothpaste by calcium carbonate, sodium benzoate,
Saccharin sodium, glycerol, lauryl alcohol sulfuric acid ester sodium, Colla cornus cervi, quintessence oil, silver sulfadiazine, zinc sulfadiazine become to be grouped into.Above
Patent is disadvantageous in that: using silver sulfadiazine, zinc sulfadiazine to be chemistry antibacterial, life-time service easily instead results in
Dysbacteriosis, increases the weight of the state of an illness.
Chinese patent document CN101327177A discloses red sage root toothpaste, and this patent adds Radix Salviae Miltiorrhizae in toothpaste, and weak point is
This technology have ignored toothpaste as article of everyday use, to be used by everyone, its safety it cannot be guaranteed that.
Chinese patent CN1244390A discloses medical metronidazole toothpaste, it is characterised in that it is with ordinary toothpaste as substrate,
Add and join certain proportion metronidazole composition.This patent is disadvantageous in that, the chemical substance of the external interpolation of life-time service as antibacterial,
Drug resistance flora can be produced produce, increase the weight of the state of an illness.
Chinese patent CN102895147A discloses a kind of has antiinflammatory and the toothpaste of antiallergic effect and processing technology thereof, its feature
It is, including anti-inflammation hemostasia active component, antiallergic analgesic activity composition and base ingredients；Described anti-inflammation hemostasia active component includes
The component of following mass percent: paeonol, glycyrrhizic acid dipotassium salt, tranamic acid, plant fiber crops element；Described antiallergic analgesic activity becomes
Point include the component of following mass percent: eugenol, potassium nitrate, plant fiber crops element；Surplus is base ingredients, preservative and water.
This patent is disadvantageous in that, styptic activity adds tranamic acid etc., and adds antiallergic analgesic activity such as potassium nitrate etc.；For a long time
The chemical substance using external interpolation all can affect the safety of toothpaste life-time service.
In sum, all there is defect in various degree in above prior art, makes application in daily life be very limited.For
Meeting vast demand, those skilled in the art are seeking to develop safe efficient the most always, quality controllable, use
Toothpaste easily.
Lisozima is a kind of from the middle clearly a kind of alkaline protease that can decompose mucopolysaccharide extracted of Fresh Egg, can be in gastrointestinal
Digested and absorb, to human non-toxic evil effect, be food preservative, nutrient and healthcare products and the medicine that a kind of safety coefficient is the highest.
Lisozima is the hydrolyzed yeast of mucopolysaccharide.Due to the decomposition of mucopolysaccharide, while coordinating interior or topical medicine, serve
Sterilization (bacteriolyze) to inflammation i.e. microorganism acts on and strength antiinflammation.Lysozyme can also effectively treat and prevent to infect
Property inflammation, non-infectious inflammation, to the prevention of the periodontals such as oral disease, particularly alveodental suppression, control and treat, rising
Arrive very important effect.Lisozima can also be combined with the acidic materials of various induction inflammation so that it is inactivation, and strengthens
Antibiotic and the curative effect of other drug, improve the mucopolysaccharide metabolism of periplast, thus be conducive to repairing by the tissue of inflammation damnification.
Lisozima can activate platelet, improves tissue local circulatory disturbance, decomposes pus, strengthens local and defends, thus preferably
Play the effects such as antibacterial, antiinflammatory, pain relieving.
At present, lisozima preparation is mainly oral formulations, is clinically used for acute and chronic pharyngitis, stomatocace and expectoration
Difficulty etc..Up to now, lisozima applies in toothpaste that there is not been reported.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of lisozima toothpaste, this toothpaste has high level of cleanliness power, brush
The age of a draught animal is felt excellent, can suppress dental plaque and/or alleviate effect of the periodontal such as gingivitis and periodontitis, and uses safety；This
Invention also provides for the preparation method of this toothpaste.
Term illustrates:
Lisozima, English name Lysozyme hydrochloride, is from the middle clearly a kind of mucopolysaccharide extracted of Fresh Egg
Alkaline protease, becomes lysozyme chloride, CAS accession number 9066-59-5 with chloride binding, and market is commercially available.
Room temperature: refer to the ambient temperature residing for experimental implementation, the present invention controls in the range of 15～30 DEG C.
Technical scheme is as follows:
A kind of lisozima toothpaste, including active component and adjuvant, described active component is lisozima, and it is at toothpaste
In percentage by weight be 0.3～4.6%.
Lisozima in toothpaste of the present invention can play following effect: (1) is combined with the acidic materials of various induction inflammation, makes
Its inactivation, and strengthen the curative effect of antibiotic and other drug；(2) improve the mucopolysaccharide metabolism of periplast, thus be conducive to
Repair by the tissue of inflammation damnification；(3) activate platelet, improve tissue local circulatory disturbance, decompose pus, strengthen local
Defence；(4) prevent wound infection, preferably play the effects such as antibacterial, antiinflammatory, pain relieving, stop extraneous bacterial invasion, and
Impaired skin there is Healing.
According to the present invention, described adjuvant is to prepare the acceptable any adjuvant needed for toothpaste, according to known in the art,
Described adjuvant includes wetting agent, thickening agent, foaming agent, protective agent, abrasive, correctives and/or other additives.
According to the invention it is preferred to, described wetting agent is glycerol and/or sorbitol, thickening agent be carboxymethyl cellulose and/or
Sodium alginate, foaming agent is sodium lauryl sulphate, and protective agent is glycine and/or empgen BB, and abrasive is carbon
Acid calcium and/or calcium phosphate, correctives is essence and/or saccharin sodium, and other additives include silicon dioxide and deionized water.
Lisozima used in the present invention is this area convenient source, commercial products.Its quality health portion drug standard 98
Version two-shift system provisioning request, wherein the titer of every 1mg must not be less than 6250 units (enzyme activity).
The present invention provides following preferred technical scheme:
A kind of lisozima toothpaste, is made up by mass parts of following raw material:
According to the present invention, further preferred that
A kind of lisozima toothpaste, is made up by mass parts of following raw material:
The most preferred:
A kind of lisozima toothpaste, is made up by mass parts of following raw material:
Or,
A kind of lisozima toothpaste, is made up by mass parts of following raw material:
Or,
A kind of lisozima toothpaste, is made up by mass parts of following raw material:
Lisozima toothpaste of the present invention, what the raw material that used was not specified is conventional commercial products.
The preparation method of a kind of lisozima toothpaste, comprises the steps:
(1) abrasive calcium carbonate or calcium phosphate being carried out micronizing, calcium carbonate crosses 400 mesh sieves, obtains with grain size analysis with laser grain size analyzer
Mean diameter is 15～21 μm；Calcium phosphate crosses 350～400 mesh sieves, and obtaining mean diameter with grain size analysis with laser grain size analyzer is 5～19 μm；
(2) step (1) addition deionized water is configured to quality than calcium carbonate or calcium phosphate deionized water=1 5～10, enters
Row milling treatment of colloid, makes suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 10～30% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～80 DEG C, rotating speed is again
60～90r/min, time 30～50 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～50r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～60 minutes, deposit in being delivered to sterilized tank, standby at 60～80 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 40～60 DEG C, is opened cutter low speed 1000～1750r/min and is sheared 8～10 minutes, then at a high speed 2500～
3000r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～90r/min, continues stirring 5～10
Minute, it is 30～50r/min stirrings at speed of agitator the most again, starts cooling, stop stirring when being cooled to 30～35 DEG C, so
After more than under 0.096MPa vacuum, be 30～50r/min at speed of agitator, mixing time 30～50min, make mastic,
Pack and get final product.
According to currently preferred, the colloid solution described in step (3), according to " Chinese Pharmacopoeia two annex VIG of version in 2010
Second method " use NDJ-1 type Rotary Viscosimeter, with No. 4 rotors, rotating speed is 6 turns per minute, the viscosity of material, at 25 DEG C
Time material dynamic viscosity be 20～30Pa.s.
According to the present invention it is further preferred that the preparation method of a kind of lisozima toothpaste, comprise the steps:
(1) abrasive calcium carbonate or calcium phosphate being carried out micronizing, calcium carbonate crosses 400 mesh sieves, obtains with grain size analysis with laser grain size analyzer
Mean diameter is in 15～21 μm；Calcium phosphate crosses 400 mesh sieves, obtains mean diameter in 5～12 μm with grain size analysis with laser grain size analyzer；
(2) step (1) addition deionized water is configured to quality than calcium carbonate or calcium phosphate deionized water=1 5～8, enters
Row milling treatment of colloid, makes suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 20～30% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～80 DEG C, rotating speed is again
60～80r/min, time 30～40 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～50r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～40 minutes, deposit in being delivered to sterilized tank, standby at 60～80 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 40 DEG C, is opened cutter low speed 1000～1200r/min and is sheared 8～10 minutes, then at a high speed 2500～
2800r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～90r/min, continues stirring 5～10
Minute, it is 30～40r/min stirrings at speed of agitator the most again, starts cooling, stop stirring when being cooled to 30～35 DEG C, so
After more than under 0.096MPa vacuum, be 30～40r/min at speed of agitator, mixing time 30～40min, make mastic,
Pack and get final product.
Below in conjunction with experimental example, the present invention is described further, but is not limited to this.
Experimental example 1, abrasive (calcium carbonate or calcium phosphate) particle diameter and the determination experiment of particle diameter distribution
Calcium carbonate, calcium phosphate are a kind of inorganic compound, experiment proves that as abrasive composition no matter the most size-reduced calcium carbonate
Shared recipe quantity number, all can leave the sand type of discomfort in the oral cavity, thus select calcium carbonate or calcium phosphate through micronizing,
Fine and smooth mastic can produce happy sensation in the oral cavity, and coarse mastic then can produce sand type.
Sieve analysis method is used to measure the particle diameter distribution of calcium carbonate, calcium phosphate.Calcium carbonate, calcium phosphate granules are carried out, and every batch to 50g
Calcium carbonate, calcium phosphate granules are measured.Using pulp classifier and standard testing sieve to be measured, amplitude is 1.5mm, during vibration
Between be 20min.The specification of sieve is 200 mesh, 250 mesh, 300 mesh, 350 mesh and 400 mesh.Use purchased from Marlven2000
Laser diffraction particle size analysis-e/or determining calcium carbonate, calcium phosphate granules screening under mean diameter, calcium carbonate, calcium phosphate average
Particle diameter and particle diameter distribution are as shown in table 1.
Particle size distribution method (D50): Malvern2000 or the suitable laser particle size analyzer of performance, take this product about 0.12g,
Making detector shading rate 8～20% scope, add water 800mL, stirs 15 minutes with the rotating speeds of 3000 turns per minute or with every point
The rotating speed stirring that clock is 3000 turns, and the most ultrasonic 2～3 minutes (ultrasonic power 16W, amplitude 3 μm), check, the company of taking in accordance with the law
The continuous meansigma methods measuring 3 times, should meet following table regulation.
Table 1 calcium carbonate, the mean diameter of calcium phosphate and particle diameter distribution
Interpretation of result: along with the increase of mesh number, calcium carbonate, calcium phosphate granules amount also increase as, the granule under screening, averagely
Particle diameter constantly reduces.
By the preparation method of embodiment 1, prescription is constant, selects calcium carbonate or the different mesh numeral system of calcium phosphate granules for toothpaste, examines
Examine calcium carbonate or calcium phosphate toothpaste mouthfeel；It is shown in Table 2:
The impact on mouthfeel of table 2 different meshes
The purpose of this experimental example is the average particle size range that assessment is different, the impact on lysozyme toothpaste feature, and confirms selected
Granule mesh number scope, i.e. 400 mesh i.e. calcium carbonate mean diameter is in 15～21 μm；350 mesh～400 mesh i.e. calcium phosphate average particle
Footpath is in 5～19 μm；Above particle diameter is rational for the present invention.
Protectant research experiment in experimental example 2, lysozyme toothpaste
Lisozima is very sensitive to temperature, and temperature, under the conditions of 40～60 DEG C, investigates addition complexing of glycin dosage molten to hydrochloric acid
The protective effect that bacterium enzymatic activity plays；The results are shown in Table 3.
Table 3 glycine consumption the selection result unit (g)
Lisozima toothpaste is to adding lisozima Potency Analysis produced by glycine；It is shown in Table 4.
Table 4 lisozima Potency Analysis
Prescription evaluation and result:
Prescription 1: transparency liquid, but titer is low；
Prescription 2: transparency liquid, but titer is relatively low；
Prescription 3: transparency liquid, titer plateaus；
Prescription 4: transparency liquid, titer plateaus；
Prescription 5: transparency liquid, titer plateaus.
Interpretation of result: above prescription is transparency liquid；In prescription 1,2, glycine consumption is low, causes lisozima titer relatively
Low, be not suitable for the requirement of this preparation.Prescription 3,4,5 is transparency liquid；Lisozima titer plateaus, is suitable for requirement.Really
Determine glycine consumption in prescription 3,4,5, as prescription of the present invention, it can be seen that add complexing of glycin agent to lisozima
Activity plays a protective role.
Lisozima toothpaste stability influence is tested by experimental example 3, empgen BB
In the toothpaste containing lisozima, sodium lauryl sulphate such teepol isoiony composition,
When coordinating with lisozima, can generate white precipitate, cause lisozima activity to reduce, lisozima toothpaste does not reaches
Expected effect, makes the application of lisozima encounter difficulty.And by the method for non-ionic components preparation toothpaste, again because of it
Relatively low foaminess is had to have impact on use.
The purpose of invention is exactly to research and solve the problems referred to above further, to obtain the toothpaste stable containing lisozima, carries out
Research, its objective is: add empgen BB interfacial activity protective agent in lisozima and teepol,
On the basis of keeping lisozima stable, can effectively improve foaminess.
1, test: the preparation of sample is by preparation method in embodiment 1, and adding empgen BB interfacial activity protective agent is
Lisozima toothpaste sample 2.Preparation method in embodiment 1, being added without empgen BB interfacial activity protective agent is salt
Acid lysozyme toothpaste sample 1.
2, Testing index: lisozima Activity determination, the sensory evaluation of foaminess
3, measurement result: preserve the lisozima activity in 1,5,10,24 months lisozima toothpaste when 40 DEG C, with
And the sensory evaluation of foaminess is shown in Table 5.
Table 5 empgen BB is to lisozima toothpaste stability
As the interfacial activity protective agent empgen BB of the present invention, thus obtain one and do not damaged lisozima work
Property and keep the good toothpaste of foaminess simultaneously.
Experimental example 4, lysozyme lotion of toothpaste rheology are studied
The mixture that toothpaste is made up of many kinds of substance.Wherein affect the principal element of paste rheological be abrasive, wetting agent,
Thickening agent.At present a certain composition (such as thickening agent) is confined in formula to toothpaste viscosity for the research in terms of toothpaste rheology
Impact, the shear stress rheology study to toothpaste.Establish the rheological assessment standard of toothpaste, so that it may objectively according to rheology
Learn mensuration and determine that formula forms.Test by normal mastic inspection project, it was demonstrated that the mastic prepared has good rheological characteristic,
Meet the requirement producing and using.
1, primary raw material, instrument and rheological data assay method
1.1 raw materials: carboxymethyl cellulose (CMC), sodium alginate；
1.2 instruments: rotary viscosimeter；High shearing mixing emulsor；Rotary vacuum pump；Reinforcement electric blender；
1.3 rheological data assay methods
After determinand places 24hs, at room temperature survey its viscosity number and then determinand is sheared in high shearing mixing emulsor 5min
(rotating speed is 4200 turns/min), surveys rapidly its viscosities il2, with [η1(η1-η2)/η1] × 100 represent thixotropic size.
2, the selection of thickening agent
By carboxymethyl cellulose (CMC) 0.5～1.6g, sodium alginate 0.5～1.6g, mix with deionized water 160g respectively after use
Magnetic force heating stirrer heats, and stirs under the conditions of 60～80 DEG C to mastic homogeneous transparent, surveys its viscosity after standing 24hr
And thixotropy, result see Fig. 1,2.
As seen from Figure 1, Figure 2, under same amount, the viscosity of carboxyl methyl cellulose is more than sodium alginate；But carboxymethyl is fine
The thixotropy of dimension element CMC is less than sodium alginate.Certain denseness and thixotropy must be had to ensure mastic for normal mastic
Stable and the satisfied requirement produced and use.Carboxyl methyl cellulose thixotropy is poor, is unsuitable for being used alone；Sodium alginate touches
Degeneration is good, but viscosity is too low.For obtaining preferable viscosity and thixotropy, make compounding to carboxyl methyl cellulose and sodium alginate
With, learn from other's strong points to offset one's weaknesses.
Table 6 compounds the mastic fluid rheology data of thickening agent
According to the rheological data in table 6, in the case of guarantee viscosity and thixotropy meet the requirements, reduce consumption as far as possible, select
Quality is than carboxyl methyl cellulose: sodium alginate 2:1 is that (i.e. in above-mentioned formula, carboxyl methyl cellulose accounts for 2 to thickening agent
Part (W/W), sodium alginate accounts for 1 part (W/W)).
Experimental example 5: wetting agent is studied at the mastic liquid choice experiment of lysozyme toothpaste
With carboxyl methyl cellulose, sodium alginate as thickening agent；Glycerol, sorbitol make wetting agent, by embodiment 1 method system
Glue, the rheological data measuring mastic liquid is shown in Table 7.
Table 7 wetting agent rheological data to mastic liquid
As shown in Table 7, selection 1,2,3 groups is appropriate.The most currently preferred wetting agent is made up of glycerol and sorbitol, its
Middle glycerol and sorbitol amount ratio are 1.0～3.0:0.5～0.7 weight ratio (W/W).
Experimental example 6: lisozima toothpaste oral cavity irritation on mucous membrane is tested
1, test material
(1) material: lisozima toothpaste, the lisozima toothpaste of embodiment 1 preparation；Excipient (blank toothpaste): use
The adjuvant of embodiment 1, by the preparation method of embodiment 1, is not added with lisozima；
(2) animal: Golden Hamster, grade is regular grade, Shandong University's Experimental Animal Center provide, and 24 male, body weight 120g
±20g。
2, oral mucosa irritation test method
Packet: take fasting 12h Golden Hamster 24, be randomly divided into lisozima toothpaste intact mucosa group, hydrochloric acid by body weight
Lysozyme toothpaste breakage mucosa group, excipient (blank toothpaste) intact mucosa group, excipient (blank toothpaste) damaged mucosa group,
Often group 6.Self left and right sides mucosa compares, and left side is administered, and right side is as blank.Before being administered, the aseptic pin of 24h is drawn
Broken mucosa group Golden Hamster left and right sides buccal mucosa.
It is administered: Golden Hamster being taken dorsal position and fixes, lisozima toothpaste group takes precise lisozima toothpaste 16mg
Putting into cheek pouch on the left of its oral cavity, excipient (blank toothpaste) group takes excipient 16mg and puts into cheek pouch on the left of its oral cavity.Often
Day is administered 3 times, continuous 3d, the lisozima toothpaste zest to Golden Hamster oral mucosa, observes to evaluate and comments with histology
Valency.Under optical frames, tissues observed morphological change is marked by table 8；
Observe and record the mucosa with medicament contact to mark by table 9 with or without erythema, erosion and edema etc.；
Table 8 oral cavity tissue reaction microscope standards of grading
Table 9 oral stimulation reaction standards of grading
(1) during testing, all animal activities are normal, and diet is normal, has no systemic adverse reactions.Each test group has no oral cavity
Mucosa is congested, hemorrhage, rotten to the corn or ulcer.Each group is administered 1:3 chamber, side mucosa and compares with control sides and have no difference, hydrochloric acid bacteriolyze
Enzyme toothpaste and excipient (blank toothpaste) group compares and has no difference.Reacting standards of grading by oral stimulation, the score of each treated animal is shown in
Table 10.
The reaction scoring of table 10 oral stimulation
Result: gross examination of skeletal muscle display lisozima toothpaste is the most non-stimulated to oral cavity intact mucosa and the damaged mucosa of Golden Hamster
Property；Histopathologic examination's display lisozima toothpaste does not the most produce the pathology such as inflammation change intact mucosa and damaged mucosa
Become；Histopathology scoring display lisozima toothpaste is to intact mucosa and the damaged equal nonirritant of mucosa.
(2) histological observation evaluation: biopsy of oral mucosa is evaluated as by pathology: each group of intact mucosa is carried out microscopy, observes
The pathological states such as its mucosal epithelium, inflammatory cell infiltration, vascular reaction and interstitial edema, find 4 groups of no significant differences, prompting
Lisozima toothpaste is to pathological changes such as the oral cavity intact mucosa NIP stimulations of Golden Hamster；Damaged each group of mucosa is carried out
Microscopy, observes its mucosal epithelium, inflammatory cell infiltration, vascular reaction and asks the pathological states such as matter edema, finding 4 groups without substantially
Difference, points out the pathological changes such as the lisozima toothpaste oral cavity intact mucosa NIP stimulation to Golden Hamster；Separately there is observation
Find, in lisozima toothpaste breakage mucosal drug delivery group, have under 4 example mirrors and show that Submucosa has good granulation tissue to be formed,
Prompting lisozima toothpaste has certain facilitation to the repair process of oral cavity breakage mucosa.Microscope is reacted by oral cavity tissue
Classification of assessment system, it is determined that the score of each treated animal is shown in Table 11.
The reaction microscope scoring of table 11 oral cavity tissue
Conclusion: the lysozyme toothpaste oral mucosa nonirritant to Golden Hamster, therefore lysozyme toothpaste is safety.
Experimental example 7: the therapeutical effect of periodontal disease is tested by lisozima toothpaste
Gingivitis and periodontitis are oral cavity commonly encountered diseases, and prevalence is high, and research proves that antibacterial and bacterial plaque are to cause gingivitis and periodontitis
Initiation factor, therefore control and remove the important measures that bacterial plaque is prevention of gingivitis and periodontitis, medicated toothpaste is observed in this research
To gingivitis and the effect of periodontitis, observe the medicated toothpaste improvement situation to gingivitis and periodontitis simultaneously.
1, materials and methods
The lysozyme toothpaste of 1.1 matched group toothpaste Flos Lonicerae odontopathy pastes, test group toothpaste Examples 1 preparation.
1.2 Therapeutic Method: test group morning and evening every day lisozima toothpaste is brushed teeth, and half an hour after of brushing teeth is not taken food.Matched group is continued to use
Former custom morning and evening Flos Lonicerae odontopathy paste is brushed teeth.Patients with periodontitis uses observation 14d continuously, and gingivitis patients uses observation 7d continuously.
Patient is advised in test to keep original oral sanitary habit, to avoid the impact of other factors.
Inclusive criteria: 186 examples, age l6～73 years old, average 37.3 years old, wherein test group 97 example, matched group 89 example.
2, observation index: for the ease of observed and recorded and statistics, indices is all converted into score value by us.
2.1 pain: 3, have an intense pain；2, moderate pain；L, mild pain；0, the most bitterly.
2.2 Movable degree: 3, III loosens；2, II loosens；L, I loosen；0, normal.
2.3 masticatory functions: 3, soft diet can not be chewed；2, hard food can not be chewed；L, hard food can be chewed, but slightly pain；0, just
Often.
2.4 sulcular bleeding index (SBI): l, the most hemorrhage；2, visiting during gingival sulcus hemorrhage, outward appearance is normal；3, gingival sulcus is visited hemorrhage, gingiva
Congested；4, gingiva has other symptom such as ulcer or swelling.
2.5 gingival index (GI): 0, normal gingiva；L, mild inflammation；2, moderate inflammation；3, hyperphlogosis.
2.6 plaque indexs (PLI): 0, without bacterial plaque；L, bacterial plaque cover below facing l/3；2, bacterial plaque covers facing l/3～2/3；
3, bacterial plaque covers facing more than 2/3.
2.7 depth of pocket indexes (PDI): 0, gingival sulcus≤2mm；L, 2mm ＜ gingival sulcus≤3.5mm；2,3.5mm ＜ gingival sulcus≤5mm；
3,5mm ＜ gingival sulcus≤6.5mm；4,6.5mm ＜ gingival sulcus≤8mm.
3, Outcome measure:
3.1 periodontitis: set M=(SBI1+GI1+PLI1+PDIl-SBIl4+GI14+PLI14+PDIl4)/4 effective: M >=0.5；Effective:
0 ＜ M ＜ 0.5；Invalid: M≤0.
3.2 gingivitiss: set N=(SBI1+GI1+PLI1-SBI7+GI7+PLI7)/3 effective: N >=l；Effective: 0.5 ＜ N ＜ l；Invalid:
N≤0.5。
4, result
The harmony of 4.1 data: 2 groups of Genders and age, through inspection there are no significant difference (P ＞ 0.05), thus illustrate test group
It is equilibrium with the composition of matched group, there is comparability.
4.2 curative effects: experimental group and matched group observed result are as follows；Periodontitis is shown in Table 12, and gingivitis is shown in Table 13, and comprehensive therapeutic effect judges to see
Table 14.
Table 12 patients with periodontitis comprehensive therapeutic effect is evaluated
*P ＜ 0.01
Table 13 gingivitis patients comprehensive therapeutic effect is evaluated
*P ＜ 0.01
Table 14 periodontitis, gingivitis patients comprehensive therapeutic effect are evaluated
*P ＜ 0.01
Result above all illustrates that test group curative effect is better than matched group.Untoward reaction: all cases in test group and matched group are the most not
See untoward reaction locally and systemically.
The present invention is with lisozima as active component, and in addition suitably toothpaste made by adjuvant, it is achieved cleaning tooth, stop blooding, anti-
The effects such as bacterium.Lisozima in the lisozima toothpaste of the present invention, can play following effect: it is not only to tooth wear
Little, and have clean the teeth, tooth protection effect；Lisozima can dissolve the antibacterial in wound, stops the breeding of antibacterial, prevents
Wound infection, and impaired skin is had Healing；The action character of lisozima toothpaste is that local uses, and is used
Raw and auxiliary material safety non-toxic, uses safer.
Beneficial effects of the present invention is as follows:
1, the lisozima toothpaste that prepared by the present invention is in good taste, and selected adjuvant is less, and toothpaste is stable.
2, the abrasive difficult absorbability calcium carbonate selected by the present invention or calcium phosphate, by controlling its granularity, so that toothpaste
Sedimentation volume ratio meets toothpaste requirement.
3, lisozima toothpaste enables lisozima to penetrate in oral cavity tissue by oral cavity, and suppress dental plaque and/or
Prevent, control and treat the periodontal such as gingivitis and periodontitis.
4, the present invention adds glycine, glycine and lisozima complexation so that preparing lisozima toothpaste process
Middle lisozima titer plateaus under the high temperature conditions.
5, the present invention uses interfacial activity protective agent empgen BB, does not damage lisozima activity and keeps tooth simultaneously
Cream foaminess is good.
6, the present invention is by sodium alginate and the rational proportioning of carboxymethyl cellulose thickener so that it is the two has fabulous working in coordination with
Effect, substantially increases the suspension of toothpaste, thixotropy, rheological characteristic, has no effect the stability of toothpaste simultaneously, thus
There is in toothpaste higher using value.
Accompanying drawing explanation
Fig. 1 is experimental example 4 viscograph, and vertical coordinate is viscosity；Abscissa is carboxymethyl cellulose (CMC) and sodium alginate
Consumption；
Fig. 2 is experimental example 4 thixotropy parameter curve, and vertical coordinate is thixotropy parameter；Abscissa is carboxymethyl cellulose (CMC)
With sodium alginate consumption.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention will be further described, but it is not limited to this.
Supplementary material explanation in embodiment:
Device involved in embodiment and equipment are mastic preparation and produce common apparatus, and market is commercially available.It is described as follows:
Malvern Marlven laser diffraction granularity analyser (model 2000) Britain produces；East, cutter (model 50L) Wenzhou City
Top Machinery Manufacturing Co., Ltd. is on sale；Universal high-efficiency pulverizer (model 30B), stainless steel cauldron (model 50L) Shandong are new
Medical apparatus corporation, Ltd of China is on sale.
Below in conjunction with specific embodiment, the present invention will be further described.Should be understood that following example are merely to illustrate the present invention,
Not for limiting the scope of the present invention.
Embodiment 1: the preparation method of a kind of lisozima toothpaste
1, a kind of lisozima toothpaste, is made up by mass parts of following raw material:
2, preparation method is as follows:
(1) calcium carbonate is carried out micronizing, cross 400 mesh sieves, obtain mean diameter in 15～21 μm with grain size analysis with laser grain size analyzer；
(2) step (1) addition deionized water is configured to quality than calcium carbonate deionized water=1 5, carries out milling treatment of colloid,
Make suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 15～25% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～80 DEG C, rotating speed is again
60～80r/min, time 30～40 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～50r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～40 minutes, deposit in being delivered to sterilized tank, standby at 60～80 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 40 DEG C, is opened cutter low speed 1000～1200r/min and is sheared 8～10 minutes, then at a high speed 2500～
2800r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～90r/min, continues stirring 5～10
Minute, it is 30～40r/min to be slowly stirred at speed of agitator the most again, starts cooling, be cooled to when 30～35 DEG C stop stirring,
Then more than under 0.096MPa vacuum, it is 30～40r/min at speed of agitator, mixing time 30～40min, make mastic,
Pack and get final product.
Embodiment 2: the preparation method of a kind of lisozima toothpaste
1, a kind of lisozima toothpaste, is made up by mass parts of following raw material:
2, preparation method is as follows:
(1) calcium phosphate carrying out micronizing, cross 400 mesh sieves, obtaining mean diameter with grain size analysis with laser grain size analyzer is 5～12 μm；
(2) step (1) addition deionized water is configured to quality than calcium phosphate deionized water=1 7, carries out milling treatment of colloid,
Make suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 20～30% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～70 DEG C, rotating speed is again
60～75r/min, time 30～45 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～40r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～60 minutes, deposit in being delivered to sterilized tank, standby at 60～70 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 50 DEG C, is opened cutter low speed 1000～1500r/min and is sheared 8～10 minutes, then at a high speed 2500～
2600r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～70r/min, continues stirring 5～10
Minute, it is 30～50r/min to be slowly stirred at speed of agitator the most again, starts cooling, be cooled to when 30～35 DEG C stop stirring,
Then more than under 0.096MPa vacuum, it is 30～40r/min at speed of agitator, mixing time 30～40min, make mastic,
Pack and get final product.
Embodiment 3: the preparation method of a kind of lisozima toothpaste
1, a kind of lisozima toothpaste, is made up by mass parts of following raw material:
2, preparation method is as follows:
(1) calcium carbonate is carried out micronizing, cross 400 mesh sieves, obtain mean diameter in 15～21 μm with grain size analysis with laser grain size analyzer；
(2) step (1) addition deionized water is configured to quality than calcium carbonate deionized water=1 8, carries out milling treatment of colloid,
Make suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 10～20% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～70 DEG C, rotating speed is again
60～65r/min, time 30～35 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～45r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～40 minutes, deposit in being delivered to sterilized tank, standby at 60～70 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 60 DEG C, is opened cutter low speed 1000～1200r/min and is sheared 8～10 minutes, then at a high speed 2500～
2700r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～65r/min, continues stirring 5～8
Minute, it is 30～40r/min to be slowly stirred at speed of agitator the most again, starts cooling, be cooled to when 30～35 DEG C stop stirring,
Then more than under 0.096MPa vacuum, it is 30～40r/min at speed of agitator, mixing time 30～40min, make mastic,
Pack and get final product.
Embodiment 4: the preparation method of a kind of lisozima toothpaste
1, a kind of lisozima toothpaste, is made up by mass parts of following raw material:
2, preparation method is as follows:
(1) calcium phosphate is carried out micronizing, cross 400 mesh sieves, obtain mean diameter in 5～12 μm with grain size analysis with laser grain size analyzer；
(2) step (1) addition deionized water is configured to quality than calcium phosphate deionized water=1 7, carries out milling treatment of colloid,
Make suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 20～30% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～65 DEG C, rotating speed is again
60～65r/min, time 30～35 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～35r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～40 minutes, deposit in being delivered to sterilized tank, standby at 60～65 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 55 DEG C, is opened cutter low speed 1000～1200r/min and is sheared 8～9 minutes, then at a high speed 2500～
2700r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～65r/min, continues stirring 5～8
Minute, it is 30～35r/min to be slowly stirred at speed of agitator the most again, starts cooling, be cooled to when 30～35 DEG C stop stirring,
Then more than under 0.096MPa vacuum, it is 30～40r/min at speed of agitator, mixing time 30～40min, make mastic,
Pack and get final product.
Claims (9)
1. a lisozima toothpaste, it is characterised in that include that active component and adjuvant, described active component are hydrochloric acid
Lysozyme, its percentage by weight in toothpaste is 0.3～4.6%.
2. lisozima toothpaste as claimed in claim 1, it is characterised in that described adjuvant be prepare toothpaste needed for
Acceptable any adjuvant, according to known in the art, described adjuvant include wetting agent, thickening agent, foaming agent, protective agent,
Abrasive, correctives and/or other additives.
3. lisozima toothpaste as claimed in claim 2, it is characterised in that described wetting agent is glycerol and/or Pyrusussuriensis
Alcohol, thickening agent is carboxymethyl cellulose and/or sodium alginate, and foaming agent is sodium lauryl sulphate, protective agent be glycine and/
Or empgen BB, abrasive is calcium carbonate and/or calcium phosphate, and correctives is essence and/or saccharin sodium, other additives
Including silicon dioxide and deionized water.
4. the lisozima toothpaste as described in claim 1-3 is arbitrary, it is characterised in that by following raw material by mass parts system
Become:
5. lisozima toothpaste as claimed in claim 4, it is characterised in that be made up by mass parts of following raw material:
6. lisozima toothpaste as claimed in claim 5, it is characterised in that be made up by mass parts of following raw material:
Or,
Or,
7. the preparation method of the lisozima toothpaste as described in as arbitrary in claim 4～6, it is characterised in that include walking as follows
Rapid:
(1) abrasive calcium carbonate or calcium phosphate being carried out micronizing, calcium carbonate crosses 400 mesh sieves, obtain mean diameter be 15～
21μm；Calcium phosphate crosses 350～400 mesh sieves, and obtaining mean diameter is 5～19 μm；
(2) step (1) addition deionized water is configured to quality than calcium carbonate or calcium phosphate deionized water=1 5～10, enters
Row milling treatment of colloid, makes suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 10～30% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～80 DEG C, rotating speed is again
60～90r/min, time 30～50 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～50r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～60 minutes, deposit in being delivered to sterilized tank, standby at 60～80 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 40～60 DEG C, is opened cutter low speed 1000～1750r/min and is sheared 8～10 minutes, then at a high speed 2500～
3000r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～90r/min, continues stirring 5～10
Minute, it is 30～50r/min stirrings at speed of agitator the most again, starts cooling, stop stirring when being cooled to 30～35 DEG C, so
After more than under 0.096MPa vacuum, be 30～50r/min at speed of agitator, mixing time 30～50min, make mastic,
Pack and get final product.
8. the preparation method of lisozima toothpaste as claimed in claim 7, it is characterised in that the glue described in step (3)
Liquid solution, uses NDJ-1 type Rotary Viscosimeter according to " Chinese Pharmacopoeia two annex VIG the second methods of version in 2010 ", with 4
Number rotor, rotating speed is 6 turns per minute, and the viscosity of material dynamic viscosity of material when 25 DEG C is 20～30Pa.s.
9. the preparation method of lisozima toothpaste as claimed in claim 7, it is characterised in that comprise the steps:
(1) abrasive calcium carbonate or calcium phosphate being carried out micronizing, calcium carbonate crosses 400 mesh sieves, obtains with grain size analysis with laser grain size analyzer
Mean diameter is in 15～21 μm；Calcium phosphate crosses 400 mesh sieves, obtains mean diameter in 5～12 μm with grain size analysis with laser grain size analyzer；
(2) step (1) addition deionized water is configured to quality than calcium carbonate or calcium phosphate deionized water=1 5～8, enters
Row milling treatment of colloid, makes suspension solution, standby；
(3) weigh each raw material by formula ratio, glycerol, sorbitol deionized water are configured to mass concentration be 20～30% molten
Liquid is standby；Carboxymethyl cellulose, sodium alginate, saccharin sodium, essence being added, under the conditions of 60～80 DEG C, rotating speed is again
60～80r/min, time 30～40 minutes, make colloid solution, standby；
(4) step (2) suspension solution is mixed with step (3) colloid solution, add sodium lauryl sulphate, 12
Alkyl betaine, silicon dioxide, the most again rotating speed be 30～50r/min stirring；After making it fully mix, at 121～125 DEG C
Under the conditions of sterilizing 30～40 minutes, deposit in being delivered to sterilized tank, standby at 60～80 DEG C；
(5) in dissolving tank, lisozima, glycine are added deionized water dissolving, then step (4) are added,
Temperature, under the conditions of 40 DEG C, is opened cutter low speed 1000～1200r/min and is sheared 8～10 minutes, then at a high speed 2500～
2800r/min shears 4～5 minutes；Closing cutter, open stirring, rotating speed is 60～90r/min, continues stirring 5～10
Minute, it is 30～40r/min stirrings at speed of agitator the most again, starts cooling, stop stirring when being cooled to 30～35 DEG C, so
After more than under 0.096MPa vacuum, be 30～40r/min at speed of agitator, mixing time 30～40min, make mastic,
Pack and get final product.
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| CN106943311A (en) * | 2017-04-07 | 2017-07-14 | 缪来耿 | It is a kind of to be used to prevent and/or treat toothpaste of periodontitis and preparation method thereof |
| CN107463529A (en) * | 2017-06-26 | 2017-12-12 | 广州薇美姿实业有限公司 | A kind of toothpaste cleaning force appraisal procedure |
| CN108888770A (en) * | 2018-07-30 | 2018-11-27 | 郑州兰茜生物工程有限公司 | A kind of oral health agent of strengthening tooth antibacterial anti-inflammatory and preparation method thereof |
| CN109908025A (en) * | 2019-04-15 | 2019-06-21 | 广州康云生物科技有限公司 | Application of the glycine betaine in protection lysozyme activity |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106943311A (en) * | 2017-04-07 | 2017-07-14 | 缪来耿 | It is a kind of to be used to prevent and/or treat toothpaste of periodontitis and preparation method thereof |
| CN107463529A (en) * | 2017-06-26 | 2017-12-12 | 广州薇美姿实业有限公司 | A kind of toothpaste cleaning force appraisal procedure |
| CN108888770A (en) * | 2018-07-30 | 2018-11-27 | 郑州兰茜生物工程有限公司 | A kind of oral health agent of strengthening tooth antibacterial anti-inflammatory and preparation method thereof |
| CN109908025A (en) * | 2019-04-15 | 2019-06-21 | 广州康云生物科技有限公司 | Application of the glycine betaine in protection lysozyme activity |
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