CN106912485A - Compound double-chain quaternary ammonium salt thimerosal and its application method and application - Google Patents

Compound double-chain quaternary ammonium salt thimerosal and its application method and application Download PDF

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CN106912485A
CN106912485A CN201710157577.7A CN201710157577A CN106912485A CN 106912485 A CN106912485 A CN 106912485A CN 201710157577 A CN201710157577 A CN 201710157577A CN 106912485 A CN106912485 A CN 106912485A
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ammonium salt
quaternary ammonium
double
chain quaternary
thimerosal
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孙建生
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Hangzhou Yi Lu Medical Devices Co Ltd
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Hangzhou Yi Lu Medical Devices Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/04Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aldehyde or keto groups, or thio analogues thereof, directly attached to an aromatic ring system, e.g. acetophenone; Derivatives thereof, e.g. acetals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A01N25/06Aerosols
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N33/00Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/02Amines; Quaternary ammonium compounds
    • A01N33/12Quaternary ammonium compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/16Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
    • A61L2/22Phase substances, e.g. smokes, aerosols or sprayed or atomised substances

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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Agronomy & Crop Science (AREA)
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  • Wood Science & Technology (AREA)
  • Dentistry (AREA)
  • Engineering & Computer Science (AREA)
  • Plant Pathology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Veterinary Medicine (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Epidemiology (AREA)
  • Toxicology (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)

Abstract

The present invention provides a kind of compound double-chain quaternary ammonium salt thimerosal includes double-chain quaternary ammonium salt, single-stranded quaternary ammonium salt and OPA, double-chain quaternary ammonium salt is double octyl alkyl dimethyl ammonium chlorides or double-track suspended self-propelled conveyor, and single-stranded quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride.It is preferred that double-chain quaternary ammonium salt is 0.04~0.06% weight, single-stranded quaternary ammonium salt is 0.20~0.30% weight, and OPA is 0.4~0.7% weight.Compound double-chain quaternary ammonium salt thimerosal is also including one or more in nonionic surfactant, inorganic anti-interference agent and synergist.Additionally provide application method and its application of compound double-chain quaternary ammonium salt thimerosal.Compound double-chain quaternary ammonium salt thimerosal of the invention is sterilized quick, and Disinfection Effect is good, safe and healthy to have no toxic side effect, and has good stability, and to dental impression silica substantially without metamorphosis, it is ensured that dental impression silica dimensional stability, it is suitable to large-scale promotion application.

Description

Compound double-chain quaternary ammonium salt thimerosal and its application method and application
Technical field
The present invention relates to thimerosal technical field, more particularly to quaternary ammonium salt thimerosal technical field is specifically referred to a kind of multiple Close double-chain quaternary ammonium salt thimerosal and its application method and application.
Background technology
Oral cavity is the ecosystem of bacterium more than, saliva, blood of the die due to directly contact patient, its disease for carrying Poison, microorganism can cause cross-infection during modelling.But due to moulage such as alginates absorbed water in water it is swollen It is swollen, the characteristics of spilling water shrinks in air so that die after water vapour, medicining liquid dipping, disinfection by ultraviolet light using easily deforming.Cause This major issue for being faced as oral cavity medical personnel for the sterilization of die in recent years.
Quaternary ammonium salt disinfectant is a cationoid surfactant, and its general structure is:
Wherein R1~R4Organic radical is represented, they are combined into a cation group with nitrogen-atoms, are sterilized live part, because Nitrogen-atoms is combined with 4 organic radicals, therefore claims " quaternary ammonium salt ", and X is anion, such as halogen, sulfate radical or other it is similar it is cloudy from Son.Quaternary ammonium salt as disinfectant, in R1~R4In the general alkyl for having a carbon bond distance up to 8~18, it is short or be longer than carbochain person and kill Bacterium power is poor.Single-stranded quaternary ammonium salt (such as 1227 i.e. dodecyl benzyl dimethyl ammonium chloride is representative) can only kill some bacterial reproductions Body and lipophilic virus, belong to poorly efficient bactericide, and double-chain quaternary ammonium salt (such as D-C8~C10 alkyl dimethyl ammonium chlorides are representative) can be killed Multiple-microorganism, including bacterial propagule, some fungies and virus.
But for single double-chain quaternary ammonium salt, the species of its microorganism that can be killed or not comprehensive enough, sterilization effect Really or not ideal enough, it is therefore desirable to provide a kind of compound double-chain quaternary ammonium salt thimerosal, it is sterilized quick, and Disinfection Effect is good, defends Raw safe without toxic side effect, has good stability, and to dental impression silica substantially without metamorphosis, it is ensured that dental impression silica dimensionally stable Property.
The content of the invention
In order to overcome above-mentioned shortcoming of the prior art, it is an object of the present invention to provide a kind of compound double-strand quaternary ammonium Salt thimerosal, it is sterilized quick, and Disinfection Effect is good, is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of compound double-chain quaternary ammonium salt thimerosal, its safe and healthy nontoxic secondary work With, have good stability, it is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of compound double-chain quaternary ammonium salt thimerosal, its to dental impression silica substantially without Metamorphosis, it is ensured that dental impression material dimensional stability, is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of preparation method of compound double-chain quaternary ammonium salt thimerosal, it prepares letter Single, easy to operate, the compound double-chain quaternary ammonium salt thimerosal being made is sterilized quick, and Disinfection Effect is good, is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of preparation method of compound double-chain quaternary ammonium salt thimerosal, it prepares letter Single, easy to operate, the compound double-chain quaternary ammonium salt thimerosal that is made is safe and healthy to have no toxic side effect, and has good stability, and is suitable to extensive Popularization and application.
It is another object of the present invention to provide a kind of preparation method of compound double-chain quaternary ammonium salt thimerosal, it prepares letter Single, easy to operate, the compound double-chain quaternary ammonium salt thimerosal being made is to dental impression silica substantially without metamorphosis, it is ensured that dental impression material Dimensional stability, is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of compound double-chain quaternary ammonium salt thimerosal in dental impression silica sterilization Using such that it is able to quick effectively sterilization is carried out to dental impression silica, is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of compound double-chain quaternary ammonium salt thimerosal in dental impression silica sterilization Using, it is safe and healthy to have no toxic side effect so as to be sterilized to dental impression silica, have good stability, it is suitable to large-scale promotion application.
It is another object of the present invention to provide a kind of compound double-chain quaternary ammonium salt thimerosal in dental impression silica sterilization Using so as to dental impression silica sterilization, to dental impression silica substantially without metamorphosis, it is ensured that dental impression silica dimensional stability, be suitable to Large-scale promotion application.
To achieve the above objectives, in the first aspect of the present invention, there is provided a kind of compound double-chain quaternary ammonium salt thimerosal, its feature It is that the compound double-chain quaternary ammonium salt thimerosal includes double-chain quaternary ammonium salt, single-stranded quaternary ammonium salt and OPA, the double-strand quaternary ammonium Salt is double octyl alkyl dimethyl ammonium chlorides or double-track suspended self-propelled conveyor, and the single-stranded quaternary ammonium salt is dodecyl dimethyl benzyl Ammonium chloride.
The weight percentage of the double-chain quaternary ammonium salt, the single-stranded quaternary ammonium salt and the OPA can be according to need It was determined that it is preferred that the weight percentage of the double-chain quaternary ammonium salt is 0.04%~0.06%, the weight of the single-stranded quaternary ammonium salt Amount percentage composition is 0.20%~0.30%, and the weight percentage of the OPA is 0.4%~0.7%.
In order to realize more preferable Disinfection Effect, it is preferred that the compound double-chain quaternary ammonium salt thimerosal also includes nonionic table One or more in face activating agent, inorganic anti-interference agent and synergist.
Wherein nonionic surfactant is mainly used in changing thimerosal surface tension, makes thimerosal and microbial cell film It is more easy to contact;Inorganic anti-interference agent is mainly used in stablizing the acid-base value of thimerosal, improves the stability of thimerosal;Synergist is main For dissolving the liposoluble substance on microbial cell film, accelerate membranolysis, improve Disinfection Effect.
The nonionic surfactant, the inorganic anti-interference agent and the synergist can be any suitable examinations Agent, more preferably, the nonionic surfactant is AEO -9 or AEO -10, described Inorganic anti-interference agent is EDETATE SODIUM, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, citric acid or sodium citrate, and the synergist is the last of the ten Heavenly stems Base glucosides, nonyl phenol polyethers -10 or nonyl phenol polyethers -14.
The weight percentage of the nonionic surfactant, the inorganic anti-interference agent and the synergist can be with root According to it needs to be determined that, more preferably, the weight percentage of the nonionic surfactant is 1%~5%, described inorganic anti-interference The weight percentage of agent is 0.01%~0.5%, and the weight percentage of the synergist is 1%~5%.
In the second aspect of the present invention, there is provided a kind of application method of above-mentioned compound double-chain quaternary ammonium salt thimerosal, it is special Point is that the compound double-chain quaternary ammonium salt thimerosal is treated into sterilizing objects carries out spraying treatment, then by the article to be sterilized It is placed in gnotobasis for a period of time, then the described compound double-chain quaternary ammonium salt thimerosal on the article to be sterilized is eluted.
The spraying treatment can realize atomization using any suitable method, and the process time of the spraying treatment can be with Determine as needed, it is preferred that the spraying treatment realizes atomization using nozzle, the process time of the spraying treatment is 30 seconds ~60 seconds.
Described a period of time can determine as needed, it is preferred that described a period of time is 5 minutes~10 minutes.
In the third aspect of the present invention, there is provided a kind of above-mentioned compound double-chain quaternary ammonium salt thimerosal is in article spraying disinfection Application.
The article is above-mentioned article to be sterilized, can be any suitable article, it is preferred that the article is dentistry Model.
Beneficial effects of the present invention are essentially consisted in:
1st, compound double-chain quaternary ammonium salt thimerosal of the invention includes double-chain quaternary ammonium salt, single-stranded quaternary ammonium salt and OPA, Double-chain quaternary ammonium salt is double octyl alkyl dimethyl ammonium chlorides or double-track suspended self-propelled conveyor, and single-stranded quaternary ammonium salt is dimethyl Base benzyl ammonium chloride, sterilized quick, Disinfection Effect is good, is suitable to large-scale promotion application.
2nd, compound double-chain quaternary ammonium salt thimerosal of the invention includes double-chain quaternary ammonium salt, single-stranded quaternary ammonium salt and OPA, Double-chain quaternary ammonium salt is double octyl alkyl dimethyl ammonium chlorides or double-track suspended self-propelled conveyor, and single-stranded quaternary ammonium salt is dimethyl Base benzyl ammonium chloride, it is safe and healthy to have no toxic side effect, have good stability, it is suitable to large-scale promotion application.
3rd, compound double-chain quaternary ammonium salt thimerosal of the invention includes double-chain quaternary ammonium salt, single-stranded quaternary ammonium salt and OPA, Double-chain quaternary ammonium salt is double octyl alkyl dimethyl ammonium chlorides or double-track suspended self-propelled conveyor, and single-stranded quaternary ammonium salt is dimethyl Base benzyl ammonium chloride, to dental impression silica substantially without metamorphosis, it is ensured that dental impression material dimensional stability, is suitable to push away on a large scale Wide application.
These and other objects of the invention, feature and advantage, are filled by following detailed descriptions and claim Split shows, and can be achieved by means, device and the combinations thereof specially pointed out in appended claims.
Specific embodiment
In order to be more clearly understood that technology contents of the invention, described in detail especially exemplified by following examples.Except non-specifically Illustrate, percentage here is weight percentage.Wherein
20kg/ barrels of double octyl alkyl dimethyl ammonium chloride Xiamen City Xianduan Science and Technology Co., Ltd
20kg/ barrels of double-track suspended self-propelled conveyor Xiamen City Xianduan Science and Technology Co., Ltd
Chemical Co., Ltd. 20kg/ barrels of dodecyl benzyl dimethyl ammonium chloride Shanghai Jinshan longitude and latitude
200kg/ barrels of Jiangsu Hai'an Petrochemical Plant of AEO -9
200kg/ barrels of Jiangsu Hai'an Petrochemical Plant of AEO -10
Co., Ltd 250g/ bottles of development in science and technology is recovered in EDETATE SODIUM Tianjin
500g/ bottles of potassium dihydrogen phosphate Chemical Reagent Co., Ltd., Sinopharm Group
500g/ bottles of sodium citrate Chemical Reagent Co., Ltd., Sinopharm Group
Co., Ltd 200kg/ barrels of Decyl Polyglucoside Jining Hong Ming chemical reagent
200kg/ barrels of the Jiangsu Province of nonyl phenol polyethers -10 Hai'an oil company
500g/ bottles of the Shanghai of nonyl phenol polyethers -14 Heng Yuan bio tech ltd
Industrial Co., Ltd. 25kg/ barrels of OPA Shanghai Ao highland barleys
Embodiment 1 is combined the preparation of double-chain quaternary ammonium salt thimerosal 1
By the double octyl alkyl dimethyl ammonium chlorides of 0.05g, 0.3g dodecyl benzyl dimethyl ammonium chlorides and 0.4g neighbour's benzene two Formaldehyde is placed in stirring and dissolving in 99.25g water, is made compound double-chain quaternary ammonium salt thimerosal 1.
Embodiment 2 is combined the preparation of double-chain quaternary ammonium salt thimerosal 2
By the double octyl alkyl dimethyl ammonium chlorides of 0.04g, 0.2g dodecyl benzyl dimethyl ammonium chlorides, 0.6g O-phthalics Aldehyde, 5g AEOs -9,0.5g EDETATE SODIUMs and 1g Decyl Polyglucosides are placed in stirring and dissolving in 92.66g water, are made Compound double-chain quaternary ammonium salt thimerosal 2.
Embodiment 3 is combined the preparation of double-chain quaternary ammonium salt thimerosal 3
By 0.05g double-track suspended self-propelled conveyors, 0.3g dodecyl benzyl dimethyl ammonium chlorides, 0.7g O-phthalics Aldehyde, 3g AEOs -10,0.28g dipotassium hydrogen phosphates, 0.02g potassium dihydrogen phosphates and 3g nonyl phenol polyethers -10 are placed in Stirring and dissolving in 92.65g water, is made compound double-chain quaternary ammonium salt thimerosal 3.
Embodiment 4 is combined the preparation of double-chain quaternary ammonium salt thimerosal 4
By the double octyl alkyl dimethyl ammonium chlorides of 0.06g, 0.2g dodecyl benzyl dimethyl ammonium chlorides, 0.59g neighbour's benzene two Formaldehyde, 1g AEOs -9,0.01g sodium citrates and 5g nonyl phenol polyethers -14 are placed in 93.14g water and stir molten Solution, is made compound double-chain quaternary ammonium salt thimerosal 4.
The BA of embodiment 4
(the finer atomization nozzle of BA one:Danvers, 030F0616)
To the quantitative disinfecting test of bacterial propagule
1st, equipment and material
(1) impression disinfection machine:Easy guideboard ESS-1 type dental models sterilizing machine (Hangzhou Yi Lu Medical Devices Co., Ltd.s).
(2) alternatively match somebody with somebody and apply mechanically thimerosal:
2% glutaral disinfectant solution (is purchased from Hangzhou LIONSER Medical Disinfectant Co., Ltd.)
1% compound quaternary ammonium salt disinfectant, 2% compound quaternary ammonium salt disinfectant (are purchased from the bright limited public affairs of rope medical disinfectant in Hangzhou Department)
1%~5% Hydrogen Peroxide Disinfection Solution (1%, 2%, 3%, 4%, 5%) (is carried by Shanghai Hubble Co., Ltd respectively The high-strength hydrogen peroxide dilution of confession is formed)
The clean good surface sterilization liquid of power (quaternary ammonium salt of 75% ethanol+0.2%, purchased from Hangzhou LIONSER Medical Disinfectant Co., Ltd.)
Compound double-chain quaternary ammonium salt thimerosal 1-4 prepared by embodiment 1-4.
2nd, test strain.Staphylococcus aureus (ATCC6538), Escherichia coli (8099), pseudomonas aeruginosa (ATCC15442), Candida albicans (ATCC10231), common micro-organisms center is comprehended by Chinese microorganism strain preservation pipe There is provided.
3rd, nertralizer:In D/E and meat soup, the purchase of B/D companies.
4th, microbiological contamination carrier:Sterile absorbent pieces of cloth:Made of white gambroon.Before cutting off, first the cloth of degreasing is pressed The size (10mm*10mm) that carrier specifies, pump edge one week each one through weft yarn, then cut off by drawn work trace.This method is made Carrier it is in the same size, and without flash.
5th, bacterium piece:To insert drying in clean work station standby for carrier after microbiological contamination.
6th, fully loaded die:Large size elastic silicone rubber die (Zhejiang Province's stomatological hospital), alginates material die (Zhejiang Province Stomatological hospital), rubber cup (Zhejiang Province's stomatological hospital), toolsetting (Zhejiang Province's stomatological hospital), dental models gypsum (Zhejiang Province oral cavity Hospital).8 every time, uniformly laid on luggage carrier in sterilizing machine.
2nd, method
1st, test basis::Nertralizer qualification test, quantitative disinfecting test respectively refer to the Ministry of Public Health《Disinfection technology standard》 2.1.5.6,2.1.1.7.6 bars are carried out.
2nd, bacterium piece lays:Bacterium piece is placed in sterilizing machine, in, stamp surfaces outward everywhere.
3rd, nertralizer qualification test:Thimerosal acts on a cycle (6 points 45 seconds, sprinkling stands 6 minutes after 45 seconds), test organisms Strain is Escherichia coli, Candida albicans, and experiment is repeated 3 times, and 3 experiments show that the nertralizer is applied to the thimerosal and white is read The killing experiment of pearl bacterium.
4th, BA:After thimerosal acts on a cycle (6 points 45 seconds, sprinkling stands 6 minutes after 45 seconds), with aseptic formality Carrier is taken out, is put into nertralizer, after being eluted through concussion, recovery counting is carried out to residual bacterium, while to place identical at room temperature The bacterium piece of time does positive control and reclaims counting.Experiment is repeated 3 times.
5th, 23 DEG C~25 DEG C of environment temperature, relative humidity 35%~45%.
3rd, result
Table 1
Table 2
Simulated field Disinfection Effect
First, equipment
1st, test strain:Candida albicans ATCC10231
2nd, nertralizer:In D/E and meat soup
3rd, sterilizing machine:Easy guideboard ESS-1 type dental models sterilizing machines
4th, alternatively match somebody with somebody and apply mechanically thimerosal:With thimerosal used in above-mentioned " to the quantitative disinfecting test of bacterial propagule ".
5th, microbiological contamination carrier:Sterile absorbent pieces of cloth
6th, fully loaded die:Large size boxing impression (Zhejiang Province's stomatological hospital), silicon rubber material (Zhejiang Province's stomatological hospital), Alginate impression (Zhejiang Province's stomatological hospital), common artificial tooth (Zhejiang Province's stomatological hospital).8 garment dye bacterium dies are placed every time.
7th, bacterial carrier:It is standby that bacterial carrier inserts drying in clean work station.
2nd, method
1st, the Ministry of Public Health《Disinfection technology standard》(version in 2002) 2.1.2.2 bars.
2nd, BA:Bacterial carrier is inserted in sterilizing machine, thimerosal work a cycle (6 points 45 seconds, it is quiet after sprinkling 45 seconds Put 6 minutes) after, carrier is taken out with aseptic formality, it is put into nertralizer, after being eluted through concussion, recovery counting is carried out to residual bacterium, Make positive control recovery counting to place the bacterial carrier of same time at room temperature simultaneously.
3rd, 23 DEG C~25 DEG C of environment temperature, relative humidity 35%~45%.
3rd, result
Through 30 dies (large size boxing impression 6, common artificial tooth 6, silicone rubber impression 9, alginate impression 9) weight Retrial is tested and shown, the different sterilized machines of thimerosal act on a cycle to contaminating the Candida albicans killing logarithm value knot in stamp surfaces Fruit see the table below:
Table 3
BA two (ultrasonic atomization)
Simulated field Disinfection Effect
Carried out by the method for the simulated field Disinfection Effect of above sterilization experiment one, but thimerosal uses ultrasonic fog Change, be combined double-chain quaternary ammonium salt thimerosal 1-4 ultrasonic atomizations 2 minutes, repeating experiment through 30 dies shows, acts on a cycle pair The Candida albicans contaminated in stamp surfaces kills logarithm value < 3.00.
Table 4
The poliovirus inactivation test of embodiment 5
First, equipment
1. experiment strain:Polio I type vaccines strain virus (are derived from CDC spinal cord ash Zhi Yan National Key Laboratories).
2. host cell:RD passage cells (are derived from virus examination section of Zhejiang Center For Disease Control and Prevention gray nucleus Scorching laboratory).
3. cell culture medium:Containing it is 1% dual anti-(penicillin and streptomycin mixed liquor 10,000U/mL, be derived from the silent winged generation of U.S.'s match you Scientific & technical corporation), 1%LG (Glu is derived from U.S. Sigma-Aldrich biology Co., Ltd), 10% cow's serum (be derived from U.S.'s Sigma-Aldrich biology has the MEM liquid of (being derived from Sigma-Aldrich biology Co., Ltd of the U.S.) Limit company).
4. disinfectant:Compound double-chain quaternary ammonium salt thimerosal 1 prepared by embodiment 1.
5. organic interfering substance:MEM liquid containing 3% cow's serum.
6. virus titer is determined:Micro plate Endpoint Dilution Method measures polio I type vaccine strains virus titer for Log (TCID50)=6.55.
7. material:Tissue Culture Flask, 96 orifice plates, dilution (MEM liquid) etc..
8. fully loaded die:8 sample large size Elastomeric oral dies are placed during test in sterilizing machine every time (to cure in Zhejiang Province oral cavity Institute), silicon rubber material.
2nd, method
1. sterilizing machine is fully loaded with:2 are respectively put in plate to be infected with Polio virus suspension (concentration is 106VLPs/ml carrier) (with the sterile absorbent pieces of cloth of embodiment 4), (Hangzhou Yi Lu medicine equipments have to be put into easy guideboard ESS-1 type dental models sterilizing machine Limit company) innner and outer fully loaded buccal impression surface everywhere.
2. thimerosal configuration
Tested using the thimerosal of fresh absorption in experiment every time, supporting easy guideboard ESS-1 type dental models disappear Malicious machine is used, and is used with thimerosal as experiment.
3. poliovirus cell toxicity test
3.1 using compound double-chain quaternary ammonium salt thimerosal 1 as " experiment concentration ", and 2 times are serially diluted to 64 times.
The thimerosal of each dilution factor is added in 3.2 96 porocyte plates, per the μ l of hole 100, each dilution factor is inoculated with 4 holes, then adds Cell suspension, per the μ l of hole 100;Cell control well is 100 μ l MEM liquid, then adds 100 μ l cell suspensions, and be arranged in parallel 4 holes, places 36.5 DEG C, containing 5%CO2Incubator culture 7 days, observe and record the growing state of cell daily.
3.3 results:Thimerosal to cell thing toxicity diluted concentration for " experiment concentration " 1:4 times, therefore contrived experiment is used Except medicine dilution factor is 1:4.
4. dilution removes prescription method qualification test (poliovirus)
Result see the table below:
The experiment of table 5 is diluted with thimerosal and removes medicine qualification result
5. polio I types inactivation of virus quantifies suspension test
Die carries out plaque assay experiment after virus inoculation inside and outside the sterilizing machine rack and determines inactivating efficacy respectively.
Tested through three repetitions, the thimerosal is in sterilizing machine full load in the work period for disinfecting time (is wherein sprayed for 9 minutes Spill the time 5 minutes, disinfection time 4 minutes), average inactivation logarithm value is >=4.00, can complete inactivation polio disease Poison, experimental result see the table below:
The thimerosal of table 6 is to poliovirus inactivating efficacy
Note:21 DEG C of environment temperature, relative humidity 51%.
Positive controls average virus infection titer TCID50Logarithm value=6.50 (scope /), negative control group culture medium without Pollution, cell growth is good.
6. conclusion
Compound double-chain quaternary ammonium salt thimerosal 1 under the conditions of 21 DEG C of temperature, humidity 51%RH with polio I type vaccine strains Viral mixed liquor acts on disinfecting time 9 minutes (wherein spraying time 5 minutes, disinfection time 4 minutes), and experiment is in triplicate The equal > 4.00 of averaging of income inactivation of virus logarithm value, can complete inactivation poliovirus.
For compound double-chain quaternary ammonium salt thimerosal 2, compound double-chain quaternary ammonium salt thimerosal 3 and compound double-chain quaternary ammonium salt thimerosal 4, with the experimental result similar with compound double-chain quaternary ammonium salt thimerosal 1.
The physicochemical property of embodiment 6 is detected
PH value:
First, equipment
1st, test specimen:Compound double-chain quaternary ammonium salt thimerosal 1-4 prepared by embodiment 1-4, quaternary ammonium salt content (press by molecular weight 354 meters), respectively 0.348%, 0.235%, 0.348%, 0.256%.
2nd, correction standard buffer solution:PBS 0.025mol/L pH6.86
Potassium Hydrogen Phthalate 0.05mol/L pH4.00
Borax 0.01mol/L pH9.18
3rd, acidometer METTLER PE20 types.
2nd, method
1st, test basis:The Ministry of Public Health《Disinfection technology standard》(version in 2002) 2.2.1.4 bars.
2nd, test condition:25 DEG C of experimental situation temperature, relative humidity 45%.
3rd, result
Result shows that the pH of four kinds of thimerosals is respectively 7.80,7.89,7.85,7.65 after tested.
Quaternary ammonium salt content:
First, equipment
1st, test specimen:Compound double-chain quaternary ammonium salt thimerosal 1-4 prepared by embodiment 1-4, active ingredient is quaternary ammonium salt.
2nd, instrument and equipment:Electronic analytical balance METTER AB204N.
3rd, standard liquid:Tetraphenylboron sodium 0.01968mol/L.
2nd, method
1st, foundation is detected:The Ministry of Public Health《Disinfection technology standard》(version in 2002) 2.2.1.2.13 bars, Q/HLS055《Hang Zhoulang The easy guideboard ESS-1 types dental models sterilizing machine Special sterilizing liquid of rope medical disinfectant Co., Ltd company standard》4.2.2 bar:Season Ammonium salt total content is determined:Determined by disinfection technology standard pertinent regulations, the mean molecule quantity of compound quaternary ammonium salt is 354, in product When effective content is calculated, molecular weight is used as design factor according to this.
3rd, result
Four kinds of sample quaternary ammoniums salt content (molecular weight is based on 354) are respectively 0.348%, 0.235%, 0.348%, 0.256%.
Stability:
First, equipment
1st, test specimen:Compound double-chain quaternary ammonium salt thimerosal 1-4 prepared by embodiment 1-4, quaternary ammonium salt content (press by molecular weight 354 meters), respectively 0.348%, 0.235%, 0.348%, 0.256%.
2nd, instrument and equipment:Electronic analytical balance METTER AB204N.
3rd, standard liquid:Tetraphenylboron sodium 0.01612mol/L.
2nd, method
1st, foundation is checked:Detection foundation:The Ministry of Public Health《Disinfection technology standard》(version in 2002) 2.2.1.2.13 bars, Q/ HLS055《The easy guideboard ESS-1 types dental models sterilizing machine Special sterilizing of Hangzhou LIONSER Medical Disinfectant Co., Ltd.'s company standard Liquid》4.2.2 bar:Quaternary ammonium salt total content is determined:Determined by disinfection technology standard pertinent regulations, the mean molecule quantity of compound quaternary ammonium salt It is 354, when product effective content is calculated, molecular weight is used as design factor according to this.
2nd, preservation condition:Materials to be placed in plastic bottle and be placed in 37 DEG C of incubators and preserve 90 days.
3rd, testing conditions:22 DEG C -24 DEG C of experimental situation temperature, relative humidity 45%-60%.
3rd, result
After compound double-chain quaternary ammonium salt thimerosal 1 is deposited through 37 DEG C, quaternary ammonium salt content is 0.316%, rate of descent < 10%.Deposit Before and after putting, sample external packing and outward appearance no significant difference, the term of validity can be set to 24 months.
For compound double-chain quaternary ammonium salt thimerosal 2, compound double-chain quaternary ammonium salt thimerosal 3 and compound double-chain quaternary ammonium salt thimerosal 4, with the experimental result similar with compound double-chain quaternary ammonium salt thimerosal 1.
Toxicity test
According to the Ministry of Public Health《Disinfection technology standard》Version in 2002, toxicity has been carried out to compound double-chain quaternary ammonium salt thimerosal 1-4 Experiment is learned, result of the test shows:
For compound double-chain quaternary ammonium salt thimerosal 1:
1st, acute oral toxicity test (mouse):The other chmice acute LD50 of passing through mouth of bisexuality is all higher than 5.0g/kg body weight, True border is nontoxic.
2nd, an intact skin irritant test (rabbit):It is subexcite.
3rd, mice bone marrow micronucleus:Acted on without micronucleus is caused.
The tested material chmice acute Oral toxicity experimental result of table 7
Conclusion:The other chmice acute LD50 of passing through mouth of bisexuality is all higher than 5.0g/kg body weight, according to acute toxicity grading criteria True border is nontoxic.
Table 8 once contacts IR after rabbit intact skin
Conclusion:Compound double-chain quaternary ammonium salt thimerosal 1 once contacts irritant test highest skin irritatin after rabbit intact skin Index is 1.7, belongs to subexcite.
The tested material mice bone marrow micronucleus result of table 9
U-test:Compare #P < 0.001 with negative control group
Conclusion:To bone marrow cells in mice polychromatic erythrocyte without cause micronucleus effect.
For compound double-chain quaternary ammonium salt thimerosal 2, compound double-chain quaternary ammonium salt thimerosal 3 and compound double-chain quaternary ammonium salt thimerosal 4, with the experimental result similar with compound double-chain quaternary ammonium salt thimerosal 1.
The impression accuracy of embodiment 7 is detected
1st, experiment material
Alginate impression material (Heraeus) (emerald tooth family alginate impression material, common coagulating type, Deng Shibai dentistry (Tianjin) Co., Ltd), super hard gypsum (Heraeus) (super hard gypsum, 1.5kg/ bags, Heraeus-Kulzer Corporation), River wood powder liquid proportioning machine (producer:Amanngirrbach (Oman gill Bach), smartbox X2 gypsum proportioning machine), river wood is true Empty mixer (producer:Amanngirrbach (Oman gill Bach), specifications and models:Smartmix X2 de-airing mixers), Silfraden oscillators (plaster vibrator, VIB24, match method Dent), enter the upper and lower gnathode of standard of resin material making day (model 500A) (STUDY MODEL, NISSIN DENTAL PROPUCTS INC), rubber cup, toolsetting, pallet, easy guideboard ESS-1 type dental models sterilizing machines, compound double-chain quaternary ammonium salt thimerosal 1 prepared by embodiment 1.
2nd, model taking method
Moulage is modulated by the water:powder ratio requirement of manufacturer's operation instruction, 21g is compared according to water, powder:The ratio of 57ml Example materials, mixer mediation 1min, deviate from die after modulus 3min, upper and lower jaw produces 24 dies respectively.By 48 dies point Into sterilization group and control group, every group of 12, the upper jaw, 12 dies of lower jaw irrigate plaster cast after sterilization group impression disinfection, control Group is non-sterile to irrigate plaster cast, 2 groups of demouldings after perfusion gypsum 30min immediately.2 dies are taken every time, sterilized, are not disappeared Poison circulation is carried out.
3rd, sterilization method
Easy guideboard ESS-1 types dental models sterilizing machine is immediately placed in after impression making, the compound double-chain quaternary ammonium salt through being atomized Thimerosal 1 acts on a cycle (total time is 45 seconds 6 minutes, wherein sprinkling 45 seconds, sterilization 6 minutes), takes out backlash developing and printing mould table Face residual disinfectancy liquid, irrigates plaster cast.
4th, die modification detection
Using the three-dimensional laser of 3shape A/S companies of Denmark production (model D700) respectively by master pattern, experimental group stone Cream model and control group plaster cast are scanned, plaster cast is alignd with sextuple Dental implantion design software first (experimental group and Control group each plaster cast is fitted with master pattern respectively), data processing then is carried out with Geomagic Studio, The variance analysis of surface deviation 0.05mm, 0.1mm and 0.2mm is taken respectively, is calculated fitting area and the gross area, digital simulation Rate.
5th, statistical method
Using the software analysis of spss 17.0, data use independent samples t test.
6th, result
Experimental group is fitted with control group with master pattern, there is deviation, and fitting area is directly proportional to surface deviation value, and 2 When upper and lower gnathode takes surface deviation 0.05mm, 0.1mm, 0.2mm between group, p value is all higher than 0.05, does not have significant difference (table 10);Model is empirically organized data carries out statistical analysis with control group data, takes surface deviation 0.05mm, 0.1mm, 0.2mm When, p value is all higher than 0.05, no difference of science of statistics (table 11).
The experimental group of table 10 and mandibular model fitting Area comparison on control group
The experimental group of table 11 and control group models fitting Area comparison
7th, conclusion
Alginate impression is carried out disinfection using easy guideboard ESS-1 types dental models sterilizing machine, sterilized model with not There is deviation, but sterilization and no significant difference of not sterilizing with master pattern in sterilized model.
Summarize opinion:The operations such as modulus, filling mould in oral cavity diagnosis are possible to take the intraoral bacterium of patient to die With cause cross-infection on model, therefore American Dental Association and disease prevention and control center require that moulage takes in the oral cavity Should be sterilized immediately after going out, in case the generation of communicable disease.The method for being clinically used for buccal impression at present is more, but die Die must be stored in 100% humidity of sealing by the contraction of its spilling water of material such as alginates, this feature of water swelling, sterilization In container, modification is just avoided that.Compared by above result of the test, it is believed that compound double-chain quaternary ammonium salt thimerosal 1 is in dentistry Fine nozzle atomization disinfection is carried out to dental impression silica under conditions of model sterilizing machine is closed, the intersection sense that die causes can be controlled Dye, and the accuracy of die can be kept.
For compound double-chain quaternary ammonium salt thimerosal 2, compound double-chain quaternary ammonium salt thimerosal 3 and compound double-chain quaternary ammonium salt thimerosal 4, with the experimental result similar with compound double-chain quaternary ammonium salt thimerosal 1.
The thimerosal that the present invention is used is a kind of composite disinfection liquid, by by double octyl group/decyl dimethyl ammonium chlorides, ten Dialkyl dimethyl benzyl ammonium chloride and OPA are combined, and nonionic surfactant, inorganic anti-interference agent, synergy The compounding such as agent.
By the hygiene security to thimerosal, bactericidal effect, inactivation of virus experiment, effective content, pH value, stabilization Property, corrosivity etc. have carried out laboratory examination, and combine onsite application, and its interference (is commented using three-dimensional optical digital technology Valency morphotropism), simulated field Disinfection Effect etc. verified.Result shows that the quaternary ammonium salt thimerosal has quickly sterilized Effect, it is safe and healthy have no toxic side effect, have good stability, supported the use with special impression disinfection machine, with good sterilization Effect, to die substantially without metamorphosis, can provide a kind of convenience, effective and ensure moulage dimensional stability for clinic Sterilization method.
In sum, compound double-chain quaternary ammonium salt thimerosal of the invention is sterilized quick, and Disinfection Effect is good, safe and healthy nontoxic Side effect, has good stability, and to dental impression silica substantially without metamorphosis, it is ensured that dental impression silica dimensional stability, it is suitable to big rule Mould popularization and application.
It should be understood by those skilled in the art that the embodiments of the invention shown in foregoing description are only used as illustrating and not limiting The system present invention.
As can be seen here, the purpose of the present invention is achieved completely and effectively.Function of the invention and structural principle Shown in embodiment and illustrated, under without departing substantially from the principle, implementation method can be made any modification.So, this hair The bright all variant embodiments included based on claim spirit and right.

Claims (10)

1. a kind of compound double-chain quaternary ammonium salt thimerosal, it is characterised in that the compound double-chain quaternary ammonium salt thimerosal includes double-strand season Ammonium salt, single-stranded quaternary ammonium salt and OPA, the double-chain quaternary ammonium salt are double octyl alkyl dimethyl ammonium chlorides or double decyl dimethyls Ammonium chloride, the single-stranded quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride.
2. double-chain quaternary ammonium salt thimerosal is combined as claimed in claim 1, it is characterised in that the weight hundred of the double-chain quaternary ammonium salt Content is divided to be 0.04%~0.06%, the weight percentage of the single-stranded quaternary ammonium salt is 0.20%~0.30%, the adjacent benzene The weight percentage of dicarbaldehyde is 0.4%~0.7%.
3. double-chain quaternary ammonium salt thimerosal is combined as claimed in claim 1, it is characterised in that the compound double-chain quaternary ammonium salt sterilization Liquid is also including one or more in nonionic surfactant, inorganic anti-interference agent and synergist.
4. compound double-chain quaternary ammonium salt thimerosal as claimed in claim 3, it is characterised in that the nonionic surfactant is AEO -9 or AEO -10, the inorganic anti-interference agent are EDETATE SODIUM, phosphoric acid hydrogen two Potassium, potassium dihydrogen phosphate, citric acid or sodium citrate, the synergist are that Decyl Polyglucoside, nonyl phenol polyethers -10 or nonyl phenol gather Ether -14.
5. double-chain quaternary ammonium salt thimerosal is combined as claimed in claim 3, it is characterised in that the nonionic surfactant Weight percentage is 1%~5%, and the weight percentage of the inorganic anti-interference agent is 0.01%~0.5%, the synergy The weight percentage of agent is 1%~5%.
6. the application method of a kind of compound double-chain quaternary ammonium salt thimerosal as any one of claim 1 to claim 5, Characterized in that, the compound double-chain quaternary ammonium salt thimerosal is treated into sterilizing objects carries out spraying treatment, then wait to disappear by described Poisonous substance product are placed in gnotobasis for a period of time, then the described compound double-chain quaternary ammonium salt thimerosal on the article to be sterilized is washed It is de-.
7. the application method of double-chain quaternary ammonium salt thimerosal is combined as claimed in claim 6, it is characterised in that the spraying treatment Realize being atomized using nozzle, the process time of the spraying treatment is 30 seconds~60 seconds.
8. the application method of double-chain quaternary ammonium salt thimerosal is combined as claimed in claim 6, it is characterised in that described a period of time It is 5 minutes~10 minutes.
9. a kind of compound double-chain quaternary ammonium salt thimerosal as any one of claim 1 to claim 5 is sprayed in article Application in sterilization.
10. application as claimed in claim 9, it is characterised in that the article is dental models.
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Application publication date: 20170704