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CN1613308A - Antiseptics and preparation thereof - Google Patents

Antiseptics and preparation thereof Download PDF

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Publication number
CN1613308A
CN1613308A CN 200410078338 CN200410078338A CN1613308A CN 1613308 A CN1613308 A CN 1613308A CN 200410078338 CN200410078338 CN 200410078338 CN 200410078338 A CN200410078338 A CN 200410078338A CN 1613308 A CN1613308 A CN 1613308A
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disinfectant
alcohol
test
opa
solution
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Chinese (zh)
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戴彦榛
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Changjiangmai Medicine Science & Technology Co Ltd Beijing
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Changjiangmai Medicine Science & Technology Co Ltd Beijing
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Priority to CN 200410078338 priority Critical patent/CN1613308A/en
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Abstract

A disinfectant is prepared from phthalaldehyde, alcohol, metallic ion chelating agent, non-ionic surfactant, pH regulator or buffer, and water. Its advantages are no poison and irritation to human body, high effect and stability, and low cost.

Description

A kind of disinfectant and preparation method thereof
Technical field
The present invention relates to a kind of disinfectant, more particularly, the present invention relates to a kind of disinfectant that contains o-phthalaldehyde(OPA).
Background technology
Though have in the market much can reach the sterilization and the disinfectants of high-effective disinfecting level, all there is certain drawback separately, strong as: peroxide poor stability, corrosivity; Alkylates class toxicity is big, poor stability; Chloride and brominated class corrosivity is strong, stimulation is big; Aldehydes (formaldehyde, glutaraldehyde) has certain toxicity, excitant, and Disinfection Effect and stability are subject to pH value influence, and metal is had certain corrosivity, and the sterilization shortcoming such as long that takes time.Therefore, the sterilization to hospital clinical and other industry brings inconvenience.
Western developed countries such as the U.S., Canada, Britain, France are developed o-phthalaldehyde(OPA) (English name O-Phthalaldehyde as far back as the nineties in last century; English abbreviation OPA; Molecular formula C 8H 6O 2) antiseptic sterilization agent, realized the quick sterilization of low concentration, nontoxic, non-stimulated, do not have good function such as corrosion, overcome many shortcomings of traditional high-effective disinfecting and bactericidal agent existence, become very popular novel sterile products.But external product enters Chinese market and all occupies high price at present, and difficulty is accepted in market.
In general, OPA is more stable under the condition of lucifuge, close drying and low temperature, yet be exposed to air or but very unstable in the aqueous solution, owing to belong to the OPA polar molecule, the interference of the various ions that are subject to exist in the medium and influence and chemical reaction takes place, wherein easier generation photoreaction under the catalysis of the effect of metal ion and light.
In sum, be badly in need of at present that a kind of production cost of research is low, low, the quick sterilization of active component concentration, disinfectant that physico chemical property are stable.
Summary of the invention
The present invention has toxicity, excitant and corrosivity and Disinfection Effect and poor stability in order to solve existing other type disinfectant, and the problem of ultra-high price of external similar disinfectant, and having proposed a kind of is the disinfectant of main active component with o-phthalaldehyde(OPA).
A kind of disinfectant is made up of the component of following weight percentage:
O-phthalaldehyde(OPA) 0.5～1.0%, alcohol 5.0～60.0%, metal ion chelation agent 0.05～10.0%, non-ionic surface active agent 0.05～10.0%, pH regulator agent or buffer 0.1～10.0%, surplus are water;
The pH of described disinfectant is 8.5～10.5.
There is no particular limitation for the content of o-phthalaldehyde(OPA) in disinfectant of the present invention, and in order to reduce cost and to meet the requirement of low concentration, the content of o-phthalaldehyde(OPA) is preferably in the scope of 0.5～1.0 weight %.
There is no particular limitation for alcohol described in the present invention, can be for having the fatty alcohol of 1～5 carbon atom, its example comprises methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol, amylalcohol or their mixture, and when selecting the mixture of alcohol for use, their mixing ratio can be arbitrary value; Preferred alcohol, propyl alcohol, isopropyl alcohol or their mixture; More preferably ethanol.
The example of described metal ion chelation agent comprises disodium ethylene diamine tetraacetate or nitrilotriacetate NTA, is preferably disodium ethylene diamine tetraacetate.There is no particular limitation for the content of described metal ion chelation agent, is generally 0.05～10.0 weight %.
Described non-ionic surface active agent is preferably aliphatic alcohol polyethenoxy base ether.There is no particular limitation for the content of described non-ionic surface active agent, is generally 0.05～10.0 weight %.
Described pH regulator agent is sodium bicarbonate, sodium carbonate, sodium hydroxide, potassium hydroxide.Described pH regulator agent is preferably sodium bicarbonate.Described pH buffer is dipotassium hydrogen phosphate and potassium dihydrogen phosphate or calcium monohydrogen phosphate.
Effect to each component is described in detail below.
O-phthalaldehyde(OPA) generally exists so that individual molecule is free in the aqueous solution, and free aldehyde radical all can both be brought into play active function, efficiently acts on thereby can bring into play low concentration.O-phthalaldehyde(OPA) is the aromatic aldehyde that has benzene ring structure, have good fat-soluble, to the permeability and the suction-operated of microorganism cultures, have stronger microprotein, enzyme amino generation cross-linking reaction and with the ability and the speed of biochemical reactions such as bacterium endochylema composition, cell membrane, peptide glycan, can produce strong biochemical action to the bacterial spore shell, and cause the shell cracking.Toxic and side effect and little to the corrosion of metal effect is actual nontoxic level product in using concentration range, no teratogenesis, mutagenesis, carcinogenesis.
In order to study the effect of other component, the inventor has designed following four prescriptions, tests.
Fill a prescription 1.: OPA 0.55%+EDTA 0.5%+ water 98.95%
Fill a prescription 2.: OPA 0.55%+EDTA 0.5%+ water 80.95%+ ethanol 18%
Fill a prescription 3.: OPA 0.55%+EDTA 0.5%+ water 80.95%+ ethanol 18%+AEO 0.1%
Fill a prescription 4.: OPA 0.55%+EDTA 0.5%+ water 80.95%+ ethanol 18%+AEO0.1%+NaHCO30.3%
Because o-phthalaldehyde(OPA) is possess hydrophilic property both, have lipophile again, add alcohol and can set up alcohol-aqueous solvent system, strengthen dissolving and the dispersive property of OPA; And ethanol can promote to accelerate the biochemical reaction of OPA and microprotein, enzyme and cell wall and cytoplasm composition, and OPA such as is played at very strong synergistic function.1. the inventor carries out check experiment with 2. two kinds of disinfectants of prescription to prescription, finds under the same conditions, and the disinfectant that adds the ethanol of 18 weight % has improved 11.09% to the killing rate of bacillus subtilis black variety gemma than the disinfectant that does not add ethanol.
Metal ion chelation agent plays a part the huge legendary turtle alloy and belongs to ion stabilized disinfectant of the present invention.Metal ion chelation agent is avoided the chemical action of metal ion and OPA, strengthens the stability of disinfectant of the present invention; Strengthen the dissolubility of OPA in alcohol-aqueous systems, increase the exposed degree of the free aldehyde radical of OPA, the biologically active of raising OPA is destroyed cell wall or membrane structure, leads to change the increase of cell permeability, even causes content to spill, and makes synergistic function thereby rise.The inventor uses disodium ethylene diamine tetraacetate (EDTA) as metal ion chelation agent, under the situation that does not add non-ionic surface active agent, two kinds of disinfectants that do not add EDTA and the EDTA that adds 0.5 weight % have been carried out stable comparative trial, result of the test is: 37 ℃ of temperature with after quite humidity is placed 90 days 75% time, the adding of EDTA makes the rate of descent of O-phthalic aldehyde be reduced to 7.58% from 15.55%.
Non-ionic surface active agent plays dissolving and the dispersion that strengthens OPA, strengthens the effect of OPA stability of solution.Non-ionic surface active agent improves the permeability of microorganism wall and cell membrane largely, strengthen the osmosis of OPA to microorganism, quicken the biochemical reaction of OPA and compositions such as microprotein, enzyme, cell wall and endochylema, improve the sterilization effect of OPA; Simultaneously can reduce microorganism and organic surface tension, strengthen the anti-organic matter interference performance of OPA, and strengthen the dirt-removing functions of this product.The inventor uses aliphatic alcohol polyethenoxy base ether (AEO) as non-ionic surface active agent, contrasted prescription 2. with the killing rate of prescription disinfectant 3. to bacillus subtilis black variety gemma, result of the test shows: under the same conditions, add the killing rate raising 5.03% of the disinfectant of AEO to bacillus subtilis black variety gemma.The inventor tests with the stability of the disinfectant of the AEO that adds 0.1 weight % not adding AEO in addition.Result of the test shows that 37 ℃ of temperature with after quite humidity is placed 90 days 75% time, the adding of AEO makes the rate of descent of O-phthalic aldehyde drop to 3.22% from 7.58% again.
PH regulator agent or buffer are with pH regulator to 8.5～10.5 of disinfectant of the present invention.The OPA generally action effect under alkali condition is stronger than the Disinfection Effect under neutrality or acid condition.The inventor with pH regulator to 8.5～9.0 of disinfectant, brings up to 100% to the killing rate of bacillus subtilis black variety gemma from 99.19% the sodium bicarbonate that adds 0.3 weight % in prescription disinfectant 3. (prescription 4.).
The preparation method of disinfectant of the present invention may further comprise the steps:
(1) add the water of alcohol, metal ion chelation agent, non-ionic surface active agent and 80% in reactor, stirring and dissolving is 30～60 minutes under 30～40 ℃ of temperature, formation stabilized uniform dicyandiamide solution;
(2) add o-phthalaldehyde(OPA) in the dicyandiamide solution that step (1) obtains, agitating solution is 50～70 minutes under 30～40 ℃ of temperature, forms stabilized uniform o-phthalaldehyde(OPA) solution;
(3) with remaining 20% water-soluble pH regulator agent or the buffer separated, filter the solution that obtains, the solution that filters is joined the o-phthalaldehyde(OPA) solution that step (2) obtains, stirred 10～20 minutes, the pH value of solution is 8.5～9.0, leaves standstill 20～40 minutes, filters and obtains disinfectant of the present invention.
Purposes and usage:
Sterilization:
Be used for various operating theater instruments, bladder, joint and laparoscope class, hemodialysis pipeline, biopsy pincers etc. need reach the various medicine equipments and the article of sterilization level.
Soaked 4 hours with disinfectant of the present invention, aseptic taking-up, aseptic water washing, aseptic preservation is standby.
Sterilization:
1. general curative apparatus, intestines and stomach and respiratory tract endoscope class etc.Soaked 10 minutes, clear water washes down.
2. the apparatus that uses of tuberculosis patient, hepatitis B patient.Soaked 15 minutes, clear water washes down.
3. the sterilization before the sterilization of medical instrument.Soaked 15 minutes, clear water washes down.
4. environment disinfected.Spray disinfectant.
5. life sterilisation of objects.Soaked 10 minutes, clear water washes down.
For the performances such as Disinfection Effect, toxicity, excitant and stability of verifying disinfectant of the present invention, the concrete disinfectant that the following row components in weight percentage of inventor is formed entrusts Beijing Disease Prevention and Control Centre to detect:
O-phthalaldehyde(OPA) 0.55%, ethanol 18%, fatty alcohol-polyoxyethylene ether 0.1%, disodium ethylene diamine tetraacetate 0.5%, sodium bicarbonate 0.3%, distilled water 80.55%.
Wherein part test is as follows.
1. acute oral toxicity test
(1) sample pre-treatments: take by weighing respectively and tried thing 4.64g, 2.15g, 1g, add deionized water to 10ml, mixing, concentration is 0.464g/ml, 0.25g/ml, 0.1g/ml.
21500mg/kg group and 10000mg/kg group are directly used degree of being subjected to thing stoste (1g/ml)
(2) experimental animal: 50 of cleaning level Kunming mouses, male and female half and half, body weight 18～22g.Provide by Military Medical Science Institute's Experimental Animal Center.The animal quality certification number: the capital is moving is betrothed to No. 99001.
(3) experimental animal feeding environment: room temperature is 20～25 ℃, and relative moisture is 46～53%RH, and group's cage is raised 5/cage.
Feed resource: Jiujiang, Chaoyang District, Beijing City mouth feed factory.The feed quality certification number: the capital is moving is betrothed to (2000) No. 007.
The Animal Lab. quality certification number: SYXK (capital) 2002-0022 number.
(4) test method: (horn method)
The laboratory animal quarantine is after 3 days, select 50 of healthy adult mouse, body weight 18～22g, female, hero half and half, dosage design is female to be 21500,10000,4640,2150/kgBW, malely be 10000,4640,2150,1000mg/kgBW, (the 21500mg/kg group gives the per os of 0.2ml stoste/10gBW) and irritates stomach and tried thing by 0.1ml/10gBW.Irritate the preceding animal overnight fasting of stomach, freely drink water.Give normal diet after irritating stomach, observed for two weeks, record poisoning sign and death condition.
(5) result of the test
(5-1) experimental session animal dead situation:
Dosage (mg/kgBW) Sex Number of animals (only) Dead animal number (only) Lethality (%)
??21500 Male and female ??5 ??- ??5 ??- ??100 ??-
??10000 Male and female ??5 ??5 ??2 ??0 ??40 ??0
??4640 Male and female ??5 ??5 ??1 ??0 ??20 ??0
??2150 Male and female ??5 ??5 ??0 ??0 ??0 ??0
??1000 Male and female ??- ??5 ??- ??0 ??- ??0
(5-2) in 14 days observation period, each organizes male mouse body weight gain, does not see death, the gross anatomy no abnormality seen.21500,10000,4640 groups of death toll of female mouse are respectively 5,2,1, the body no abnormality seen.Surviving animals gross anatomy no abnormality seen.
Female mice per os LD 50(95% crediblely is limited to 5700～15000mg/kgBW) for 9260mg/kgBW.
Male mice per os LD 50For greater than 10000mg/kgBW.
(6) conclusion (of pressure testing)
Judge according to acute toxicity pole marks in " disinfection technology standard " (1999) is accurate, deciding under the experiment condition strong female, the male mice per os LD of plain board O-phthalic disinfectant 505000mg/kgBW belongs to poison level practically.
2. acute skin irritation test
(1) sample pre-treatments: directly with being tried thing stoste.
(2) experimental animal: 4 of rabbit, male and female half and half, body weight 2.5～3.0kg plant in one grade of New Zealand.Culturing factory by Beijing tonneau laboratory animal provides, the animal quality certification number: the capital is moving is betrothed to (2000) No. 024.
(3) experimental animal feeding environment: room temperature is 21～25 ℃, and relative moisture is 47～51%RH, and single cage is raised.
Feed resource: Jiujiang, Chaoyang District, Beijing City mouth feed factory.The feed quality certification number: the capital is moving is betrothed to (2000) No. 007.
The Animal Lab. quality certification number: SUXK (capital) 2002-0022 number.
(4) test method
Select 4 of the intact healthy rabbits of skin for use, its post both sides, back were cut left and right each the about 3cm * 3cm of unhairing area by hair in preceding 24 hours in test.Get during test and tried to be applied to a side fur skin surface on two layers of gauze that thing 0.2ml is applied to 2.5cm * 2.5cm, oilpaper covers, immobilization with adhesive tape.Opposite side skin is as blank.Seal after 4 hours, prop up and remove covering, and remove going or staying with the warm water cleaning and tried thing, the observation in 1,24 and 48 hour after removal is tried thing is coated with the skin reaction of reactionaries position, and scoring.
(5) result of the test:
Numbering Body weight (kg) 1 hour 24 hours 48 hours
The sample contrast The sample contrast The sample contrast
The swollen spot of red bright pink water spots is swollen The swollen spot of red bright pink water spots is swollen The swollen spot of red bright pink water spots is swollen
1 2 3 4 ?2.7 ?2.8 ?3.0 ?2.5 ??0???0???0???0 ??0???0???0???0 ??0???1???0???0 ??0???0???0???0 ??0???0???0???0 ??0???0???0???0 ??0???1???0???0 ??0???0???0???0 ??0???0???0???0 ??0???0???0???0 ??0???0???0???0 ??0???0???0???0
Integral mean value ??0.25?????0.0 ??0.25?????0.0 ??0.0??????0.0
Stimulus intensity Nonirritant nonirritant nonirritant
(6) conclusion (of pressure testing)
Judge according to skin irritatin reaction standards of grading in " disinfection technology standard " (1999), tried thing disinfectant of the present invention and under this experiment condition, be nonirritant.
3. PCEMNR micronucleus test
(1) sample pre-treatments: take by weighing respectively and tried thing 5.0,2.0,0.5 gram, add deionized water to 10ml, mixing is made into that concentration is respectively 0.5g/ml, 0.25g/ml, 0.1g/ml is subjected to test solution.
(2) experimental animal: 50 of cleaning level Kunming mouses, male and female half and half, body weight 25～30g.Provide by Military Medical Science Institute's Experimental Animal Center.
The animal quality certification number: the capital is moving is betrothed to No. 99001.
(3) experimental animal feeding environment: room temperature is that room temperature is 20～22 ℃, and relative moisture is 30～35%RH, and group's cage is raised 5/cage.
Feed resource: Jiujiang, Chaoyang District, Beijing City mouth feed factory.The feed quality certification number: the capital is moving is betrothed to (2000) No. 007.
The Animal Lab. quality certification number: SYXK (capital) 2002-0022 number.
(4) test method
Select 50 healthy mices for use, be divided into 5 groups with grid, every group female, male each 5, establish three dosage groups altogether, the dosage design is respectively 1/2LD 50, 1/50LD 50, 1/20LD 50, promptly being equivalent to 5000,2000, the 500mg/kg body weight, other establishes negative control and positive controls, and positive group gives cyclophosphamide 40mg/kgBW.Tried the equal per os of thing and positive thing and irritate stomach, adopt 30 hours dose regimens, promptly twice dosing interval is 24 hours, after the last administration 6 hours, routine was got breastbone film-making, fixing, dyeing, under oily mirror every animal is observed 1000 polychromatic erythrocytes, calculate micronuclear rates, carry out statistical analysis.
(5) result of the test
Dosage The sex number of animals is had a liking for polychromatocyte micronucleus cell micronuclear rates PEC/NCE (mg/kgBW) (only) number (individual) number (individual) (‰)
Negative control Female 55 * 1,000 9 1.8 1.15 ± 0.10 male 55 * 1,000 7 1.4 1.25 ± 0.19
Low dosage (500) Female 55 * 1,000 8 1.6 1.10 ± 0.17 male 55 * 1,000 6 1.2 1.48 ± 0.33
Middle dosage (2000) Female 55 * 1,000 9 1.8 1.31 ± 0.18 male 55 * 1,000 9 1.8 1.29 ± 0.21
High dose (5000) Female 55 * 1,000 12 3.0 1.36 ± 0.24 male 55 * 1,000 16 3.2 1.30 ± 0.17
Positive control Female 55 * 1,000 198 39.2 1.10 ± 0.22 male 55 * 1,000 214 42.8 1.13 ± 0.18
(6) conclusion (of pressure testing)
According to PCEMNR nuclear test standard determination in " disinfection technology standard " (1999), disinfectant PCEMNR nuclear test result of the present invention is negative.
4. cumulative toxicity test
(1) sample pre-treatments: take by weighing respectively and tried thing 0.5g, 0.75g, 1.1g, 1.7g, 2.5g, 10ml mixing.Now join for each issue.
(2) experimental animal: 20 of cleaning level Kunming mouses, body weight 18～20g.Provide by Military Medical Science Institute's Experimental Animal Center.
The animal quality certification number: the capital is moving is betrothed to No. 99001.
(3) experimental animal feeding environment: room temperature is that room temperature is 21～24 ℃, and relative moisture is 44～54%RH, and group's cage is raised 10/cage.
Feed resource: Jiujiang, Chaoyang District, Beijing City mouth feed factory.The feed quality certification number: the capital is moving is betrothed to (2000) No. 007.
The Animal Lab. quality certification number: SYXK (capital) 2002-0022 number.
(4) test method: (dosage escalation cumulative coefficient method)
Select 20 healthy mices for use, female, male each 10, according to dosage increase progressively cumulative coefficient method design dosage, female, the property of this given the test agent, the LD of male mice 50All greater than 5000mg/kgBW, dosage is respectively 500,750,1100,1700,2500mg/kgBW so establish.Weigh before irritating stomach each issue, adjust dosage, press the 0.1ml/10BW per os and irritate stomach.Cumulative coefficient is calculated in off-test after 20 days.
(5) result of the test
The accumulation test result
The contamination fate (my god) 1～4 5～8 9～12 13～16 17～20
Every day poisoning dosage (LD 50) 0.10 0.15 0.22 0.34 0.50
Accumulation poisoning dosage (LD 50) 0.40 1.00 1.90 3.26 5.26
Jenny death toll (only) 00000
Buck death toll (only) 00000
As seen from the above table, jenny accumulation death toll is 1, and buck accumulation death toll is 0.The duration of test animal increases to some extent, and female mouse was dead 1 in the 16th day, no abnormality seen.Surviving animals is in the 21st dead beyond the highest heavens, the gross anatomy no abnormality seen, and calculating cumulative coefficient is 5.26.
(6) conclusion (of pressure testing)
According to cumulative toxicity split pole standard determination in " disinfection technology standard " (1999), under this experiment condition, disinfectant cumulative coefficient of the present invention is the weak property accumulated greater than 5.
5. colibacillaryly kill test
(1) test strain: the 6th generation of Escherichia coli 8099 (Military Medical Science Institute provides).
(2) neutralizer: the PBS that contains 0.8% glycine, Tween-80,0.5% lecithin
(3) stainless steel carrier (diameter 1.5cm disk)
(4) test basis: " disinfection technology standard " third edition. first fascicle 2.4.1.6 and the 2.6.4.2.
(5) neutralizer approval test method: experimental concentration is 5969mg/L for strong plain board O-phthalic aldehyde; Sterilizing time is 1min; In and the time be 10min; Experimental condition is 20-22 ℃ of water-bath; The test triplicate adopts carrier to soak quantitative disinfecting test neutralizer approval test method.
(6) bactericidal assay method: experimental condition is 20-22 ℃; The test triplicate.Adopt carrier to soak the quantitative disinfecting test method.
(7) result of the test
(7-1) neutralizer approval test result: under 20-22 ℃ of water bath condition, through three repeated test results, error is 1.29% between the 3rd, 4,5 group three groups; 6th, 7,8 groups of asepsis growths.
Neutralizer approval test result
Each test growth bacterium number (cfu sheet) bacterium that on average grows
Group 123 numbers (cfu sheet)
1???????0????????????0????????????0????????????0
2???????1.20×10 2???1.60×10 2??1.15×10 2???1.32×10 2
3???????1.46×10 2???1.84×10 2??1.25×10 2???1.52×10 2
4???????1.60×10 2???1.89×10 2??1.22×10 2???1.57×10 2
5???????1.57×10 2???1.96×10 2??1.16×10 2???1.56×10 2
6???????0????????????0????????????0????????????0
7???????0????????????0????????????0????????????0
8???????0????????????0????????????0????????????0
(7-2) bactericidal assay result:
Under 20-22 ℃ of water bath condition, prove that through three repeated test results strong plain board O-phthalaldehyde disinfectant O-phthalic aldehyde 4800mg/L dilution effect 1min is 99.92% (99.91%-99.93%) to colibacillary average kill ratio; It is 99.92% (99.92%-99.93%) to colibacillary average kill ratio that O-phthalic aldehyde 3600mg/L dilution is made 7min.
Bactericidal assay result
The Soviet Union's rate of on average going out of O-phthalic aldehyde effect different time (min) and scope (%)
(mg/L)????????????1??????????????3????????????????5????????????????7
5969?????????????99.99??????????100.00???????????100.00???????????100.00
(99.99-99.99)??(100.00-100.00)??(100.00-100.00)??(100.00-100.00)
4800?????????????99.92??????????99.97????????????99.99????????????100.00
(99.91-99.93)??(99.97-99.99)????(99.99-100.00)???(100.00-100.00)
3600?????????????84.62??????????95.63????????????99.52????????????99.92
(83.40-85.60)??(94.61-97.13)????(99.42-99.62)????(99.92-99.93)
Positive control: 1.56 * 10 6Cfu/ sheet (1.16 * 10 6-1.96 * 10 6The cfu/ sheet)
Neutralizer, PBS, the equal asepsis growth of medium negative control.
(8) conclusion (of pressure testing)
Under 20-22 ℃ of water bath condition, prove through three repeated test results, the PBS that contains 0.8% glycine, 3% Tween-80,0.5% lecithin disinfectant of the present invention to escherichia coli vector theorem bactericidal assay neutralizer approval test in, in can be effectively and disinfectant O-phthalic aldehyde of the present invention be the residual action of 5969mg/L to test organisms, and neutralizer, neutralized reaction product to test organisms growth do not have obviously influence.
Disinfectant O-phthalic aldehyde 4800mg/L dilution effect 1mim of the present invention, 3600mg/L dilution effect 7min are 99.92% to colibacillary average kill ratio.
6. staphylococcus aureus kills test
(1) test strain: the 7th generation of staphylococcus aureus ATCC6538 (Military Medical Science Institute provides).
(2) neutralizer: the PBS that contains 0.8% glycine, 3% Tween-80,0.5% lecithin
(3) stainless steel carrier (diameter 1.5cm disk)
(4) test basis: " disinfection technology standard " third edition. the first fascicle 2.6.4.2.
(5) bactericidal assay method: experimental condition is 20-22 ℃; The test triplicate.Adopt carrier to soak the quantitative disinfecting test method.
(6) result of the test
Under 20-22 ℃ of water bath condition, prove that through three repeated test results strong plain board O-phthalaldehyde disinfectant O-phthalic aldehyde 4800mg/L dilution effect 1min is 99.93% (99.92%-99.94%) to colibacillary average kill ratio; It is 99.94% (99.94%-99.95%) to colibacillary average kill ratio that O-phthalic aldehyde 3600mg/L dilution is made 7min.
Bactericidal assay result
The Soviet Union's rate of on average going out of O-phthalic aldehyde effect different time (min) and scope (%)
(mg/L)?????????????1??????????????3????????????????5????????????????7
5969???????????????99.99??????????100.00???????????100.00???????????100.00
(99.99-99.99)??(100.00-100.00)??(100.00-100.00)??(100.00-100.00)
4800???????????????99.93??????????99.98????????????99.99????????????100.00
(99.92-99.94)??(99.98-99.99)????(99.99-100.00)???(100.00-100.00)
3600???????????????87.24??????????96.64????????????99.62????????????99.94
(86.42-88.59)???(96.19-97.14)????(99.52-99.69)????(99.94-99.95)
Positive control: 1.63 * 10 6Cfu/ sheet (1.16 * 10 6-1.92 * 10 6The cfu/ sheet)
Neutralizer, PBS, the equal asepsis growth of medium negative control.
(7) conclusion (of pressure testing):
The average kill ratio of disinfectant O-phthalic aldehyde 4800mg/L dilution effect 1mim staphylococcus aureus of the present invention is 99.93%; The average kill ratio of O-phthalic aldehyde 3600mg/L diluting effect 7mim staphylococcus aureus is 99.94%.
7. Candida albicans kills test
(1) the 7th generation of test strain: Candida albicans ATCC 10231 (Military Medical Science Institute provides).
(2) neutralizer: the PBS that contains 0.8% glycine, 3% Tween-80,0.5% lecithin
(3) stainless steel carrier (diameter 1.5cm disk)
(4) test basis: " disinfection technology standard " third edition. first fascicle 2.4.1.6 and the 2.6.4.2.
(5) neutralizer approval test method: experimental concentration is 5969mg/L for strong plain board O-phthalic aldehyde; Sterilizing time is 1min; In and the time be 10min; Experimental condition is 20-22 ℃ of water-bath; The test triplicate adopts carrier to soak quantitative disinfecting test neutralizer approval test method.
(6) bactericidal assay method: experimental condition is 20-22 ℃; The test triplicate.Adopt carrier to soak the quantitative disinfecting test method.
(7) result of the test
Neutralizer approval test result: under 20-22 ℃ of water bath condition, through three repeated test results, error is 1.63% between the 3rd, 4,5 group three groups; 6th, 7,8 groups of asepsis growths.
Neutralizer approval test result
Each test growth bacterium number (cfu sheet) bacterium number of on average growing
Group 123 (cfu sheet)
1???????0????????????0????????????0????????????0
2???????6.95×10 2???6.15×10 2??6.80×10 2???6.63×10 2
3???????8.15×10 5???7.80×10 5??8.60×10 5???8.18×10 5
4???????8.70×10 5???7.45×10 5??9.40×10 5???8.52×10 5
5???????9.10×10 5???7.15×10 5??9.10×10 5???8.45×10 5
6???????0????????????0????????????0????????????0
7???????0????????????0????????????0????????????0
8???????0????????????0????????????0????????????0
Bactericidal assay result: under 20-22 ℃ of water bath condition, prove that through three repeated test results strong plain board O-phthalaldehyde disinfectant O-phthalic aldehyde is that the on average rate of going out that 5969mg/L effect effect 1min reads the ring bacterium to white is 99.91% (99.91%-99.92%); O-phthalic aldehyde 4800mg/L dilution effect 3min is 99.93% (99.92%-99.94%) to the oidiomycetic average kill ratio of white.
Bactericidal assay result
The Soviet Union's rate of on average going out of O-phthalic aldehyde effect different time (min) and scope (%)
(mg/L)????????????1??????????????3??????????????5????????????????7
5969??????????????99.91??????????99.99??????????100.00???????????100.00
(99.91-99.92)??(99.99-99.99)??(100.00-100.00)??(100.00-100.00)
4800??????????????99.86??????????99.93??????????99.99????????????100.00
(99.81-99.89)??(99.92-99.94)??(99.99-100.00)???(100.00-100.00)
3600??????????????80.22??????????91.18??????????99.09????????????99.86
(79.23-81.60)??(90.69-91.70)??(99.04-99.17)????(99.79-99.90)
Positive control 8.45 * 10 5Cfu/ sheet (7.15 * 10 5-9.10 * 10 5The cfu/ sheet)
Neutralizer, PBS, the equal asepsis growth of medium negative control.
(8) conclusion (of pressure testing)
Under the 20-22 water bath condition, prove through three repeated test results, contain 0.8% glycine, 3% Tween-80.The PBS of 05% lecithin disinfectant of the present invention to Candida albicans carrier quantitative germicidal test neutralizer approval test in, in can be effectively and O-phthalaldehyde disinfectant O-phthalic aldehyde of the present invention be the residual action of 5969mg/L to test organisms, and neutralizer, neutralized reaction product do not have obviously influence to the test growth.
Disinfectant O-phthalic aldehyde of the present invention is that 5969mg/L effect 1min is 99.91% to the oidiomycetic average kill ratio of white; O-phthalic aldehyde 4800mg/L dilution effect 3min is 99.93% to the average kill ratio of white pearl bacterium.
Bacillus subtilis black variety bud cell kill test
(1) test strain: bacillus subtilis var ATCC 9372 brood cells (Military Medical Science Institute provides)
(2) neutralizer: the PBS that contains 0.8% glycine, 3% Tween-80,0.5 lecithin.
(3) stainless steel carrier (diameter 1.5cm disk).
(4) test basis: " disinfection technology standard " third edition, first fascicle 2.4.1.6 and the 2.6.4.2.
(5) neutralizer approval test method: experimental concentration is 5969mg/L for strong plain O-phthalaldehyde disinfectant O-phthalic aldehyde; Sterilizing time is 60min; In and the time be 10min; Experimental condition is 20-22 ℃ of water-bath; The test triplicate.Adopt carrier to soak quantitative disinfecting test neutralizer approval test method.
(6) bactericidal assay method: experimental condition 20-22 ℃; The test triplicate.Adopt carrier to soak the quantitative disinfecting test method.
(7) result of the test
Neutralizer approval test result:
Under 20-22 ℃ of water bath condition, through three repeated test results, error rate is 1.39% between the 3rd, 4,5 group three groups; 6th, 7,8 groups of asepsis growths.
Neutralizer approval test result
Each test growth bacterium number (cfu sheet) bacterium number of all growing
Group 123 (cfu sheet)
1????????0????????????0????????????0????????????0
2????????1.02×10 3???1.70×10 3??2.10×10 3???1.61×10 3
3????????1.06×10 6???1.68×10 6??2.27×10 6???1.67×10 6
4????????1.19×10 6???1.54×10 6??2.26×10 6???1.66×10 6
5????????1.19×10 6???1.63×10 6??2.34×10 6???1.72×10 6
6????????0????????????0????????????0????????????0
7????????0????????????0????????????0????????????0
8????????0????????????0????????????0????????????0
Bactericidal assay result:
Under 20-22 ℃ of water bath condition, prove that through three repeated test results strong plain O-phthalaldehyde disinfectant O-phthalic aldehyde is 5969mg/L effect 70min to withered grass bacterium black mutation born of the same parents' the on average rate of going out is that the average kill ratio that 99.94% (99.94%-99.95%), effect 120min join withered grass bacterium black mutation tooth born of the same parents is 100.00% (100.00%-100.00%).
Bactericidal assay result
The Soviet Union's rate of on average going out of O-phthalic aldehyde effect different time (min) and scope (%)
(mg/L)????????????70?????????????90??????????????120??????????????150
5969??????????????99.94??????????99.99???????????100.00???????????100.00
(99.94-99.95)??(99.99-100.00)??(100.00-100.00)??(100.00-100.00)
4800??????????????99.14??????????99.94???????????99.99????????????99.99
(99.08-99.24)??(99.94-99.95)???(99.99-100.00)???(100.00-100.00)
3600??????????????83.70??????????92.38???????????99.46????????????99.94
(81.11-86.53)??(91.55-93.71)???(99.34-99.53)????(99.94-99.95)
Positive control 1.72 * 10 6Cfu/ sheet (1.19 * 10 6-2.34 * 10 6The cfu/ sheet)
Neutralizer, PBS, the equal asepsis growth of medium negative control.
(8) conclusion (of pressure testing)
Under 20-22 ℃ of water bath condition, prove through three repeated test results, contain 0.8% glycine, 3% Tween-80.The PBS of 0.5% lecithin disinfectant of the present invention to withered grass bacterium black mutation brood cell carrier quantitative germicidal test neutralizer approval test in, the disinfectant O-phthalic aldehyde of the present invention that can effectively neutralize is the residual action of 5969mg/L to test organisms, and neutralizer, neutralized reaction product do not have obviously influence to the test growth.
Disinfectant O-phthalic aldehyde of the present invention is 5969mg/L effect 70min to withered grass bacterium black mutation brood cell's average kill ratio is that 99.94% (99.94%-99.95%), effect 120min are 100.00% (100.00%-100.00%) to withered grass bacterium black mutation brood cell's average kill ratio.
9. stability test
(1) test basis: " disinfection technology standard " third edition, first fascicle 424
(2) test method: seal-packed disinfectant stock solution of the present invention is put 37 ℃ of constant temperature deposit and test after 14 days.Measure three duplicate samples, every duplicate samples replication three times is got its mean value.
(3) result of the test
Prove through three replication results, disinfectant stock solution of the present invention after 37 ℃ of constant temperature are deposited 90 days, stoste O-phthalic aldehyde average out to 0.5672% (W/V), O-phthalic aldehyde rate of descent average out to 4.98%.
The stability test result
The sample sequence number O-phthalic aldehyde (%) before 37 ℃ of preservations O-phthalic aldehyde (%) after 37 ℃ of preservations Rate of descent (%)
????1-1 ??0.6097 ??0.5735
????1-2 ??0.5904 ??0.5546
????1-3 ??0.6097 ??0.5735
????2-1 ??0.5904 ??0.5546
????2-2 ??0.5904 ??0.5735
????2-3 ??0.5904 ??0.5735
????3-1 ??0.6097 ??0.5735
????3-2 ??0.5904 ??0.5735
????3-3 ??0.5904 ??0.5546
Mean value ??0.5969 ??0.5672 4.98
(4) conclusion (of pressure testing)
O-phthalaldehyde disinfectant stoste of the present invention after 37 constant temperature are deposited 90 days, stoste O-phthalic aldehyde average out to 0.5672%, O-phthalic aldehyde rate of descent average out to 4.98%.
In addition, can find out significantly that from the component of disinfectant of the present invention disinfectant of the present invention does not have corrosivity.And detect through Beijing Disease Prevention and Control Centre, disinfectant of the present invention has the moderate corrosion to copper, and stainless steel, carbon steel are not had corrosion, does not have corrosion to aluminium base.
Embodiment
Adopt the mode of specific embodiment to explain the present invention below, but the present invention is not limited to these embodiment.
Embodiment 1
(1) add 18kg ethanol, 0.5kg disodium ethylene diamine tetraacetate, 0.1kg fatty alcohol-polyoxyethylene ether and 64kg water in reactor, stirring and dissolving is 45 minutes under 30～40 ℃ of temperature, forms the stabilized uniform dicyandiamide solution;
(2) add the 0.55kg o-phthalaldehyde(OPA) in the dicyandiamide solution that step (1) obtains, agitating solution is 60 minutes under 30～40 ℃ of temperature, forms stabilized uniform o-phthalaldehyde(OPA) solution;
(3) with the water-soluble sodium bicarbonate of separating 0.3kg of 16.55kg, filter the solution that obtains, the solution that filters is joined the o-phthalaldehyde(OPA) solution that step (2) obtains, stirred 115 minutes, the pH value of solution is 8.8, leaves standstill 30 minutes, filtration obtains disinfectant of the present invention, and pH is 9.
The disinfectant that present embodiment makes has following composition:
O-phthalaldehyde(OPA) 0.55%, ethanol 18%, fatty alcohol-polyoxyethylene ether 0.1%, disodium ethylene diamine tetraacetate 0.5%, sodium bicarbonate 0.3%, distilled water 80.95%.
Embodiment 2
The preparation method is identical with embodiment 1, and different is to form content:
O-phthalaldehyde(OPA) 1.0%, propyl alcohol 40.0%, disodium ethylene diamine tetraacetate 0.01%, fatty alcohol-polyoxyethylene ether 5.0%, sodium hydroxide 0.1%, water 63.89%, pH are 9.5.

Claims (10)

1. a disinfectant is characterized in that, it is made up of the component of following weight percentage:
O-phthalaldehyde(OPA) 0.5～1.0%, alcohol 5.0～60.0%, metal ion chelation agent 0.05～10.0%, non-ionic surface active agent 0.05～10.0%, pH regulator agent or buffer 0.1～10.0%, surplus are water;
The pH of described disinfectant is 8.5～10.5.
2. according to the disinfectant of claim 1, it is characterized in that described alcohol is the fatty alcohol with 1～5 carbon atom.
3. according to the disinfectant of claim 1, it is characterized in that described alcohol is ethanol, propyl alcohol, isopropyl alcohol or their mixture.
4. according to the disinfectant of claim 1, it is characterized in that described alcohol is ethanol.
5. according to the disinfectant of claim 1, it is characterized in that described metal ion chelation agent is disodium ethylene diamine tetraacetate or nitrilotriacetate NTA.
6. according to the disinfectant of claim 1, it is characterized in that described non-ionic surface active agent is an aliphatic alcohol polyethenoxy base ether.
7. according to the disinfectant of claim 1, it is characterized in that described pH regulator agent is sodium bicarbonate, sodium carbonate, sodium hydroxide, potassium hydroxide.
8. according to the disinfectant of claim 1, it is characterized in that described pH buffer is dipotassium hydrogen phosphate and potassium dihydrogen phosphate or calcium monohydrogen phosphate.
9. according to the disinfectant of claim 1, it is characterized in that described pH regulator agent is a sodium bicarbonate.
10. the preparation method of the disinfectant of claim 1 is characterized in that, it may further comprise the steps:
(1) add the water of alcohol, metal ion chelation agent, non-ionic surface active agent and 80% in reactor, stirring and dissolving is 30～60 minutes under 30～40 ℃ of temperature, formation stabilized uniform dicyandiamide solution;
(2) add o-phthalaldehyde(OPA) in the dicyandiamide solution that step (1) obtains, agitating solution is 50～70 minutes under 30～40 ℃ of temperature, forms stabilized uniform o-phthalaldehyde(OPA) solution;
(3) with remaining 20% water-soluble pH regulator agent or the buffer separated, filter the solution that obtains, the solution that filters is joined the o-phthalaldehyde(OPA) solution that step (2) obtains, stirred 10～20 minutes, the pH value of solution is 8.5～9.0, leaves standstill 20～40 minutes, filters and obtains disinfectant of the present invention.
CN 200410078338 2004-09-24 2004-09-24 Antiseptics and preparation thereof Pending CN1613308A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
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CN101821224A (en) * 2007-04-05 2010-09-01 马丁家族托拉斯 Method for stabilizing aldehydes
CN101926362A (en) * 2009-06-23 2010-12-29 上海利康消毒高科技有限公司 Compound orthophaladetyde phenyl ammonium chloride disinfectant and preparation method thereof
CN102197811A (en) * 2011-04-12 2011-09-28 陈义平 Compound orthophthalaldehyde disinfectant
US8088829B2 (en) * 2009-09-09 2012-01-03 Howard Martin Biocidal aldehyde composition
CN102461499A (en) * 2010-11-17 2012-05-23 民政部一零一研究所 Disinfector for remains and preparation method thereof
CN101785460B (en) * 2009-01-23 2013-12-18 上海利康消毒高科技有限公司 O-phthalaldehyde disinfectant and preparation method thereof
CN103636601A (en) * 2013-12-10 2014-03-19 山东新华医疗器械股份有限公司 O-phthalaldehyde disinfectant and preparation method thereof
CN104621104A (en) * 2015-02-02 2015-05-20 山东威高药业股份有限公司 Disinfectant with low corrosiveness
CN106614579A (en) * 2016-10-12 2017-05-10 南京金甙尔生物技术有限公司 Disinfectant and application thereof
CN107711835A (en) * 2017-11-07 2018-02-23 济南市利东医疗设备有限公司 A kind of O-phthalaldehyde disinfectant and preparation method thereof
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101821224B (en) * 2007-04-05 2015-08-19 马丁家族托拉斯 Methods of Stabilizing Aldehydes
CN101821224A (en) * 2007-04-05 2010-09-01 马丁家族托拉斯 Method for stabilizing aldehydes
CN101785460B (en) * 2009-01-23 2013-12-18 上海利康消毒高科技有限公司 O-phthalaldehyde disinfectant and preparation method thereof
CN101926362A (en) * 2009-06-23 2010-12-29 上海利康消毒高科技有限公司 Compound orthophaladetyde phenyl ammonium chloride disinfectant and preparation method thereof
US8088829B2 (en) * 2009-09-09 2012-01-03 Howard Martin Biocidal aldehyde composition
CN102461499B (en) * 2010-11-17 2014-06-18 民政部一零一研究所 Disinfector for remains and preparation method thereof
CN102461499A (en) * 2010-11-17 2012-05-23 民政部一零一研究所 Disinfector for remains and preparation method thereof
CN102197811B (en) * 2011-04-12 2014-03-12 陈义平 Compound orthophthalaldehyde disinfectant
CN102197811A (en) * 2011-04-12 2011-09-28 陈义平 Compound orthophthalaldehyde disinfectant
CN103636601A (en) * 2013-12-10 2014-03-19 山东新华医疗器械股份有限公司 O-phthalaldehyde disinfectant and preparation method thereof
CN103636601B (en) * 2013-12-10 2015-08-05 山东新华医疗器械股份有限公司 O-phthalaldehyde disinfectant and preparation method thereof
CN104621104A (en) * 2015-02-02 2015-05-20 山东威高药业股份有限公司 Disinfectant with low corrosiveness
CN106614579A (en) * 2016-10-12 2017-05-10 南京金甙尔生物技术有限公司 Disinfectant and application thereof
CN107711835A (en) * 2017-11-07 2018-02-23 济南市利东医疗设备有限公司 A kind of O-phthalaldehyde disinfectant and preparation method thereof
US11497581B2 (en) 2018-11-05 2022-11-15 Medivators Inc. Endoscope cleaning and inspection system and method
US11793601B2 (en) 2018-11-05 2023-10-24 Medivators Inc. Endoscope cleaning and inspection system and method
US12245904B2 (en) 2018-11-05 2025-03-11 Medivators Inc. Endoscope cleaning and inspection system and method
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