CN102416011A - Broad-spectrum and high-efficiency antibacterial washing liquor - Google Patents
Broad-spectrum and high-efficiency antibacterial washing liquor Download PDFInfo
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- CN102416011A CN102416011A CN2011103050329A CN201110305032A CN102416011A CN 102416011 A CN102416011 A CN 102416011A CN 2011103050329 A CN2011103050329 A CN 2011103050329A CN 201110305032 A CN201110305032 A CN 201110305032A CN 102416011 A CN102416011 A CN 102416011A
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Abstract
The invention relates to a medicine, in particular to broad-spectrum and high-efficiency antibacterial washing liquor and a preparation method thereof. The invention is characterized in that the antibacterial washing liquor is prepared by the following materials according to the weight ratio: 0.0001-2.0 of N-coconut-oil fatty-acid acyl L-arginine ethyl ester DL-pyrrolidone carboxylate, 0.0001-1.0 of dodecyl dimethyl benzyl ammonium chloride, 10.0-99.995 of water, and the balance of auxiliary materials. The broad-spectrum and high-efficiency antibacterial washing liquor has the following characteristics and advantages that pathogenic microorganisms are killed in a broad-spectrum and high-efficiency manner; ureaplasma urealytium, gonococcocci and trichomonas vaginalis can be killed in one minute; the killing rate for escherichia coli, staphylococcus aureus and candida albicans is respectively more than 99%; non-toxic; no stimulation is caused to the skin; no allergic reaction is caused; no stimulation is caused to the eyes; no stimulation is caused to vaginal mucosa; and the pH value of a preparation is close to that in the normal vagina.
Description
Technical field
The present invention relates to a kind of medicine, be specifically related to a kind of wide spectrum, anti-bacterial lotion and preparation method thereof efficiently.
Background technology
The high speed development of society has greatly improved people's living standard.It is healthy that the women more and more payes attention to the reproductive tract of oneself, usually with some care product cleaning reproductive tract.Reproductive tract infection also is women's frequently-occurring disease and a commonly encountered diseases, and the medicine of this type of disease of market treatment is a lot, and washing liquid is one type of preparation that comparison is accepted by numerous women.
Most of washing liquids in the market are bacteriostatic lotion, can not be real kill pathogenic microorganism, can only play the growth that suppresses pathogenic microorganism, its result of use is limited.In view of the acquired patent of my company (a kind of wide spectrum, microbicide efficiently; The patent No.: ZL 200710066058.6) technology, I can fast, efficiently kill pathogenic microorganism at this wide spectrum, the high-efficiency antimicrobial washing liquid of company's exploitation.So the development and the continuity of this patent acquired patent (patent No.: ZL 200710066058.6) that is company.
Summary of the invention
The purpose of this invention is to provide a kind of wide spectrum, efficient, stable anti-bacterial lotion.This anti-bacterial lotion is nontoxic, non-stimulated to skin, ametaboly is reacted, pH value non-stimulated to eyes, non-stimulated to vaginal mucosa, product is close with normal intravaginal pH value.It can efficiently kill gonococcus, trichomonal vaginitis, Ureaplasma urealyticum, pyococcus (like staphylococcus aureus), intestinal (like escherichia coli) and pathogenic fungus (like Candida albicans).Aspect stable, at least two years effect duration.
Another object of the present invention provides a kind of method for preparing anti-bacterial lotion.Anti-bacterial lotion by this method preparation is colourless, stable aqueous solution.This washing liquid can directly be used, and does not need dilution.
A purpose more of the present invention be with this anti-bacterial lotion process lotion, liniment is used to treat skin, membrane disease.
A purpose more of the present invention is that this anti-bacterial lotion is processed skin, mucosa disinfectant.
Anti-bacterial lotion of the present invention can also use separately can combine suitable instrumentation, like condom, contraceptive diaphragm, contraceptive membrane, sanitary towel or suitable delayed release device.
A purpose more of the present invention is the synthetic amino acid derivativges, particularly Oleum Cocois aminoacid pyrrolidone carboxylic acid salt that contains 10～14 carbochains.
Wide spectrum of the present invention, the purpose of anti-bacterial lotion is to realize through following technical scheme efficiently:
This anti-bacterial lotion is processed by following raw material by weight ratio:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
Its surplus is an adjuvant.
Described wide spectrum, anti-bacterial lotion efficiently is characterized in that can adding following one or more raw materials by weight ratio in this anti-bacterial lotion:
Myristyl dimethyl amine oxide: 0.001-3.0,
Sodium chloride: 0.0001-1.0,
Aloe gel: 0.0010-4.0,
Malic acid: 0.0001-0.1
Described wide spectrum, anti-bacterial lotion efficiently is characterized in that water wherein can use deionized water, distilled water or purified water, also can adopt glycerol, gelatin glycerol, ethanol, propylene glycol, Polyethylene Glycol, water and other solvent mixing by different proportion.
Said wide spectrum, anti-bacterial lotion efficiently, it is characterized in that wherein dodecyl dimethyl benzyl ammonium chloride can adopt with this prescription in compatible other surfactant such as betanin, Octoxinol, chlorhexidine, benzalkonium chloride, benzalkonium bromide or the two ten alkyl-dimethyl ammonium chlorides of each composition replace.
Said wide spectrum, anti-bacterial lotion efficiently, it is characterized in that wherein malic acid can adopt with this prescription in replacement such as compatible other regulator of each composition such as citric acid, tartaric acid, maleic acid.
Wide spectrum, the anti-bacterial lotion method for preparing comprises the following steps: efficiently
1.. take off by weight ratio and state raw material, at room temperature N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt and dodecyl dimethyl benzyl ammonium chloride are added in the deionized water, make homogeneous solution 30 ℃ of stirring and dissolving:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
2.. be filled in the suitable containers with the filling machine branch and get product.
Said wide spectrum, anti-bacterial lotion efficiently is characterized in that its preparation method comprises the following steps:
1.. take off by weight ratio and state raw material, at room temperature N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt and dodecyl dimethyl benzyl ammonium chloride are added in the deionized water, make homogeneous solution 30 ℃ of stirring and dissolving:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
2.. above-mentioned solution is being continued to keep 30 ℃ under the stirring, and adding following raw material by weight ratio:
Myristyl dimethyl amine oxide: 0.001-3.0,
Sodium chloride: 0.0001-1.0,
Malic acid: 0.0001-0.1
3.. continue to stir the decline temperature to room temperature, become the water white transparency aqueous solution;
4.. be filled in the suitable containers with the filling machine branch and get product.
Said wide spectrum, anti-bacterial lotion efficiently is characterized in that this anti-bacterial lotion can be made into different dosage forms, comprises lotion, liniment; This anti-bacterial lotion can be used for killing gonococcus, trichomonal vaginitis, Ureaplasma urealyticum, pyococcus (staphylococcus aureus), intestinal (escherichia coli), pathogenic fungus (Candida albicans).This anti-bacterial lotion can be used for vagina control women ' s genital tract infection disease; Be used for the sterilization of men and women's external genitalia, cleaning; Be used to treat skin, membrane disease; Be used for skin, mucomembranous surface sterilization; Be used for article, air sterillization.
The amino acid derivativges, particularly Oleum Cocois aminoacid pyrrolidone carboxylic acid salt of said wide spectrum, 10～14 carbochains containing in the anti-bacterial lotion prescription efficiently, structural formula is following:
A represented amino acid group in the formula, R represents C
10-C
14The coco-nut oil fatty acid group.In the structural formula, amino acid group can be arginine, lysine, histidine, high-lysine, or non-natural amino acid residue or other dipeptides that has cation group or tripeptides that has cation group.
Said wide spectrum, the synthesis step of the Oleum Cocois aminoacid pyrrolidone carboxylic acid salt in the anti-bacterial lotion is following efficiently:
1.. the preparation solution A: with the dimethyl furan is solution, mixes 1.2 parts of N, N '-two hexamethylene carbon imidodicarbonic diamide (Dicyclohexylcarbodiimide (DCC)) and 1 part of myristic acid (CH
3(CH
2)
10COOH), stirred 2 hours under the room temperature.Add and be dissolved in dichloromethane (CH
2Cl
2) in 1.2 parts of N-hydroxy succinic acid imines (Hydroxylsuccinimide (NHS)) (above-mentioned " part " is in molar ratio), continue to be stirred to and form deposition, this deposition is useless by-product carbamide bicyclohexane (Dicyclohexane urea).Remove by filter deposition, promptly get solution A.
2.. the preparation solution B: with the dimethyl furan is solvent, under 0 ℃ of condition, mixes and stirs 1 part of hydrochloric acid L-arginine ethyl ester and 1 part of sodium hydroxide 30 minutes, adds 1.3 parts of triethylamines (above-mentioned " part " is in molar ratio).Mix and be stirred to and become homogeneous solution.Be to be solution B.
3.. the preparation amino acid salts: at room temperature mixed solution A and solution B, stirred 2 hours.Vacuum is removed organic solvent, and the mixed liquor of water or water and ethane carries out recrystallization to product.Crystallization is dissolved in methanol, adds the sodium hydroxide of equivalent, the mixture of water, ethanol, ether extracts product, dry organic facies under the vacuum.Again product is dissolved in methanol, adds the DL-2-pyrrolidone-5-carboxylic acid of equal portions, stir, reaction is removed methanol and is promptly got end product after accomplishing under the vacuum.
The specific embodiment
Below in conjunction with instance the present invention is done further explanation.But the present invention is not limited to these embodiment.
1.N-the synthetic and preparation of coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt:
This amino acid derived system is got with the pyrrolidone carboxylic acid salt addition by aminoacid ethyl ester and coco-nut oil fatty acid acidylate (amino is arranged on the r-carbon bond of acyl group) again.Do not contain halogen family element (like chlorine and bromine) in this amino acid derivativges molecular structure.
Oleum Cocois aminoacid pyrrolidone carboxylic acid salt structural formula is following:
A represented amino acid group in the formula, R represents C
10-C
14The coco-nut oil fatty acid group.In the structural formula, amino acid group can be arginine, lysine, histidine, high-lysine, or non-natural amino acid residue or other dipeptides that has cation group or tripeptides that has cation group.
Oleum Cocois arginine pyrrolidone carboxylic acid salt can make according to the following steps:
1.. the preparation solution A: with the dimethyl furan is solution, mixes 1.2 parts of N, N '-two hexamethylene carbon imidodicarbonic diamide (Dicyclohexylcarbodiimide (DCC)) and 1 part of myristic acid (CH
3(CH
2)
10COOH), stirred 2 hours under the room temperature.Add and be dissolved in dichloromethane (CH
2Cl
2) in 1.2 parts of N-hydroxy succinic acid imines (Hydroxylsuccinimide (NHS)) (above-mentioned " part " is in molar ratio), continue to be stirred to and form deposition, this deposition is useless by-product carbamide bicyclohexane (Dicyclohexane urea).Remove by filter deposition, promptly get solution A.
2.. the preparation solution B: with the dimethyl furan is solvent, under 0 ℃ of condition, mixes and stirs 1 part of hydrochloric acid L-arginine ethyl ester and 1 part of sodium hydroxide 30 minutes, adds 1.3 parts of triethylamines (above-mentioned " part " is in molar ratio).Mix and be stirred to and become homogeneous solution.Be to be solution B.
3.. the preparation amino acid salts: at room temperature mixed solution A and solution B, stirred 2 hours.Vacuum is removed organic solvent, and the mixed liquor of water or water and ethane carries out recrystallization to product.Crystallization is dissolved in methanol, adds the sodium hydroxide of equivalent, the mixture of water, ethanol, ether extracts product, dry organic facies under the vacuum.Again product is dissolved in methanol, adds the DL-2-pyrrolidone-5-carboxylic acid of equal portions, stir, reaction is removed methanol and is promptly got end product after accomplishing under the vacuum.
Anti-bacterial lotion of the present invention is prepared with following raw materials according by weight ratio:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
Water wherein can be used deionized water, distilled water or purified water, also can adopt other solvent, like glycerol, gelatin glycerol, ethanol, propylene glycol, Polyethylene Glycol, water and other solvent mixing by different proportion.
In this prescription, also can add following one or more compositions by weight ratio:
Myristyl dimethyl amine oxide: 0.001-3.0,
Sodium chloride: 0.0001-1.0,
Malic acid: 0.0001-0.1.
Malic acid in the prescription can use with this prescription in other compatible acid of other composition, like citric acid, tartaric acid, maleic acid etc.
In this prescription, also can add one or more adjuvants.Like spice, pigment, flavour enhancer, emulsifying agent etc.
The method for preparing of anti-bacterial lotion of the present invention
The preparation of anti-bacterial lotion of the present invention comprises the steps:
1.. take off by weight ratio and state raw material,, make homogeneous solution at 30 ℃ with they mixings:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0,
Water: 10.0-99.995.
2.. if hope in this anti-bacterial lotion, to add myristyl dimethyl amine oxide and Aloe gel, only need take off the raw material of face by weight ratio, join in the said mixture, be in harmonious proportion and stir into colourless transparent liquid:
Myristyl dimethyl amine oxide: 0.001-3.0,
Sodium chloride: 0.00001-1.0,
Malic acid: 0.0001-0.1.
3.. being filled to the filling machine branch must finished product in the suitable containers.
The application of anti-bacterial lotion of the present invention
Anti-bacterial lotion of the present invention is mainly used in intravaginal and prevents and treats sexually transmitted disease (STD), control women ' s genital tract infection disease.This anti-bacterial lotion also can be made into appropriate formulation and is used to treat skin, membrane disease, sterilization skin, mucosa, air or article.This anti-bacterial lotion also can combine suitable apparatus, uses like condom, contraceptive diaphragm, contraceptive membrane, sanitary towel or delayed release device.
The present invention has following characteristics and advantage:
1.. wide spectrum, kill pathogenic microorganism efficiently.Killed " Ureaplasma urealyticum ", " gonococcus ", " trichomonal vaginitis " in 1 minute; The killing rate that " escherichia coli ", " staphylococcus aureus " are reached " Candida albicans " is all greater than 99%.
2.. nontoxic; Non-stimulated to skin; The ametaboly reaction; Non-stimulated to eyes; Non-stimulated to vaginal mucosa; The pH value of preparation is with normal intravaginal close.
The preparation of embodiment 1. anti-bacterial lotions of the present invention
1. the raw material and the weight proportion thereof of 36 prescriptions have been listed in the table 1.Each prescription is got its raw material respectively by weight ratio, make homogeneous solution or water white transparency water solublity by above-mentioned method for preparing.
The raw material and the weight proportion (kg) of table 1. prescription
Annotate: NaCl=sodium chloride; The C1=myristyl dimethyl amine oxide; DH
2O=deionized water, distilled water or purified water; C3=N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt; The M1=dodecyl dimethyl benzyl ammonium chloride; The MA=malic acid.
1 be the compound method that example further specifies this anti-bacterial lotion solution to fill a prescription below:
1.. with 0.1Kg N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt, 0.1Kg dodecyl dimethyl benzyl ammonium chloride 30 ℃ be in harmonious proportion with the 99.28Kg deionized water and stir water white homogeneous solution.
2.. keep 30 ℃ of adding 0.05Kg sodium chloride, 0.4Kg myristyl dimethyl amine oxide, 0.07Kg malic acids to make it abundant dissolving.
3.. being filled to the filling machine branch must finished product in the suitable containers.
The effectiveness that embodiment 2. anti-bacterial lotions of the present invention are killed Ureaplasma urealyticum detects
1.. main material
A. test strain: Ureaplasma urealyticum (Ureaplasma Urealyticum) the international standard strain of going down to posterity;
B. culture medium: high-efficiency mycoplasma fluid medium;
C. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Test foundation: method and operation sequence in Ministry of Public Health " disinfection technology standard " (version in the 2002) second portion " experiment of disinfectant microbicidel ", the pathophorous laboratory diagnosis of associativity (calendar year 2001) chapter 13, four.
Method of testing: carry out according to job instruction NCSTD-JX15-2008 specified standard operation sequence.
Experimental temperature: 25 ℃～28 ℃.
3.. test result
Table 8. test specimen is to the killing action of Ureaplasma urealyticum
Annotate :+: the Ureaplasma urealyticum growth is arranged;-: no Ureaplasma urealyticum growth.
4.. test result
Testing result shows: final concentration is test specimen and the effect of Ureaplasma urealyticum suspension 1 minute of 200 times of dilutions (embodiment 1: prescription 4), can kill Ureaplasma urealyticum.
Embodiment 3. anti-bacterial lotions of the present invention are killed gonococcal effectiveness and are detected
1.. main material
A. the reference culture G that provides of test strain: WHO;
B. culture medium: 10% blood plate;
C. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Test basis: press method and operation sequence in Ministry of Public Health " disinfection technology standard " (version in the 2002) second portion " experiment of disinfectant microbicidel ".
The method of inspection: carry out according to job instruction NCSTD-JX03-2008 specified standard operation sequence.
Experimental temperature: 25 ℃～28 ℃.
3.. test result
Table 9. test specimen is to gonococcal killing action
Annotate :+: see the gonococcus growth;-: do not see the gonococcus growth.
4.. test result
Testing result shows:
Final concentration is that (embodiment 1: prescription 3) test specimen and the effect of gonococcus suspension can be killed gonococcus in 1 minute in 200 times of dilutions.
Final concentration is that (embodiment 1: prescription 4) test specimen and the effect of gonococcus suspension can be killed gonococcus in 1 minute in 200 times of dilutions.
The effectiveness that embodiment 4. anti-bacterial lotions of the present invention are killed trichomonal vaginitis detects
1.. main material
A. test strain: trichomonal vaginitis clinical strain;
B. culture medium: liver infusion culture medium;
C. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Experimental basis: method and operation sequence in Ministry of Public Health " disinfection technology standard " (version in the 2002) second portion " experiment of disinfectant microbicidel " make an experiment in conjunction with the trichomonal vaginitis characteristics.Laboratory temperature: 20 ℃～25 ℃.
Experimental technique: carry out according to job instruction NCSTD-JX17-2008 specified standard operation sequence.
3.. test result
Table 10. test specimen is to the killing effect of trichomonal vaginitis
Annotate :+: represent to have survival infusorian and vigor better;-: expression does not have the survival infusorian, and the polypide fragment is arranged.
4.. test result
Testing result shows: final concentration is that (embodiment 1: prescription 2) test specimen and trichomonal vaginitis effect can be killed trichomonal vaginitis in 1 minute in 50 times of dilutions.
The effectiveness of embodiment 5. anti-bacterial lotion deactivation staphylococcus aureuses of the present invention detects
1.. main material
A. test strain: staphylococcus aureus-ATCC6538 (the 5th～6 generation);
B. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) and GB15981-1995 " evaluation methodology and the standard of sterilization and sterilization effect " carry out.Laboratory temperature: 20 ± 1 ℃.
3.. test result
Table 12. test specimen is to the bactericidal action of staphylococcus aureus
4.. test result
Test specimen was to staphylococcus aureus effect 2 minutes, and average bactericidal rate is 100.00%, and sample has bactericidal action to this bacterium.
The effectiveness of embodiment 6. anti-bacterial lotion deactivation Candida albicans of the present invention detects
1.. main material
Test strain: Candida albicans-ATCCl0231,5-6 generation;
Test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) and GB15981-1995 " evaluation methodology and the standard of sterilization and sterilization effect " carry out.Laboratory temperature: 20 ± 1 ℃.
3.. test result
Table 13. test specimen is to the oidiomycetic bactericidal action of white
4.. test result
Test specimen was to Candida albicans effect 2 minutes, and average bactericidal rate is 97.49%.Act on 5 minutes, average bactericidal rate is 99.95%, and sample has bactericidal action to this bacterium.
The effectiveness of embodiment 7. anti-bacterial lotion colibacillus deactivatings of the present invention detects
1.. main material
Test strain: 5～6 generations of escherichia coli-8099, the;
Test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) and GB15981-1995 " evaluation methodology and the standard of sterilization and sterilization effect " carry out.Laboratory temperature: 20 ± 1 ℃.
3.. test result
Table 14. test specimen is to colibacillary bactericidal action
4.. test result
Test specimen was to escherichia coli effect 2 minutes, and average bactericidal rate is 100%, and sample has bactericidal action to this bacterium.
Embodiment 8. anti-bacterial lotions of the present invention are to the irritation test of vaginal mucosa
1.. main material
Experimental animal: 6 of female New Zealand large ear rabbits.
Test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) vaginal mucosa irritant test.Test is established and is tried thing group and negative control group, every group of 3 animals.Experimental situation temperature: 20 ℃～22 ℃.
3.. test result
Histopathological examination sees the following form.
The scoring of table 15. test specimen vaginal mucosa IR
Annotate: average integral=IR integration addition is divided by observing sum (observing sum=number of animals * 3).
SI equals the test group average integral and subtracts the matched group average integral.This sample stimulus index is-0.4.
4.. test result
Under this experimental condition, test specimen is-0.4 to the SI of White Rabbit vaginal mucosa, is classified as nonirritant by vaginal mucosa stimulus intensity grade scale.
The skin allergic reaction test of embodiment 9. anti-bacterial lotions of the present invention
1.. main material
Experimental animal: totally 48 of regular grade Cavia porcelluss (female, hero half and half);
Test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
The test of Ministry of Public Health " disinfection technology standard " (version in 2002) skin allergic reaction.Experiment is established three groups altogether: tried thing group, negative control group and positive controls.Experimental situation temperature: 21 ℃～24 ℃.
3.. test result
Table 16. test specimen is to the allergy result of the test of guinea pig skin
4.. test result
Under this experimental condition, test specimen is tested animal subject guinea pig skin allergy and is not seen skin allergic reaction.
The skin irritation test of embodiment 10. anti-bacterial lotions of the present invention
1.. main material
A. experimental animal: 4 of regular grade new zealand white rabbits;
B. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
The test of Ministry of Public Health " disinfection technology standard " (version in 2002) skin irritation.The experimental situation temperature: 22 ℃～24 ℃, relative humidity: 54%～66%.
3.. test result
Table 17. test specimen is to White Rabbit one whole skin irritation test reaction scoring
4.. test result
Under this experiment condition, test is a nonirritant by skin irritation strength grading standard determination to test specimen to animal subject White Rabbit one whole skin irritation.
The acute eye irritation test of embodiment 11. anti-bacterial lotions of the present invention
1.. main material
A. experimental animal: 4 of new zealand white rabbits;
B. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) acute eye irritation test method.The experimental situation temperature: 18 ℃～22 ℃, relative humidity: 48%～50%.
3.. test result
Table 18. test specimen is to White Rabbit acute eye irritation test result
4.. test result
Under this experiment condition, scoring is judged to be nonirritant by grade scale to test specimen to animal subject White Rabbit acute eye irritation test result.
The acute oral toxicity test of embodiment 12. anti-bacterial lotions of the present invention
1.. main material
A. experimental animal: totally 20 of SPF level Kunming kind white mice (female, male half and half);
B. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 5) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) acute oral toxicity test.Experimental enviroment condition: 20 ℃～23 ℃ of temperature, relative humidity 50%～70%.
3.. test result
Animal subject is at viewing duration, and no abnormality seen shows, and body weight gain is normal, occurs dead.Pathological change is not seen in all animal gross anatomies.
Table 19. test specimen chmice acute per os toxicity test result
4.. test result
Under this experiment condition, test specimen is to animal subject white mice acute oral toxicity test median lethal dose(LD 50) LD
50Greater than 5000mg/kg.bw, estimate the nontoxic level in true border according to the per os acute toxicity grading criteria.
The pH value of embodiment 13. anti-bacterial lotions of the present invention is measured
1.. main material
A. instrument and equipment: Seven Multi type pH/ electrical conductivity/ion comprehensive tester.
B. proofread and correct and use standard solution:
A. Potassium Hydrogen Phthalate standard buffer solution (20 ℃ of pH 4.00),
B. mixed phosphate standard buffer solution (20 ℃ of pH 6.88),
C. Borax standard buffer solution (20 ℃, pH 9.23);
C. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (2002 editions) 2.2 sterile products physical and chemical inspection technical specifications.Test atmosphere: room temperature: 16 ℃, relative humidity: 42%.
3.. test result
The pH value meansigma methods of the test specimen stock solution of this mensuration is 4.39, sample determination 2 times, and the result sees the following form.
The pH value of table 20. test specimen is measured the result
4.. test result
Through detecting, the pH meansigma methods of test specimen is 4.39.
The stability test of embodiment 14. anti-bacterial lotions of the present invention
1.. main material
A. bacterial strain: Candida albicans-ATCC10231 (the 5th～6 generation);
B. test specimen: the anti-bacterial lotion of pressing embodiment 1 (prescription 1) preparation.
2.. test foundation and method
Ministry of Public Health " disinfection technology standard " (version in 2002) and GB15981-1995 " evaluation methodology and the standard of sterilization and sterilization effect " carry out.Experimental enviroment condition: 20 ± 1 ℃ of temperature.
3.. test result
Under 20 ± 1 ℃ of conditions, three times the repeated trials result shows: constant-temperature enclosed preservation is after 90 days under 37 ℃ of conditions for test specimen, and to Candida albicans effect 10 minutes, average bactericidal rate was 99.99%, and the result sees table 16:
Table 21. insulation before and after test sample is to the oidiomycetic bactericidal action of white
4.. test result
Constant-temperature enclosed preservation is after 90 days under 37 ℃ of conditions for test specimen, and to Candida albicans effect 10 minutes, average bactericidal rate was 99.99%.The bactericidal action of this product at room temperature can keep 2 years at least.
Claims (10)
1. a wide spectrum, anti-bacterial lotion efficiently is characterized in that this anti-bacterial lotion processed by following raw material by weight ratio:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
Its surplus is an adjuvant.
2. wide spectrum according to claim 1, anti-bacterial lotion efficiently is characterized in that can adding following one or more raw materials by weight ratio in this anti-bacterial lotion:
Myristyl dimethyl amine oxide: 0.001-3.0,
Sodium chloride: 0.0001-1.0,
Aloe gel: 0.0010-4.0,
Malic acid: 0.0001-0.1.
3. wide spectrum according to claim 1, anti-bacterial lotion efficiently; It is characterized in that water wherein can use deionized water, distilled water or purified water, also can adopt glycerol, gelatin glycerol, ethanol, propylene glycol, Polyethylene Glycol, water and other solvent mixing by different proportion.
4. wide spectrum according to claim 1, anti-bacterial lotion efficiently, it is characterized in that wherein dodecyl dimethyl benzyl ammonium chloride can adopt with this prescription in compatible other surfactant such as betanin, Octoxinol, chlorhexidine, benzalkonium chloride, benzalkonium bromide or the two ten alkyl-dimethyl ammonium chlorides of each composition replace.
5. according to claim 1 and 2 described wide spectrums, anti-bacterial lotion efficiently, it is characterized in that wherein malic acid can adopt with this prescription in replacements such as compatible other regulator of each composition such as citric acid, tartaric acid, maleic acid.
6. wide spectrum according to claim 1, anti-bacterial lotion efficiently is characterized in that its preparation method comprises the following steps:
1.. take off by weight ratio and state raw material, at room temperature N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt and dodecyl dimethyl benzyl ammonium chloride are added in the deionized water, make homogeneous solution 30 ℃ of stirring and dissolving:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
2.. be filled in the suitable containers with the filling machine branch and get product.
7. wide spectrum according to claim 2, anti-bacterial lotion efficiently is characterized in that its preparation method comprises the following steps:
1.. take off by weight ratio and state raw material, at room temperature N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt and dodecyl dimethyl benzyl ammonium chloride are added in the deionized water, make homogeneous solution 30 ℃ of stirring and dissolving:
N-coco-nut oil fatty acid acyl group L-arginine ethyl ester DL-pyrrolidone carboxylic acid salt: 0.0001-2.0,
Dodecyl dimethyl benzyl ammonium chloride: 0.0001-1.0
Water: 10.0-99.995,
2.. above-mentioned solution is being continued to keep 30 ℃ under the stirring, and adding following raw material by weight ratio:
Myristyl dimethyl amine oxide: 0.001-3.0,
Sodium chloride: 0.0001-1.0,
Malic acid: 0.0001-0.1
3.. continue to stir the decline temperature to room temperature, become the water white transparency aqueous solution;
4.. be filled in the suitable containers with the filling machine branch and get product.
8. wide spectrum according to claim 1 and 2, anti-bacterial lotion efficiently is characterized in that this anti-bacterial lotion can be made into different dosage forms, comprises lotion, liniment; This anti-bacterial lotion can be used for killing gonococcus, trichomonal vaginitis, Ureaplasma urealyticum, pyococcus (staphylococcus aureus), intestinal (escherichia coli), pathogenic fungus (Candida albicans).This anti-bacterial lotion can be used for vagina control women ' s genital tract infection disease; Be used for the sterilization of men and women's external genitalia, cleaning; Be used to treat skin, membrane disease; Be used for skin, mucomembranous surface sterilization; Be used for article, air sterillization.
9. according to the amino acid derivativges, particularly Oleum Cocois aminoacid pyrrolidone carboxylic acid salt of the said wide spectrum of claim 1,10～14 carbochains containing in the anti-bacterial lotion prescription efficiently, structural formula is following:
A represented amino acid group in the formula, R represents C
10-C
14The coco-nut oil fatty acid group.In the structural formula, amino acid group can be arginine, lysine, histidine, high-lysine, or non-natural amino acid residue or other dipeptides that has cation group or tripeptides that has cation group.
10. wide spectrum according to claim 11, the synthesis step of the Oleum Cocois aminoacid pyrrolidone carboxylic acid salt in the anti-bacterial lotion is following efficiently:
1.. the preparation solution A: with the dimethyl furan is solution, mixes 1.2 parts of N, N '-two hexamethylene carbon imidodicarbonic diamide (Dicyclohexylcarbodiimide (DCC)) and 1 part of myristic acid (CH
3(CH
2)
10COOH), stirred 2 hours under the room temperature.Add and be dissolved in dichloromethane (CH
2Cl
2) in 1.2 parts of N-hydroxy succinic acid imines (Hydroxylsuccinimide (NHS)) (above-mentioned " part " is in molar ratio), continue to be stirred to and form deposition, this deposition is useless by-product carbamide bicyclohexane (Dicyclohexane urea).Remove by filter deposition, promptly get solution A.
2.. the preparation solution B: with the dimethyl furan is solvent, under 0 ℃ of condition, mixes and stirs 1 part of hydrochloric acid L-arginine ethyl ester and 1 part of sodium hydroxide 30 minutes, adds 1.3 parts of triethylamines (above-mentioned " part " is in molar ratio).Mix and be stirred to and become homogeneous solution.Be to be solution B.
3.. the preparation amino acid salts: at room temperature mixed solution A and solution B, stirred 2 hours.Vacuum is removed organic solvent, and the mixed liquor of water or water and ethane carries out recrystallization to product.Crystallization is dissolved in methanol, adds the sodium hydroxide of equivalent, the mixture of water, ethanol, ether extracts product, dry organic facies under the vacuum.Again product is dissolved in methanol, adds the DL-2-pyrrolidone-5-carboxylic acid of equal portions, stir, reaction is removed methanol and is promptly got end product after accomplishing under the vacuum.
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| CN108244138A (en) * | 2018-01-17 | 2018-07-06 | 上海化工研究院有限公司 | A kind of anti-mildew dose of antibiotic waste residue and preparation method thereof |
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| CN108619006A (en) * | 2017-03-24 | 2018-10-09 | 株式会社漫丹 | Two-layer hair cosmetics |
| CN108619006B (en) * | 2017-03-24 | 2021-05-07 | 株式会社漫丹 | Two-layer hair cosmetic |
| CN108244138A (en) * | 2018-01-17 | 2018-07-06 | 上海化工研究院有限公司 | A kind of anti-mildew dose of antibiotic waste residue and preparation method thereof |
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| CN109704625A (en) * | 2018-12-19 | 2019-05-03 | 贵州科之杰新材料有限公司 | A kind of concrete admixture preservative and preparation method thereof |
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| CN112220728A (en) * | 2020-11-12 | 2021-01-15 | 河南美凝生物科技有限公司 | Gynecological cleaning fluid with antibacterial and prebiotics maintenance functions and preparation method thereof |
| CN113398057A (en) * | 2020-12-22 | 2021-09-17 | 重庆中佳信健康管理有限公司 | Bacteriostatic agent and preparation method thereof |
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