CN102600206A - Nano composite skin disinfection lotion and preparation method thereof - Google Patents
Nano composite skin disinfection lotion and preparation method thereof Download PDFInfo
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- CN102600206A CN102600206A CN2012100569460A CN201210056946A CN102600206A CN 102600206 A CN102600206 A CN 102600206A CN 2012100569460 A CN2012100569460 A CN 2012100569460A CN 201210056946 A CN201210056946 A CN 201210056946A CN 102600206 A CN102600206 A CN 102600206A
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Abstract
The invention discloses nano composite skin disinfection lotion and a preparation method thereof. The skin disinfection lotion comprises chlorhexidine acetate, zinc oxide, edetic acid, emulsifying agent and water. The emulsifying agent consists of vegetable oil, tri-n-butyl phosphate and triton x-100. The total volume ratio of the vegetable oil to the tri-butyl-phosphate to the triton x-100 is 2-8:1:1; the concentration of the chlorhexidine acetate is 0.5-3g/L, the concentration of the zinc oxide is 0.01-0.5g/L, the grain size is 50-100nm, and the concentration of the edetic acid is 0.01-0.2g/L. The nano composite skin disinfection lotion has the advantages of wide antibacterial spectrum of inorganic antibacterial agent, fine persistence and heat resistance, difficulty in drug resistance and the like, can achieve a prefect skin disinfection effect, and has an important application value.
Description
Technical field
The present invention relates to a kind of nano combined skin degerming emulsion and preparation method thereof.
Background technology
Skin and mucosa are that human body is resisted effective barrier that the profit tissue is invaded in microorganism, but on its surface abundant microorganism are arranged.In daily life, through adversary and Mucocutaneous sterilization, can prevent the infection of infectious intestinal disease, skin pyesis and genitourinary system; In health system, carrying out skin degerming is the important leverage of modern medical service, also is one of most important, the most simple and easy to do measure of control hospital infection.Skin and mucous membrane disinfection agent kind commonly used at present is numerous, but defective is more or less all arranged, like the quaternary ammonium salt narrow antimicrobial spectrum, a little less than the sterilizing ability; Ethanol is big to skin and mucous membrane irritation property; The povidone iodine bactericidal effect persistent period is shorter; The chlorhexidine acetate class is prone to produce Resistant strain.The tradition disinfectant is difficult to meet fully the needs of clinical each medical personnel of section hand disinfection, thereby causes cross infection.Therefore, need find new kind, novel form or new compound prescription, to reach ideal skin degerming effect.
Summary of the invention
The purpose of this invention is to provide a kind of nano combined skin degerming emulsion and preparation method thereof.
Nano combined skin degerming emulsion provided by the invention comprises chlorhexidine acetate, zinc oxide, ethylenediaminetetraacetic acid, emulsifying agent and water.
Above-mentioned sterilization emulsion also can only be made up of said components.Wherein, said emulsifying agent is made up of vegetable oil, three normal-butyl phosphate and TritonX x-100; Said vegetable oil is 2-8 with the cumulative volume ratio of three normal-butyl phosphate and TritonX x-100: 1: 1, and preferred 8: 1: 1; Said vegetable oil is at least a in soybean oil, the Oleum Arachidis hypogaeae semen, preferred soybean oil.
The concentration of said chlorhexidine acetate in said sterilization emulsion is 0.5～3g/L, preferred 2g/L;
Said oxidation zinc concentration is 0.01～0.5g/L, preferred 0.1g/L; Particle diameter is 50-100nm;
The concentration of said ethylenediaminetetraacetic acid in said sterilization emulsion is 0.01～0.2g/L, preferred 0.1g/L;
In this sterilization emulsion, oil phase comprises emulsifying agent vegetable oil and organic solvent three normal-butyl phosphate and TritonX x-100, and water is made up of chlorhexidine acetate aqueous solution, edta solution and zinc oxide.Said emulsifying agent accounts for the 10-20% of said sterilization emulsion cumulative volume, preferred 10%.
In the said nano combined skin degerming emulsion, the diameter of drop is 10-30nm.
The method of the above-mentioned sterilization emulsion of preparation provided by the invention comprises the steps: to obtain said sterilization emulsion with carrying out emulsifying after aforementioned each component mixing.
In the said homogenizing step, temperature is a room temperature, and pressure is 25～35Mpa.
The disinfectant liquid for skin that it is active component that the application of the nano combined skin degerming emulsion that the invention described above provides in skin degerming or preparation skin antiseptic reaches with this nano combined skin degerming emulsion also belongs to protection scope of the present invention.
Wherein, said skin antiseptic or disinfectant liquid for skin all are staphylococcus aureus, escherichia coli and Candida albicans of killing skin surface.
The present invention is with traditional skin antiseptic chlorhexidine acetate and nano zine oxide compatibility; And adding synergist ethylenediaminetetraacetic acid; It is good both to have brought into play organic type of antibacterial bactericidal effect; Fireballing characteristics can make again that prescription obtains that inorganic antiseptic has a broad antifungal spectrum, lasting effect are good, good heat resistance, being difficult for producing characteristics such as drug resistance, reach ideal skin degerming effect.Adopt the inventive method, above-mentioned prescription through the high pressure homogenize emulsion process, is utilized comprehensive effects such as liquid decompression, expansion, blast under the condition of high voltage; Liquid component is fully reacted, and the emulsion that obtains not only is uniformly dispersed, and is not stratified; And obtain than fine grained, reach emulsifying effectiveness preferably.Therefore, this prescription still has bactericidal property preferably when reducing chlorhexidine acetate.This prescription does not contain alcohols, and to mucocutaneous nontoxic non-stimulated, safety in utilization is better.Emulsion liquid not only makes prescription have good surface appearance, has also increased its stability.Experiment showed, that (1) emulsion of the present invention kills 90% staphylococcus aureus and only need 0.80 minute, escherichia coli need 0.78min, and Candida albicans needs 0.99min; To staphylococcus aureus, escherichia coli, Candida albicans effect 3min, average kill ratio is all greater than 99.9%.(2) simulated field experiment shows, nano combined skin degerming emulsion is significantly higher than the simple chlorhexidine acetate aqueous solution with same amount to the suppression ratio of the 6h of natural bacteria, 12h, 24h.(3) the on-the-spot disinfection experiment result of skin shows that this emulsion is 94.09% to experimenter's hand effect 2min to the natural bacteria average kill ratio.(4) the high temperature accelerated test shows, this emulsion 54 ℃ deposit 14d after the active constituent content rate of descent be 2.02%, have good stable property.(5) toxicity test shows that this emulsion can use safely on human body skin, mucosa, and environment and human body are not had harm and stimulation.
Description of drawings
Fig. 1 is transmission electron microscope (Philips, TECNAI10) photo of the nano combined skin degerming emulsion of embodiment 1 preparation gained.
Fig. 2 is the AFM photo of the nano combined skin degerming emulsion of embodiment 1 preparation gained.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, but the present invention is not limited to following examples.Said method is conventional method if no special instructions.Said material all can get from open commercial sources if no special instructions.
Antibacterial of adopting among the present invention or bacteriostatic functional component are chlorhexidine acetate and zinc oxide.In traditional skin antiseptic, chlorhexidine acetate has characteristics (Doebbeling BN, Stanley GL such as bactericidal effect is good, toxicity is low, zest is little, has a broad antifungal spectrum; Sheetz C T; Et al.Comparative efficiency of alternative hand-washing agents in reducing nosocomial infections in intensive care units [J] .New English Journal of Medicine.1992,11,327 (19): 1390-91); But found the appearance (Fei Chunnan of its Resistant strain in recent years; Liu Jun, Shen Peng etc. the nosocomial infection cause of disease is to the chemical sproof progress of common disinfectant. environment and health magazine, 2007; 12,24 (12)).Ethylenediaminetetraacetic acid can be strengthened the effect of many antibiotic substance to gram negative bacteria, has report that ethylenediaminetetraacetic acid and liquor hibitane Combined application can be strengthened its bactericidal effect to bacillus pyocyaneus, staphylococcus epidermidis, serratia marcesens, Aspergillus fumigatus, Candida albicans.
Compare with nano materials such as titanium oxide, silicon dioxide silver ion complex, nano zine oxide has good antibacterial performance and chemical compatibility.Its antibiotic mechanism is mainly: (1) ZnOw and granule reach nanoscale, thereby have special skin effect and high oxidation activity that nano material possesses; (2) zinc oxide is a kind of semi-conducting material, wherein has a large amount of elemental oxygens to discharge; (3) the formed network structure of unique four needle-likes of ZnOw is that antibiotic ion provides the high efficiency of transmission path; When electronegative antibacterial touches the arbitrary position of network, owing to the positive and negative charge captivation, a large amount of zinc ioies are come so that the speed of electric current is mobile; The penetration cell wall; Destroy synthetic (Zuowan Zhou, Shikai Liu, Lixia Gu.Studies on the strength and wear resistance of tetratod-shaped ZnO whisker-reinforced rubber composites. [J] the Applied Polymer Science of thalline internal protein; 2001,80:1520-24).
The present invention is a kind of disinfectant with chlorhexidine acetate, nano zine oxide and the compound use of synergist ethylenediaminetetraacetic acid, and forms a kind of oil-in-water Emulsion structure.The toxicity of considering disinfectant should be controlled at zone of reasonableness; The highest 3g/L that is limited to of chlorhexidine acetate that the present invention uses, zinc oxide is controlled at 0.5g/L, and ethylenediaminetetraacetic acid is controlled at 0.2g/L; The three has synergistic function, has good sterilizing function.
The present invention also provides the preparation technology of a kind of chlorhexidine acetate and nano zine oxide composite skin sterilization emulsion.This method adopts the high pressure homogenize mixing method; Compare with magnetic force mixing method and hypervelocity cutting machine mixing method, stirring, shearing, high-speed impact effect are not only arranged, also utilize comprehensive effects such as liquid decompression, expansion, blast under the condition of high voltage; Liquid is fully reacted, reach better emulsifying effectiveness.The emulsion that adopts this method to obtain not only is uniformly dispersed, and is not stratified, and it is thinner to obtain granule.Concrete steps are: take by weighing a certain amount of chlorhexidine acetate, ethylenediaminetetraacetic acid adds respectively and fills in the beaker of distilled water, put agitator heat (60～70 ℃) stir, to dissolving fully.Under the room temperature condition, the speed of the edta solution after the dissolving by 1～2ml/min is slowly added in the chlorhexidine acetate solution, the limit edged stirs, and notes not producing white casse.Suction pipe is drawn a certain amount of compound emulsifying agent and is added in the above-mentioned mixed solution, stirs.Take by weighing a certain amount of nano zine oxide in proportion, add in the mixed solution, after putting agitator and stirring, form through high pressure homogenizer emulsifying.In the preparation process, wherein the optimal proportion volume ratio scope of emulsifying agent and organic solution is 4: 1～1: 1 in the oil phase, and the optimum volume ratio scope of water and oil phase is 10: 1～5: 1.
Embodiment 1,
With the 0.05g chlorhexidine acetate, the 0.001g ethylenediaminetetraacetic acid adds respectively in the beaker that fills 20～30ml distilled water, put agitator heat (60～70 ℃) stir, to dissolving fully.Edta solution after the dissolving is slowly added in the chlorhexidine acetate solution, and the limit edged stirs, and notes not producing white casse.Suction pipe is drawn 15ml compound emulsifying agent (containing soybean oil 9ml, three normal-butyl phosphate 3ml, TritonX x-1003ml) and is added in the above-mentioned mixed solution, stirs.Take by weighing 0.05g in proportion, particle diameter is the nano zine oxide of 50～100nm; Add in the mixed solution; After solution supplied the rearmounted agitator of 100ml and stir, at room temperature, emulsifying formed the opaque emulsion of milky under 25～35Mpa operating pressure condition through high pressure homogenizer.
Final concentration is in each component of sterilization emulsion of preparing by mentioned component and method: chlorhexidine acetate 0.5g/L, ethylenediaminetetraacetic acid 0.01g/L, nano zine oxide 0.5g/L, emulsifying agent account for 15% of this sterilization emulsion cumulative volume.Fig. 1 prepares transmission electron microscope (Philips, TECNAI10) photo of the nano combined skin degerming emulsion of gained for this embodiment.Can know that by figure the diameter of drop is 10～30nm in this emulsion, has reached Nano grade.Fig. 2 prepares the AFM photo of the nano combined skin degerming emulsion of gained for this embodiment.Can know that by figure the particle diameter of nano zine oxide is 50～100nm in this emulsion.
Embodiment 2,
With the 0.2g chlorhexidine acetate, the 0.01g ethylenediaminetetraacetic acid adds respectively in the beaker that fills 20～30ml distilled water, put agitator heat (60～70 ℃) stir, to dissolving fully.Edta solution after the dissolving is slowly added in the chlorhexidine acetate solution, and the limit edged stirs, and notes not producing white casse.Suction pipe is drawn 10ml compound emulsifying agent (containing soybean oil 8ml, three normal-butyl phosphate 1ml, TritonX x-1001ml) and is added in the above-mentioned mixed solution, stirs.Take by weighing 0.01g in proportion, particle diameter is the nano zine oxide of 50-100nm; Add in the mixed solution; After solution supplied the rearmounted agitator of 100ml and stir, at room temperature, emulsifying formed the opaque emulsion of milky under 25～35Mpa operating pressure condition through high pressure homogenizer.
Each component final concentration of sterilization emulsion of preparing by mentioned component and method is chlorhexidine acetate 2g/L, and ethylenediaminetetraacetic acid 0.1g/L, nano zine oxide 0.1g/L, emulsifying agent account for 10% of this sterilization emulsion cumulative volume.This embodiment prepares the transmission electron microscope of the nano combined skin degerming emulsion of gained, and (Philips, TECNAI10) photo and AFM photo and Fig. 1 and Fig. 2 do not have substantive difference, here Ao Shu no longer.Can know that by figure the diameter of drop is 10～30nm in this emulsion, has reached Nano grade.
Embodiment 3,
With the 0.3g chlorhexidine acetate, the 0.02g ethylenediaminetetraacetic acid adds respectively in the beaker that fills 20～30ml distilled water, put agitator heat (60～70 ℃) stir, to dissolving fully.Edta solution after the dissolving is slowly added in the chlorhexidine acetate solution, and the limit edged stirs, and notes not producing white casse.Suction pipe is drawn 20ml compound emulsifying agent (containing soybean oil 10ml, three normal-butyl phosphate 5ml, TritonX x-1005ml) and is added in the above-mentioned mixed solution, stirs.Take by weighing 0.001g in proportion, particle diameter is the nano zine oxide of 50-100nm; Add in the mixed solution; After solution supplied the rearmounted agitator of 100ml and stir, form the opaque emulsion of milky through high pressure homogenizer emulsifying under room temperature, 25～35Mpa operating pressure condition.
In this example sterilization emulsion in each component concentration be chlorhexidine acetate 3g/L, ethylenediaminetetraacetic acid 0.2g/L, nano zine oxide 0.01g/L, emulsifying agent account for 20% of this sterilization emulsion cumulative volume.This embodiment prepares the transmission electron microscope of the nano combined skin degerming emulsion of gained, and (Philips, TECNAI10) photo and AFM photo and Fig. 1 and Fig. 2 do not have substantive difference, here Ao Shu no longer.Can know that by figure the diameter of drop is 30nm in this emulsion, has reached Nano grade.
Embodiment 4,
With the 0.19g chlorhexidine acetate, the 0.02g ethylenediaminetetraacetic acid adds respectively in the beaker that fills 20～30ml distilled water, put agitator heat (60～70 ℃) stir, to dissolving fully.Edta solution after the dissolving is slowly added in the chlorhexidine acetate solution, and the limit edged stirs, and notes not producing white casse.Suction pipe is drawn 20ml compound emulsifying agent (containing soybean oil 10ml, three normal-butyl phosphate 5ml, TritonX x-1005ml) and is added in the above-mentioned mixed solution, stirs.Take by weighing 0.05g in proportion, particle diameter is the nano zine oxide of 50-100nm; Add in the mixed solution; After solution supplied the rearmounted agitator of 100ml and stir, at room temperature, emulsifying formed the opaque emulsion of milky under 25～35Mpa operating pressure condition through high pressure homogenizer.
In this example sterilization emulsion in each component concentration be: chlorhexidine acetate 1.9g/L, ethylenediaminetetraacetic acid 0.2g/L, nano zine oxide 0.5g/L, emulsifying agent account for 20% of this sterilization emulsion cumulative volume.This embodiment prepares the transmission electron microscope of the nano combined skin degerming emulsion of gained, and (Philips, TECNAI10) photo and AFM photo and Fig. 1 and Fig. 2 do not have substantive difference, here Ao Shu no longer.Can know that by figure the diameter of drop is 30nm in this emulsion, has reached Nano grade.
Through test, the sterilization emulsion that the foregoing description 1-4 prepares gained all satisfies following physicochemical character:
Outward appearance: milky is opaque
PH value: 7.68
Particle diameter under the Electronic Speculum (nm): 10～30nm
Stability: adopt the high temperature accelerated test, this emulsion is placed 14 days bactericidal active ingredient rate of descent≤10% at 54 ℃ of calorstats, has good stable property.
The BA of above-mentioned nano combined skin degerming emulsion provided by the invention (test is all carried out with reference to " disinfection technology standard ") as follows; The gained result is the meansigma methods that above-mentioned 4 embodiment prepare the nano combined skin degerming emulsion of gained result of the test if no special instructions:
The carrier of 1 pair of different microorganisms soaks quantitative disinfecting test
Test organisms is staphylococcus aureus ATCC 6538, escherichia coli 8099, Candida albicans ATCC 10231.By the consumption of a slice bacterium sheet 5.0ml, the nanometer emulsion stock solution (positive control is PBS) of sterilizing is added respectively in the aseptic plate.Put preheating 5min in 19～21 ℃ of water-baths, add the bacterium sheet again.The effect certain hour is equipped with in the test tube of 5.0ml nertralizer (PBS that contains 2.5g/L glycine, 5g/L lecithin, 2.5% Tween 80 and 10% calf serum) neutralization 10min with the immigration of bacterium sheet.Beat test tube 80 times, with bacterium and mixing on the eluting bacterium sheet.Get eluent 0.5ml and do the viable bacteria counting, calculate killing rate.The result sees table 1.
Table 1, nanometer sterilization emulsion is to the killing effect of different microorganisms
Annotate: test temperature is 19～21 ℃.The average bacterium number of positive controls, staphylococcus aureus is the 1540000cfu/ sheet, and escherichia coli are the 3210000cfu/ sheet, and Candida albicans is the 3480000cfu/ sheet.
Table 1 result shows that to staphylococcus aureus, escherichia coli effect on the cloth sheet 3 minutes, average kill ratio all >=99.90% with nanometer sterilization emulsion stock solution; To staphylococcus aureus, escherichia coli, Candida albicans effect 5 minutes, average kill ratio can reach 100% with its stock solution.
2, different dilution factors are to the influence test of emulsion bactericidal effect
Test is carried out carrier with 1/2 diluent of nanometer sterilization emulsion stock solution, 1/10 diluent to Candida albicans and is soaked and quantitatively kill experiment, and test temperature is 19～21 ℃.The result sees table 2.
The different dilution factors of table 2, nanometer sterilization emulsion are to the killing effect of Candida albicans effect different time
Annotate: test temperature is 19～21 ℃.The average bacterium number of positive controls, the stock solution group is the 3300000cfu/ sheet, the dilution group is the 2600000cfu/ sheet.
Table 2 result shows, with nanometer sterilization emulsion diluent effect in 1: 1 10min, can reach 99.99% to the oidiomycetic average kill ratio of white, acts on 20 minutes, and average kill ratio can reach 100%; Is 98.16% with its 1: 10 diluent effect 30min to the Candida albicans killing rate.
3, temperature is to the influence test of prescription bactericidal effect
Under 25 ℃, 30 ℃, 35 ℃ conditions, use nanometer sterilization emulsion stock solution that Candida albicans is carried out the carrier immersion respectively and quantitatively kill experiment.The result sees table 3.
Table 3, nanometer sterilization emulsion act on different time to the oidiomycetic killing effect of white under different temperatures
Annotate: positive controls bacterium number is the 2300000cfu/ sheet, and the result is three test meansigma methodss.
Table 3 result shows that at 20～35 ℃, nanometer sterilization emulsion stock solution raises with temperature to the oidiomycetic killing rate of white and rises.
4, organic substance influence experiment
Behind the calf serum of adding 25% and 50%, the carrier that carries out nanometer sterilization emulsion stock solution soaks quantitatively kills experiment in the Candida albicans suspension of the sheet of dying cloth.The result sees table 4.
Table 4, Organic substance are killed the influence of Candida albicans effect to nanometer sterilization emulsion
Annotate: test temperature is 19～21 ℃.The result is three test meansigma methodss.
Table 4 result shows, dyes system bacterium sheet with the bacteria suspension that contains volume fraction 50% calf serum, and nanometer sterilization emulsion stock solution is killed the Candida albicans effect is not still had obvious influence.
5, the comparison of different formulations composition bactericidal effect
Solution A, B and C are all carried out carrier soak quantitative disinfecting test, relatively three's physicochemical property reaches the killing effect to microorganism, and the gained result is shown in table 5-8.
Table 5, embodiment 1 different formulations performance are relatively
In the table 5, solution A be according to embodiment 1 identical method, only do not add ethylenediaminetetraacetic acid, obtain solution A;
Solution B be according to embodiment 1 identical method, only the oxidation zinc concentration is replaced with 1g/L, obtain solution B;
Former embodiment 1 preparation gained sterilization emulsion is numbered solution C;
Table 6, embodiment 2 different formulations performances are relatively
In the table 6, solution A be according to embodiment 2 identical methods, only do not add ethylenediaminetetraacetic acid, obtain solution A;
Solution B be according to embodiment 2 identical methods, only the oxidation zinc concentration is replaced with 1g/L, obtain solution B;
Former embodiment 2 preparation gained sterilization emulsions are numbered solution C;
Table 7, embodiment 3 different formulations performances are relatively
In the table 7, solution A be according to embodiment 3 identical methods, only do not add ethylenediaminetetraacetic acid, obtain solution A;
Solution B be according to embodiment 3 identical methods, only the oxidation zinc concentration is replaced with 1g/L, obtain solution B;
Former embodiment 3 preparation gained sterilization emulsions are numbered solution C;
Table 8, embodiment 4 different formulations performances are relatively
In the table 8, solution A be according to embodiment 4 identical methods, only do not add ethylenediaminetetraacetic acid, obtain solution A;
Solution B be according to embodiment 4 identical methods, only the oxidation zinc concentration is replaced with 1g/L, obtain solution B;
Former embodiment 4 preparation gained sterilization emulsions are numbered solution C;
Solution D be according to embodiment 4 identical methods, only the oxidation zinc concentration is replaced with 1g/L, and does not add ethylenediaminetetraacetic acid, obtain solution D.
Table 5-8 Experiment on Microbiology is the result show; Compare with the solution A that does not contain ethylenediaminetetraacetic acid; After adding ethylenediaminetetraacetic acid in the prescription of solution C three kinds of microorganism killing effects are significantly increased, explain that ethylenediaminetetraacetic acid and chlorhexidine acetate have synergistic function; In solution B and solution D, deposit has appearred after leaving standstill for a long time behind the adding 1g/L nano zine oxide in the prescription, formulation stability is had appreciable impact, and the microorganism killing effect is compared no significance raising with solution C.
6, relatively to the natural bacteria antibacterial ability
Each 3 of the subsequent use silica gel tubes of sterilizing are soaked in respectively in chlorhexidine acetate aqueous solution that contains same amount and the nanometer sterilization emulsion that gets by the present invention's preparation, soak fully to take out after 3 minutes and dry.Each one of the silica gel tube of chlorhexidine acetate, the nanometer sterilization emulsion of learning from else's experience is put in the same plate; Put 3 plates altogether; The uncovered Microbiological Lab's windowsill of putting takes out with aseptic nipper in 6h, 12h, 24h, puts into the test tube that contains the 5ml nertralizer; Shake and leave standstill 10min, observed result behind inoculated and cultured 48～72h after striking.Result of the test is seen table 9.
Table 9, different disposal group are placed the growth inhibited situation of different time to natural bacteria
Through SAS statistical analysis, P
6h=0.000221, P
12h=0.001, P
24h=0.001.
Table 9 result shows; Sterilize two groups of samples of emulsion effect after same place is placed 6h, 12h, 24h simultaneously through simple chlorhexidine acetate solution and nanometer respectively; The growing state of natural bacteria all has significant difference, and simple chlorhexidine acetate group natural bacteria bacterium colony number average is higher than nanometer sterilization emulsion group.
7, hand site test results
Behind the each other abundant rubbing of experimenter's both hands, with cotton examination semar technique left hand is sampled, as the matched group of not sterilizing.Then, the nanometer emulsion stock solution 3ml that sterilizes is smeared evenly at the right hand.Act on 2 minutes, the right hand is smeared adopted sterilization group appearance.During sampling, 5 refer to close up, and aseptic cotton is wiped away in being contained in invisible spectro 5ml nertralizer soak, and after extracting on the tube wall, referring to that curved surface extremely refers to follow double rub 2 times from finger tip, whenever embrocate one time again, and cotton swab is rotated once.Cotton is wiped away head cuts into the dress nertralizer in vitro.Neutralization 10 minutes is beaten test tube and is wiped away bacterium and mixing with the eluting cotton.Get eluent and do the viable bacteria counting, calculate killing rate.Result of the test is seen table 10.
Table 10, nanometer sterilization emulsion effect 2min is to the killing effect of natural bacteria on hand
Table 10 result shows, nanometer sterilization emulsion effect 2 minutes is 94.09% to the average kill ratio of natural bacteria on hand.
More than test explanation; Each composition has synergistic function in this sterilization emulsion; Utilize chlorhexidine acetate that the present invention prepares and nano zine oxide composite skin sterilization emulsion can kill various bacteria such as staphylococcus aureus, escherichia coli, Candida albicans etc. fast and efficiently, the hand natural bacteria is had lasting antimicrobial effect.
The toxicological test of nano combined skin degerming emulsion provided by the invention:
This experiment is undertaken by " disinfection technology standard " (2002 editions) specific requirement.
1 acute oral toxicity test
Selecting body weight is 20 of Switzerland's kind Kunming outbreeding system healthy mices (female, hero half and half) of 18～22g, establishes a dose groups 6000mg/kg, after empty stomach 16h hour, presses the disposable per os of 0.2ml/10g body weight and irritates stomach.After irritating stomach, observe 14 days animal poisoning manifestations and death toll continuously, calculate LD
50The result shows that nanometer sterilization emulsion is to chmice acute per os toxicity test LD
50＞5000mg/kg body weight belongs to actual nontoxic level.
The test of 2 skin irritation
Selecting body weight is 4 of the rabbit of 2.2～3.0kg, and male and female are not limit.24h before test cuts scope 3cm with the hair of back part of animal both sides
2To be tried thing stock solution 0.2ml next day drips in 2.5cm
2On 2 layers of gauze of size and apply ointment or plaster, then with the covering of the non-stimulated oilpaper of one deck, the non-stimulated immobilization with adhesive tape of reuse at a side skin surface.Opposite side is as blank (or solvent control).Effect 4h is then with the residual thing that tried of warm water flush away; Tried 1h behind the thing, 24h, 48h respectively at removal, observed the local skin reaction, marked.The result shows that this emulsion acts on rabbit skin 4h, does not cause the animal skin IR, skin irritation index＜0.4, and stimulus intensity belongs to nonirritant.
3 eye irritant tests
Selecting body weight is 4 of 2.0～3.0 rabbit, and male and female are not limit.Get stock solution 1-2 and drip, splash in the rabbit one branch hole conjunctival sac, another branch hole is as normal control; Drip and to be tried the passive closed 4s of eye behind the thing, use normal saline flushing 5min.1h, 24h, 48h, 4d, the 7d damage and the recovery situation of tame lagophthalmos conjunctiva, iris and cornea that detect by an unaided eye behind eye drip.The result shows that this emulsion is up to 0 to the acute eye irritation score index of rabbit, and stimulus intensity belongs to nonirritant.
4 micronucleus tests
Select Switzerland to plant 50 of Kunming outbreeding system mices (female, hero half and half), body weight 25-30g.Female, male Mus is all divided in 5 groups at random.According to The acute toxicity tests, 4 test group are irritated stomach by body weight with the thing stock solution of being tried of 5000mg/kg, 2500mg/kg, 1000mg/kg dosage respectively, and negative control is irritated stomach with distilled water, and positive control is irritated stomach with cyclophosphamide (40mg/kg).Irritate stomach 2 times, 24 hours at interval, 6h drew materials conventional film-making microscopy behind the 2nd the filling stomach.Carry out statistical procedures with the U check.The result shows that this emulsion does not have the micronucleus of causing effect to PCEMNR.
This toxicity test result shows, nano combined skin degerming emulsion safety provided by the invention, nontoxic, non-stimulated can and have protective effect in human body skin, the safe handling of mucosa multipath.
Claims (10)
1. a nano combined skin degerming emulsion comprises chlorhexidine acetate, zinc oxide, ethylenediaminetetraacetic acid, emulsifying agent and water.
2. sterilization emulsion according to claim 1 is characterized in that: said nano combined skin degerming emulsion is made up of chlorhexidine acetate, zinc oxide, ethylenediaminetetraacetic acid, emulsifying agent and water.
3. sterilization emulsion according to claim 1 and 2 is characterized in that: said emulsifying agent is made up of vegetable oil, three normal-butyl phosphate and TritonX x-100; Said vegetable oil is 2-8 with the cumulative volume ratio of three normal-butyl phosphate and TritonX x-100: 1: 1, and preferred 8: 1: 1; Said vegetable oil is at least a in soybean oil, the Oleum Arachidis hypogaeae semen, preferred soybean oil.
4. according to the arbitrary described sterilization emulsion of claim 1-3, it is characterized in that: the concentration of said chlorhexidine acetate in said sterilization emulsion is 0.5～3g/L, preferred 2g/L;
Said oxidation zinc concentration is 0.01～0.5g/L, preferred 0.1g/L, and particle diameter is 50-100nm;
The concentration of said ethylenediaminetetraacetic acid in said sterilization emulsion is 0.01～0.2g/L, preferred 0.1g/L;
Said emulsifying agent accounts for the 10-20% of said sterilization emulsion cumulative volume, preferred 10%.
5. according to the arbitrary described sterilization emulsion of claim 1-4, it is characterized in that: in the said nano combined skin degerming emulsion, the diameter of drop is 10-30nm.
6. a method for preparing the arbitrary said sterilization emulsion of claim 1-5 comprises the steps: the arbitrary said component of claim 1-5 is mixed the back emulsifying, obtains said sterilization emulsion.
7. method according to claim 6 is characterized in that: in the said homogenizing step, temperature is a room temperature, and pressure is 25～35Mpa.
8. the application of the arbitrary said sterilization emulsion of claim 1-5 in skin degerming or preparation skin antiseptic.
9. the disinfectant liquid for skin that is active component with the arbitrary said sterilization emulsion of claim 1-5.
10. application according to claim 8 or the described disinfectant liquid for skin of claim 9 is characterized in that: said skin antiseptic or disinfectant liquid for skin all are staphylococcus aureus, escherichia coli and Candida albicans of killing skin surface.
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| CN2011103168392A CN102379898A (en) | 2011-10-18 | 2011-10-18 | Nanometer composite skin disinfection emulsion and preparation method thereof |
| CN2012100569460A CN102600206A (en) | 2011-10-18 | 2012-03-06 | Nano composite skin disinfection lotion and preparation method thereof |
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| CN103230386A (en) * | 2013-04-18 | 2013-08-07 | 徐州医学院 | Clean-free skin and hand micro-emulsion disinfectant agent and preparation method thereof |
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| CN103081940B (en) * | 2013-02-05 | 2014-06-18 | 河南科技学院 | Compound chlorhexidine acetate microemulsion disinfectant and its preparation method |
| GB201306980D0 (en) * | 2013-04-17 | 2013-05-29 | Blueberry Therapeutics Ltd | Methods |
| CN107041849A (en) * | 2017-04-11 | 2017-08-15 | 稳健医疗用品股份有限公司 | A kind of medical disinfecting emulsion and its preparation method and application |
| CN110100909A (en) * | 2019-05-06 | 2019-08-09 | 萌生健康管理(北京)有限公司 | A kind of compound oily preparation method of composition and its application with bacteriostasis |
| CN111281811A (en) * | 2020-03-20 | 2020-06-16 | 高密丽美生物科技有限公司 | Washing-free disinfecting skin-care cream and preparation method thereof |
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| CN103230386A (en) * | 2013-04-18 | 2013-08-07 | 徐州医学院 | Clean-free skin and hand micro-emulsion disinfectant agent and preparation method thereof |
| CN103230386B (en) * | 2013-04-18 | 2014-12-31 | 徐州医学院 | Clean-free skin and hand micro-emulsion disinfectant agent and preparation method thereof |
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