CN110292045A - A kind of antimicrobial compositions preparation method and application containing epsilon-polylysine - Google Patents

A kind of antimicrobial compositions preparation method and application containing epsilon-polylysine Download PDF

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Publication number
CN110292045A
CN110292045A CN201910381429.2A CN201910381429A CN110292045A CN 110292045 A CN110292045 A CN 110292045A CN 201910381429 A CN201910381429 A CN 201910381429A CN 110292045 A CN110292045 A CN 110292045A
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composition
polylysine
antimicrobial
epsilon
solvent
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CN110292045B (en
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张慧明
冯士清
吕萌
蒙雪艳
于跃
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Beijing Meike Xingye Biotechnology Co Ltd
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Beijing Meike Xingye Biotechnology Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/04Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aldehyde or keto groups, or thio analogues thereof, directly attached to an aromatic ring system, e.g. acetophenone; Derivatives thereof, e.g. acetals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/06Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing keto or thioketo groups as part of a ring, e.g. cyclohexanone, quinone; Derivatives thereof, e.g. ketals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/28Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/42Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing within the same carbon skeleton a carboxylic group or a thio analogue, or a derivative thereof, and a carbon atom having only two bonds to hetero atoms with at the most one bond to halogen, e.g. keto-carboxylic acids
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/46N-acyl derivatives
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
    • A01N47/42Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
    • A01N47/44Guanidine; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/35Ketones, e.g. benzophenone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/42Amides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4906Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
    • A61K8/4926Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having six membered rings
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88Polyamides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives

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  • Dermatology (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a kind of preparation method and applications of antimicrobial compositions containing epsilon-polylysine.It is by accounting for 1~20% epsilon-polylysine of total composition, 5~35% other antimicrobials and 60~90% solvent and builder composition.Antimicrobial is the mixture of one or both of decoyl hydroximic acid, levulic acid, levulic acid sodium, parahydroxyacet-ophenone, lauroyl arginine ethyl ester hydrochloride, tropolone, Octenidine.Solvent and builder are 1,2- propylene glycol, methyl propanediol, 1,3- propylene glycol, 1,3- butanediol, 1,2- hexylene glycol, 1,2- pentanediol, 1, one of 2- ethohexadiol, Decane-1,2-diol, polyethylene glycol, Sensiva SC50, propylene carbonate or at least two with the mixture of water.This composition can be water-soluble, facilitates addition to use, is widely used in the fields such as cosmetics, wet tissue, facial mask, washing.

Description

A kind of antimicrobial compositions preparation method and application containing epsilon-polylysine
The earlier application patent of the application is applying date 2019.04.29;Application number 201910355595.5;Denomination of invention For the patent application patent of " a kind of antimicrobial compositions preparation method and application containing epsilon-polylysine ".
Technical field
The present invention relates to a kind of antimicrobial compositions containing epsilon-polylysine, are mainly used for cosmetics, wet tissue, washing etc. The antiseptic and inhibiting bacteria function of people's nursing product and household items.
Background technique
Epsilon-polylysine (hereinafter referred to as ε-PL) derives from streptomyces albus tunning, is a kind of preventing for natural microbial source Rotten agent is approved by the FDA in the United States as safety food antistaling agent, is widely used in food fresh keeping in October, 2003.ε-PL antimicrobial spectrum is wide, To Gram-positive, negative bacteria, mould, saccharomycete has inhibiting effect, but a little to the inhibitory effect relative mistake of mould, therefore Often with other food categories preservative fit applications.
ε-PL is used as preservative, its advantage is that good water solubility, easy to use, light, thermal stability is good, and pH is applied widely, And ε-PL can be decomposed into lysine in human body, can be digested completely, not only without any toxic side effect, and And can be used as the source of human body lysine, it is a kind of natural, efficiently, safe food preservative.ε-PL is approved by the FDA in the United States For GRAS substance, additive amount uses highest usage amount 0.25g/kg in standard up to 0.025%, in Food Additives Used in China.
Existing patent is mostly that ε-PL compounds application in the food industry with natural antiseptic agent, is related to ε-PL and other anti-corrosions Agent compatibility case used in daily chemical products is less.And ε-PL and the ingredient with bacteriostatic activity outside preservative catalogue are common Using and be applied to cosmetics compatibility it is even more rare.
Chinese patent application publication No. CN103549622A data of publication of application on 2 5th, 2014, discloses a kind of collaboration Inhibit the natural bacteriostatic agent composition of common microbiological, wherein the combination of ε-PL and streptococcus lactis solves conventional bacteriostasis method In the larger problem of single bacteriostatic agent dosage, while expanding antimicrobial spectrum;Chinese patent application publication No. CN104958248A, Shen Please date of publication on October 7th, 2015, disclose a kind of biological bacteria inhibiting composition and its application in cosmetics, it is characterised in that Composition includes ε-PL, nisin, natamycin, glycerol, 1,3-BDO and pungent glycol, and composition has good Bacteriostasis especially has significant synergistic effect in terms of inhibiting Candida albicans, pseudomonas aeruginosa and aspergillus niger, can answer For reducing the additive amount of original preservative in skin type and washing class cosmetics;Chinese patent publication No. CN106691892A, Date of publication on May 24th, 2017 a kind of antibacterial wet tissue and preparation method thereof is disclosed, a kind of mild, safety wet tissue is provided, The potassium sorbate of ε-PL or its hydrochloride and 0.01-3% that solution on base material contains 0.01-3% are loaded, gained is wet Towel has achieved the effect that excellent in antibiotic property, skin moisture-keeping, the residual aspect of performance after wiping.
It is not difficult to find that natural microbial source preservative is as safely and effectively antibacterial kind in the retrieval to existing patent More and more attract attention, and actually at present in three big microbialpreservatives of international endorsement, nisin Antimicrobial spectrum is relatively narrow, mainly inhibited to bacterium, and more demanding to use condition, increases pH value or illumination, high temperature etc. Condition all can strong influence its bacteriostatic activity;Natamycin just for the fungi on cell membrane containing ergosterol there is suppression to kill Effect, it is then completely ineffective to bacterium, and also natamycin is insoluble in the organic solvents such as water or alcohol, and it is living under illumination or hot conditions Property ingredient be easy loss.Therefore it is also best selection that remaining polylysine, which just becomes uniquely, and polylysine antimicrobial spectrum is wide, right Bacterium, fungi, saccharomycete have inhibiting effect;Stability is good, and sterling and solution are in illumination and high temperature (120 DEG C, 60min) condition The lower reduction without changing colour with active constituent;It is water-soluble excellent, while alcoholic solution soluble easily in water;Degradable in vivo is that L- relies ammonia Acid, one kind as the necessary amino acid of human body;To sum up, polylysine is that a kind of safe and efficient stable standard amino acid solution is antibacterial Agent.It is used in compounding with some kinds with bacteriostatic activity, the needs of product microbial safety is not only able to satisfy, can also expire Sufficient consumer is to mild safe and non-stimulating pursuit.
It is safe and efficient the object of the present invention is to provide the antimicrobial compositions preparation method and application of-PL containing ε a kind of, Property is stablized, good water solubility, is easy to use, and compounding improves the antimicrobial spectrum of polylysine, especially enhances to fungi strain Inhibiting effect can add in the personal care articles of nearly all category, it can also be used to which the antibacterial anti-corrosion of household articles for washing expands Big use scope of the polylysine in daily chemical products, while the usage amount of chemical preservative in daily chemical products can be reduced.
Summary of the invention
The present invention provides a kind of composition containing ε-PL, antimicrobial, solvent and builder, ε-in the composition PL is compounded with Multiple components, is improved disadvantage poor to fungi inhibiting effect itself, is enhanced the fungistatic effect of ε-PL, expands Antimicrobial spectrum, and can be applied in a variety of personal care articles, daily chemical products and family product, the composition is to common mould And saccharomycete has excellent inhibiting effect, antimicrobial spectrum is wide, effect stability, and usage amount is low.
Component contained by the present invention has:
A)ε-PL;
B) antimicrobial;
C) solvent and builder.
A in the composition) ε-PL.
B in the composition) antimicrobial includes decoyl hydroximic acid, levulic acid, levulic acid sodium, para hydroxybenzene second The mixture of one or both of ketone, lauroyl arginine ethyl ester hydrochloride, tropolone, Octenidine.
C in the composition) solvent and builder include 1,2- propylene glycol, methyl propanediol, 1,3- propylene glycol, 1,3- Butanediol, 1,2- hexylene glycol, 1,2- pentanediol, 1,2- ethohexadiol, Decane-1,2-diol, polyethylene glycol, Sensiva SC50, the third two One of alcohol carbonic ester or at least two with the mixture of water.
Wherein, A in the composition) ε-PL weight percentage be 1-20%;Preferably 1-15%;More preferably 5- 12%.
B in the composition) antimicrobial weight percentage be 5-35%;Preferably 10-30%.
C in the composition) solvent and builder weight percentage be 60-90%;Preferably 60-75%.
The present composition is the preparation method comprises the following steps: by A) ε-PL C) after container is added in the ingredient in solvent and auxiliary agent in addition to water Stirring, is warming up to 35-40 DEG C, adds C) in aqueous solvent and B) antimicrobial, stirring to it is complete it is molten after to obtain the final product.
The present composition all has mould, saccharomycete under the additive amount of 0.5-1.2% and inhibits to make well With.Product applicability is wide, and usage amount is small, at low cost, other used antimicrobial acivity compositions, and some is that can be used for food Preservative, some belongs to non-stimulated or low stimulation by chick chorioallantoic membrane chorion irritation test and the detection of human body patch test Ingredient, it is harmless therefore credible in terms of safety irritation.Composition can be water-soluble, and various occasions can make With.
Personal care articles of the present invention, household articles for washing etc. include but is not limited to cream, lotion, facial cleanser, Gel The products such as curry, shampoo, shower cream, hand cleanser, toothpaste, toner, detergent, liquid detergent, wet tissue class.
Detailed description of the invention
Fig. 1 is stability data of the ε-PL in part formulation
Fig. 2 is that the illumination of product and high-temperature stability compare in the composition 2# of-PL containing ε and documents
Arrange from left to right: 2# is initial;2#54℃24h;2# illumination 30d;Comparison is initial;54 DEG C of comparison is for 24 hours;Compare illumination 30d
Fig. 3 is that the composition part formulation of-PL containing ε challenges test result-directed toward bacteria result
Fig. 4 is the result that the composition part formulation of-PL containing ε challenges that test result-is directed to fungi
Specific embodiment
The following examples facilitate those skilled in the art and the present invention are more fully understood, but do not limit in any way The present invention.In these embodiments, all dosages and ratio are by weight.
Embodiment 1
1 antimicrobial compositions each component content (weight %) of table
Preparation method: in the 100mL there-necked flask with stirring, thermometer, 1 each component content of table, addition ε-PL and molten are pressed Ingredient in agent than water is stirred and heated to 35~40 DEG C, adds water, maintains relevant temperature, stirs and that remaining is added is anti- Microorganism agent ingredient, continue to stir to it is complete it is molten after be cooled to 35 DEG C hereinafter, up to stable transparent antimicrobial compositions solution Formula.
Embodiment 2
Investigate cold-resistant, heat-resisting, the light durability of part formulation in embodiment 1, and with documents (publication No. CN104958248A, it is a kind of biology bacteria inhibiting composition and its application in cosmetics) described in product compare, as a result see Fig. 1, Fig. 2, table 2.
2 part formulation stability of table
Fig. 1, Fig. 2, table 2 show that color does not change under composite formula illumination and hot conditions, and targeted activity object content is protected Hold constant, and contrast product color under illumination and hot conditions generates large change, embodies the group of-PL containing ε in this explanation Close the good stability of object.
Contrast product formula combination:
ε-PL 0.5%;Nisin 0.1%;Natamycin 0.4%;Glycerol 5%;1,3 butylene glycol 3%;Xin Gan Alcohol 1%.
Embodiment 3
Anti- (suppression) bacterium test --- minimum inhibitory concentration (MIC value) measurement.
The minimum inhibitory concentration (MIC value) of part antimicrobial compositions and ε-PL in table 1 are measured by suspension method, as a result It is shown in Table 3.
3 fraction compositions minimum inhibitory concentration (MIC value) of table
Table 3 is that ε-PL single-item and fraction compositions are formulated minimum inhibitory concentration, it can be seen that ε-PL imitates the inhibition of fungi Fruit relatively differs more to bacterium, and composite formula compounds other kinds on the basis of containing ε-PL 10%-20% and resists micro- life Agent, the MIC value that MIC value is scaled sterling can still compare favourably with single-item, for being formulated 5#, to staphylococcus aureus MIC be 500ppm, wherein ε-PL content be 20%, the MIC value for being converted into sterling is then 100ppm, than simple ε-PL MIC150ppm illustrates that the antimicrobial of compounding can expand the antimicrobial spectrum of ε-PL compared to decreasing;And to the antibacterial of aspergillus niger Synergistic effect becomes apparent, in the formula of 3500ppm containing 20% ε-PL, be scaled sterling MIC be 700ppm, it is more single The 2000ppm of ε-PL reduces 2/3rds.So in actual use, under relatively low additive amount (general≤1.2%) The requirement for anticorrosion of product can still be met.
Embodiment 4
Inhibitor effectiveness test --- Microbial Challenge test.
With reference to the protective system efficiency evaluation method that cosmetics spices and essence association, the U.S. (CTFA) is recommended, 28 days lists are carried out It is secondary to connect the test of bacterium challenge.
1. test strain: bacterium (E. coli, staphylococcus aureus S.aureus, pseudomonas aeruginosa P.aeruginosa;Fungi (aspergillus niger A.niger, candida albicans bacterium C.albicans).It is inoculated with using Mixed Microbes, bacterium is mixed Combined bacteria suspension 107CFU/mL;Fungi Mixed Microbes suspension 106CFU/mL。
2. test specimen: preparing facial mask formula of liquid by table 4, wherein anti-corrosion composition, which adds type and using content, is respectively A -1.0%5#, B -0.8%6#, C -1.2%7#, D -0.8%10#, 0.15% ε-PL of E -, and numbered and made with protective system For sample number into spectrum, to investigate the fungistatic effect of different protective systems.
4 composition preservation challenge experimental basis formula of table
3. sample inoculation: weighing each 2 parts of 100 grams of above-mentioned cosmetics A, B, C, D respectively, it is outstanding to be separately added into 1mL mixed cell Turbid and 1mL mixed fungus suspension are uniformly mixed, and sample is saved in (22.5 ± 2.5 DEG C) of room temperature, and respectively at 0,2,7, 14, the clump count in 21,28 days detection cosmetics, to judge protective system efficiency.
4. test result
In 0,2,7,14,21 and 28 day sample detection of inoculation, the result is shown in table 5, Fig. 3, Fig. 4:
5 composition Microbial Challenge test result of table
Table 5 and Fig. 3, Fig. 4 show that compared with ε-PL is used alone, the compounded combination of ε-PL and a variety of antimicrobials uses It can reach good fungistatic effect, i.e. antimicrobial can overcome the disadvantages that ε-PL to the disadvantage of fungi inhibiting effect difference, is significantly expanded Its antimicrobial spectrum.Composition can be used as the excellent bacteriostatic agent of daily chemical products.
Embodiment 5
Irritation test --- patch test
Using 30 qualified volunteers as object, the lotion 0.020g-0.025g sample containing composite formula is taken (including protective system is respectively A -1.0%5#, B -0.8%6#, C -1.2%7#, D -0.8%10#) is placed in spot tester In coyote hole, the back or forearm song side of subject will be pasted on low sensitization adhesive tape added with the spot tester of tested material, it is light with palm Pressure is allowed to equably be pasted on skin, continues 24 hours.The 0.5h after removing tested material spot tester, is pressed with 48h for 24 hours 6 standard sight dermoreaction of table, and observation is recorded as a result, to there is positive reaction number as data.
6 skin closure type patch test dermoreaction grade scale of table
7 skin closure type patch test dermoreaction test result of table
Table 7 is the results show that each group of formula is nonirritant to human body in actual use, and ε-PL is as a kind of natural micro- life The preservative of material resource, feature good, non-stimulated with safety itself, compounds with other kinds of antimicrobial, reduces Using the ratio of chemical component, a possibility that irritation occurs is also reduced.

Claims (6)

1. a kind of antimicrobial compositions containing epsilon-polylysine, which is characterized in that the composition contains: epsilon-polylysine resists Microorganism agent, solvent and builder;
Antimicrobial is decoyl hydroximic acid, levulic acid, levulic acid sodium, parahydroxyacet-ophenone, laurel in the composition The mixture of one or both of acyl arginine ethyl ester hydrochloride, tropolone, Octenidine;
In the composition solvent and builder be 1,2- propylene glycol, methyl propanediol, 1,3- propylene glycol, 1,3 butylene glycol, 1,2- hexylene glycol, 1,2- pentanediol, 1,2- ethohexadiol, Decane-1,2-diol, polyethylene glycol, Sensiva SC50, propylene glycol carbonic acid One of ester or at least two with the mixture of water.
2. composition according to claim 1, which is characterized in that epsilon-polylysine weight percent contains in the composition Amount is 1-20%.
3. composition according to claim 1, which is characterized in that antimicrobial weight percent contains in the composition Amount is 5-35%.
4. composition according to claim 1, which is characterized in that solvent and builder weight percent in the composition It is 60-90% than content.
5. composition described in -4 according to claim 1, which is characterized in that preparation method are as follows: Xiang Peifang solvent and synergy help Sequentially add epsilon-polylysine, water, antimicrobial in liquid in agent in addition to water, 35-40 DEG C of computer heating control, stirring and dissolving The stable antimicrobial compositions containing epsilon-polylysine can be obtained.
6. composition according to claim 1 is used for personal care articles, wet tissue, the use of household articles for washing antiseptic and inhibiting bacteria function On the way.
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