CN104738033A - Preservative composition derived from plants - Google Patents
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- CN104738033A CN104738033A CN201510057218.5A CN201510057218A CN104738033A CN 104738033 A CN104738033 A CN 104738033A CN 201510057218 A CN201510057218 A CN 201510057218A CN 104738033 A CN104738033 A CN 104738033A
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Abstract
The invention discloses a preservative composition derived from plants. A cosmetic preservative composition mainly comprises following plant source substances in percentage by weight: 0.05-10% of citral, 0.05-10% of vanillin, 0.05-10% of anisic acid and 0.05-10% of magnolol. The preservative composition is relatively wide in antibacterial spectrum and can be used as a preservative to be used for cosmetics to take the effects of inhibiting the growth of bacteria and fungi; and antibacterial components of the composition are selected from plant active substances both used as medicines and foods, have no harms to a human body, have no irritation, no allergy and no toxic or side effect, and can be safely applied to the cosmetics. The cosmetic preservative can be used for effectively inhibiting microorganisms in the cosmetics from breeding and can replace or reduce the use amount of a chemically synthetic preservative when used for the cosmetics, so that the irritation caused by the chemically synthetic preservative in a product is reduced and the product safety is improved; and meanwhile, the stability of the cosmetics is not influenced.
Description
Technical field
The present invention relates to a kind of preservative prescription, be specifically related to a kind of cosmetics preservative be combined into by plant origin substances in percentage by weight.
Technical background
Vanillic aldehyde, has another name called vanillin, is the widely used edible spices of one, has strong milk breath.Assumed name is called 3-methoxy-4-hydroxybenzaldehyde.Vanillic aldehyde uses as conventional spices, finds that vanillic aldehyde has restraining and sterilizing bacteria ability to bacterium class bacterial classification.Make vanillic aldehyde while playing perfuming effect as spices, the effect of antiseptic and inhibiting bacteria function can be played again, for vanillic aldehyde is applied to the space that cosmetic industry provides more wide.Vanillic aldehyde has fungistatic effect to Escherichia coli, is 0.235% to colibacillary minimum inhibitory concentration (MIC).Vanillic aldehyde has fungistatic effect to staphylococcus aureus, and the minimum inhibitory concentration (MIC) of vanillic aldehyde to staphylococcus aureus is 0.294%.Vanillic aldehyde has fungistatic effect to saccharomycete, and vanillic aldehyde is 0.118% to saccharomycetic minimum inhibitory concentration (MIC).Vanillic aldehyde has fungistatic effect to aspergillus niger, and the minimum inhibitory concentration (MIC) of vanillic aldehyde to aspergillus niger is 0.059%.
Anisic acid is active ingredient in Chinese anise, research shows, containing sterilization, Substance in Chinese anise, as anisic acid (3%), anisaldehyde (48%) etc., Chinese anise water extract is prepared natural antiseptic agent as raw material by existing application.Have stronger inhibitory action to Escherichia coli, hay bacillus, golden yellow grape bacillus, aspergillus niger, aspergillus flavus, mould, water soluble ingredient respectively is 13.5,17.5,13,30.8,29.5,32.6mm to the above-mentioned size for examination bacterium inhibition zone.
Citral is a kind of monoterpene, colourless or light yellow transparent liquid, having strong lemon sample fragrance, be used in foods and cosmetics usually used as flavor enhancement, preservative and aromatic, is also the primary raw material of synthetic vitamin A, irisone, methylionone.Chemical name is 3,7-dimethyl-2,6-octadiene-1-aldehyde, and molecular formula is C
10h
160.In addition, citral has desinsection, repellent, the effect such as antibacterial, anti-oxidant.The anti-bacterial result: citral can anti-candida albicans, and its minimum inhibitory concentration value (MIC) is 0.05%.In AGP test experiment, citral all has good resistance to Escherichia coli, bacillus subtilis and staphylococcus aureus.When citral volumetric concentration is greater than 0.01%, colibacillary growth rate reduces; When being greater than 0.03%, its number of viable cells reduces fast, limits its regeneration.
Magnolol is the Magnolia cortex P.E of sepia to white fine powder, the active ingredient of antibacterial action in Cortex Magnoliae Officinalis skin.There is special, lasting myorelaxant effects and strong antibacterial action, can Antiaggregating activity on platelet.Main as antibacterial, antifungal clinically.Magnolol has significant antibacterial activity to gram-positive bacteria, acid resistance bacterium, yeast-like fungi and filamentous fungi.Show with lowest concentration of antimicrobial (MIC) test that streptomycin sulphate, amphotericin B are contrast, the anti-tangerine grass bacillus of magnolol, staphylococcus aureus specific activity streptomycin sulphate are high; Anti-trichophyton mentagrophytes specific activity amphotericin B is high; Anti-black-koji mould is active identical with amphotericin B.The anti-caries tooth effect of magnolol is very remarkable, and be 6.3 μ g/ml to the minimum inhibitory concentration (MIC) of caries bacteria, its antibacterial activity is better than typical antibacterial biological alkali jamaicin (MIC:50 μ g/ml).In addition, magnolol also has obvious antibacterial activity for causing the bacillus anthracis of human malignant's running sore and fine hair shape module disease.
The Preservative Technology for Personal Care of current countries in the world report is more than 200 kinds, comprise phenols, ester class, halide and quaternary ammonium salt etc., wherein with the propylparaben (preservative that nipagin esters) Lei, Kay pine, imidazolidinyl urea and Bronopol the most often use.And chemical preservative is one of cosmetic material easily causing skin safe sex chromosome mosaicism, many countries have all made strict regulation to its kind and using dosage.
Parabens is that the whole world is all approved, tradition uses, non-stimulated, not sensitization and the high cosmetics preservative of safety, such preservative occupies the prostatitis of frequency of utilization ranking always over several years, but there is report parabens can cause contact dermatitis and have estrogen active now, its whether harmful topic having become discussion at present, although science there is no this and makes decision, but industrial circle in order to cosmetic product perspective develop, to the cosmetics containing animals and plants composition, especially green natural cosmetics generally reduce or do not use nipagin esters to make preservative.And for the practical problem being easy to exceed standard containing the cosmetics of animals and plants composition and green Cosmetics microorganism, there is no ripe effective standardization special anti-corrosion system at present, from natural animal-plant, find wide spectrum, the focus that efficient, low toxicity, natural preservative have become area research.
The active ingredient to antibacterial action can be caused in plant to have: alkaloids, flavonoids, coumarin and lactone, saponins, phenolic compound, Anthraquinones, terpenoid etc.Antibacterial mechanisms in natural plants mainly contains the following aspects: (1) acts on cell wall and cell membrane system, destroys barrier cell, makes cell can not growth and breeding; (2) act on genetic material or cell particles structure, hinder copying of hereditary information; (3) act on enzyme or functional protein, make the material base of cell loss growth and breeding.
Report that Plants up to ten thousand contains antibacterial substance at present.The natural antiseptic agent of plant resource generally derives from the Chinese herbal medicines such as Radix Glycyrrhizae, cordate houttuynia, the capsule of weeping forsythia, ginkgo; The spices such as anise, Chinese cassia tree, thyme, cloves; The fruits and vegetables such as green tea, apple material; And the wild plant such as the fruit of a cubeb litsea tree, five-leaved chaste tree, gurgeon stopper.Antipathogenic composition is generally present in other parts of the essential oil fraction of leaf, flower and bud, bulb, root, fruit or plant.Its active ingredient comprises the secondary metabolic compounds such as alkaloid, flavonoids, lactone, terpene, phenols, Anthraquinones, and natural plants antibacterial peptide.Japan develops natural antiseptic agent country comparatively rapidly in recent years, develop natural antiseptic agent tens of kinds at present, wherein plant extracts class accounts for larger proportion, as ginkgo biloba p.e, mulberry-leaf extract, cinnamomum cassia extract, Flos Caryophylli extract, Ginger P.E, Rosmarinus officinalis extract, sweet green pepper extract and Fructus Piperis extract etc.Wherein forsythia suspense extraction has been ratified to use as preservative in Japan.
The antibacterial agent of animal origin mainly contains: lyase bacterium, lactotransferrin, ovotransferrin, shitosan, pleurocidin, Protamine, defensin etc.
Microbe-derived antibacterial agent mainly contains: nisin, Roche rhzomorph, partially coccus element, natamycin, polylysine etc.
Antimicrobial test shows, although each Plant Extracts has respective no antimicrobial spectrum, show antibacterial broad spectrum activity, but the secondary metabolite of traditional anti-inflammatory Chinese herbal medicine (comprises Gram-positive bacteria and Gram-negative bacteria to bacterium, as Escherichia coli, salmonella, hay bacillus, staphylococcus aureus etc.) there is good antibacterial ability, fungi (comprising yeast and mould, as Candida albicans, aspergillus niger etc.) antibacterial ability is differed; And spice extract all has antibacterial ability to bacterium, fungi, especially there is stronger antibacterial ability to fungi; The antimicrobial acivity of Antimicrobial Peptides From Plants is mainly manifested on efficient antifungal, also there is inhibitory action to some Gram-positive bacterias and negative bacteria.
Summary of the invention
The object of the invention solves the limitation of prior art, propose one and use citral, vanillic aldehyde, anisic acid, magnolol four kinds of components simultaneously, with reaching bacteriostasis Escherichia coli, golden yellow grape bacillus, white being read to coccus etc. during the having and use under various conditions of the cosmetics preservative of this configuration.
Concrete technical scheme is as follows
Plant antiseptic agent provided by the present invention, every 100g is containing, for example lower component
In the present invention, vanillic aldehyde and anisic acid play main antibacterial action; Citral plays anti-interference and does flavouring agent effect, citric acid for regulating acid-base value.
The cosmetics preservative prescription of this plant origin has following characteristics:
1. has a broad antifungal spectrum.It has good anti-microbe ability, and antibacterial category is very wide, and for the multiple microorganism with different extinction spectrum, all have and kill or bacteriostasis, namely antibacterial band is very broad.The various noxious bacteria kinds of having tested confirmation comprise the Gram-negative bacterias such as Escherichia coli, and hay bacillus and streptococcus etc. more than 30 plants gram-positive bacteria.Fungi and yeasts, comprises Candida albicans etc.
2. good bacteriostasis property.Prove through repeated pathogene microorganism " minimum inhibitory concentration " (MIC) experiment, its natural plant preservative has very strong antibacterial efficacy, even if under the consumption diluted very much, this efficient performance also can show.Such as, vanillic aldehyde has fungistatic effect to Escherichia coli, is 0.235% to colibacillary minimum inhibitory concentration (MIC).Vanillic aldehyde has fungistatic effect to staphylococcus aureus, and the minimum inhibitory concentration (MIC) of vanillic aldehyde to staphylococcus aureus is 0.294%.Vanillic aldehyde has fungistatic effect to saccharomycete, and vanillic aldehyde is 0.118% to saccharomycetic minimum inhibitory concentration (MIC).Vanillic aldehyde has fungistatic effect to aspergillus niger, and the minimum inhibitory concentration (MIC) of vanillic aldehyde to aspergillus niger is 0.059%.
3. these natural plant preservative raw material sources are daily conventional natural plants, and the chemical preservative replacing chemical industry to synthesize for raw material with safe and harmless natural plants, being down to minimum to the infringement of human skin cell.
4. non-stimulated or allergy.For many years, first reason lethal by prescription drug is anaphylactic shock, and anaphylactogen penicillin ex hoc genus anne antibiotic often.Cosmetics are also like this, when the concentration of drug use a certain in cosmetics is higher than Diazolidinyl Urea during certain value, make human body produce allergy.Epidermis toxicological experiment result proves, the non-stimulated or allergy to human skin cell of 1% or 2% composite natural antiseptic agent.
5. can be compatible with other natural drugs.Have the Chinese tradition traditional Chinese medicine and pharmacy of more than 5000 year history to confirm, Chinese medicine compound prescription is usually more conducive to treatment than herbal medicine folk prescription.Wherein Chinese anise popular important compound formula so far especially.These fact proved, natural antiseptic agent has synergistic function.According to the beneficial effect that such scheme can obtain be:
A. the present invention provides a kind of that citric acid, vanillic aldehyde, anisic acid honokiol is composite as cosmetics preservative first.
B. plant antiseptic agent provided by the invention has very wide antimicrobial spectrum.Its antibacterial bands of a spectrum had are very wide, can kill active ingredient or suppress harmful microorganism breeding.This plant antiseptic agent still has good antibacterial action when temperature 120 DEG C.Its feature also had is neutrality (PH6.8 ~ 7.2), safety non-toxic, harmless, non-stimulated, without irritated, have no side effect.
C. well compatible with natural drug, there is the features such as biodegradability.
Embodiment
Below provide the specific embodiment of the present invention, be used for being further described formation of the present invention.
The present invention is a kind of novel plant preservative, by weight proportion, comprise the citral of 0.05 ~ 10%, 0.05 ~ 10% vanillic aldehyde, 0.05 ~ 10% anisic acid, magnolol 0.05 ~ 10%, citric acid and deionized water.
Deionized water: adopt the non-heat treated preparations such as ion-exchange, hyperfiltration, ultrafiltration; Described citric acid, for regulating described plant antiseptic agent pH value, makes plant antiseptic agent PH finally 6.8 ~ 7.2.
For solving technical problem of the present invention, by realizing by the following technical solutions, a kind of method producing described novel plant preservative can also be proposed, comprises step:
A, by weight proportion, choose the citral of 0.05 ~ 10%, 0.05 ~ 10% vanillic aldehyde, 0.05 ~ 10% anisic acid, magnolol 0.05 ~ 10%, 10 ~ 15% deionized water;
B, above-mentioned four kinds of compositions fully to be mixed in mixing kettle, obtain plant antiseptic agent stoste;
C, add citric acid by the plant antiseptic agent stoste obtained in above-mentioned steps B, make its pH value be 6.8 ~ 7.2
D, add deionized water by the liquid obtained in above-mentioned steps C again, thus finally obtain described plant antiseptic agent.
In above-mentioned steps B, citral, vanillic aldehyde, anisic acid, magnolol and deionized water turn abundant mixing with 180r/min in mixing kettle.
Embodiment 1
The preparation process of this plant antiseptic agent is described with a specific embodiment below:
1, to configure this biological preservative 100g, raw material is taken in prescription ratio.
2, by the abundant mix and blend mixing in mixing kettle of above-mentioned citral, vanillic aldehyde, anisic acid, magnolol and deionized water, under stirring, add citric acid, make solution PH to 6.8 ~ 7.2.
3, obtained solution is added deionized water to 100g, namely obtain this plant antiseptic agent.
Plant antiseptic agent prepared by said method has has a broad antifungal spectrum, can suppress the Gram-positive bacterias such as Gram-negative bacteria and staphylococcus such as Escherichia coli; Derive from natural, have no side effect; The effects such as natural moisture preserving.Not only as the preservative of the safety in cosmetics, and can also play natural nourishing effect at corrosion-resistant simultaneously.
The plant antiseptic agent prepared by said method carries out the test of microorganism system challenge, tests with staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, and candida albicans is as inoculation bacterium.The addition of plant antiseptic agent is 50%, inoculated bacteria total concentration 2.2 × 10
8cFU/ml, inoculated fungi total concentration is 5.18 × 10
7cFU/ml, observed through 28 days, within the 7th day, began all to be less than 10CFU/ml to the 28th day bacterium, fungi concentration.This plant antiseptic agent, by the test of antimicrobial preservation system challenge, can be used as preservative completely and plays antisepsis.
Embodiment 2
The plant-derived products prepared using said method is below prepared facial mask as cosmetics preservative and its application at cosmetics is described.
By weight, choosing the ratio of above-mentioned biological preservative in face pack prescription is 50%.
A, by face pack prescription first by other compositions outside biological preservative composition by Process configuration good;
B, steps A are under the stirring of 200r/min, and temperature less than 40 DEG C, slowly, adds biological preservative continuously;
30 minutes are left standstill after C, fully stirring;
D, filling, packaging
Embodiment 3
The plant antiseptic agent prepared by said method and single raw material carry out bacteriostatic test, test is with staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, candida albicans, as inoculation bacterium, adopts the test of K ~ B paper disk method to compare the difference of bacteriostasis between them.
Concrete process of the test is as follows:
1, experimental technique
By Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa inoculates on MH liquid nutrient medium respectively, at 37 DEG C, cultivate 24h; Candida albicans inoculation is husky protects weak liquid nutrient medium, at 25 DEG C, cultivate 5d.With physiological saline, four kinds of bacterial culturess being diluted to concentration is respectively 1.0 × 10
6the bacteria suspension of CFU/ml.
Prepare citral respectively, vanillic aldehyde, anisic acid, magnolol and the antiseptic agent solution prepared by said method, concentration is 10mg/ml.
Be coated on nutrient agar panel by above-mentioned four kinds of bacteria suspensions respectively with aseptic cotton carrier and make lawn, then cut-off footpath is the sterilizing filtrate disk of 3cm.After evenly picking 5 kinds of drug solutions made respectively, then be attached to respectively on flat board that four kinds of different bacteria suspensions make.Bacterial culture 24h, fungal culture 5d, observed result.
1) evaluation method:
Paper disk method bacteriostatic diameter >=10mm is that effectively bacteriostatic diameter≤10mm is invalid.
2) experimental result is in table 1
The antibacterial result of table 1 paper disk method preservative
Analysis result obtains, and natural antiseptic agent prepared by said method has good fungistatic effect.All better than the fungistatic effect of each single raw material, outstanding composite natural antiseptic agent has synergistic advantage.
Ag content is 100 ~ 10000ppm
Embodiment 3
Adopt and repeat the Microbiology challenge test method-CTFA method (challenge experiment) adding bacterium, specific experiment process is as follows:
1. excitation experiment uses microorganism
The microorganism of provocative test has gram-positive cocci, as staphylococcus aureus (at least one); The gram-Negative bacillus of fermentation, as Escherichia coli (at least two kinds); The gram-Negative bacillus of non-fermented, as Pseudomonas aeruginosa (at least one); Mould, as black-koji mould and Aspergillus flavus (at least one); Saccharomycete, as Candida albicans (at least one); Aerobic spore production bacteria and bacillus subtilis etc. all can be selected, some preservative resistant effects by product separation bacterial strain out also the optional excitation experiment that is used as use microorganism.
2. microbial inoculant concentration
Microbial inoculant concentration is 1.0 × 10
6cFU/ml, apply some make up yeast and mold concentrations of eye is 1.0 × 10
4cFU/ml.
3. the time-program(me) of sampling and measuring
Sampling excites the time-program(me) of mensuration to be postvaccinal 0, and 3,7,14,21,28 days sampling and measuring, and add bacterium once
4. the standard of validity
Different with use position according to product purpose, the standard slightly difference of validity.The liquid of the eye that clear stipulaties is moisture and the standard of semiliquid cosmetics are: 1. live bacterium excite in 7 days reduce 99.9%, and in experimentation continue reduce; 2. saccharomycete and mould reduced by more than 90% in 7 days, and constantly reduced in whole experimentation; 3. in whole experimentation, have inhibitory action to Bacillus, this standard is selected in experiment herein.
5. test procedure
(1) the experiment preparation of inoculum (bacterium liquid)
Pure culture should be selected as experiment bacterial strain.Before experiment, should be seeded on peptone agar or ordinary broth agar medium respectively with fresh slant culture, cultivate 24 hours in 30.37 DEG C; With physiological saline, culture is diluted to every milliliter containing bacterium number about 1.0 × 10
5individual.The saccharomycete of standby experiment and mould, should be seeded on sabouraud's agar or improvement Martin's agar medium inclined-plane respectively with fresh slant culture.Aspergillus niger is cultivated 7 days at 20 ~ 28 DEG C, with normal saline dilution to every milli well about 1.0 × 10
5the bacterium suspension of spore.
(2) medium
The suitableeest medium giving the growth of each experimental strain should be selected.As to bacterium, available egg is from peptone agar medium.Broth medium, can use sabouraud's agar, improvement Martin medium, czapek agar medium to saccharomycete and mould.Also other can be selected to be suitable for the eugonic medium of these bacteria growings.
(3) experimental implementation
5 parts of samples are got, every part of 20mL with the test tube of the sterilization of suitable large small band plug; Every part of sample is inoculated by the ratio identical in 0.1ml inoculum 20ml sample.After making inoculation, the microorganism concn of test solution is 1.0 × 10
5~ 1.0 × 10
6cFU/ml test solution.Measure the microbe quantity of the rear every part of sample of inoculation, calculate the number of every milliliter of microorganism, as test micro initial concentration.After inoculation, sample carries out cultivating (or cultivating at specified temperatures) at 28 DEG C.After inoculation after 3,7,14,21,28 days, measure the biological number of the work of sample with the method for plate culture count, record the change of its outward appearance, when starting using each sample, the concentration of microorganism is as theoretical concentration, calculates the percentage of often kind of microbiology turbidity.
According to the validity of above-mentioned criterion evaluation preservative.
(1) antiseptic effect excellent (W:well preservative), after namely adding bacterium four times, when adding the 7th day after bacterium, survival bacterium amount is reduced to not higher than 0.01% of initial concentration at every turn.
(2) antiseptic effect still can (M:marginal preservative), and when adding the 7th day after bacterium, survival bacterium amount is reduced to not higher than 0.1% of initial concentration at every turn.
(3) antiseptic effect difference (P), when adding the 7th day after bacterium at every turn, survival bacterium amount > 1000/g.
Table 2 preservative challenge test result
Finally illustrate, above embodiment is only in order to illustrate that technical scheme of the present invention is unrestricted, although with reference to preferred embodiment to invention has been detailed description, those skilled in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in right of the present invention.
Claims (4)
1. a preservative prescription for plant origin, is characterized in that: its main component comprises plant origin material: citral, vanillic aldehyde, anisic acid, magnolol.
2. the preservative prescription of a plant origin, it is characterized in that: the plant origin material comprising following percentage by weight: citral 0.05 ~ 10%, vanillic aldehyde 0.05 ~ 10%, anisic acid 0.05 ~ 10%, magnolol 0.05 ~ 10%, PH conditioning agent citric acid and balance deionized water.
3. the preservative prescription of a plant origin, it is characterized in that: the preparation method of preservative: choose the vanillic aldehyde of weight ratio 0.05 ~ 10%, 0.05 ~ 8% citral, 0.05 ~ 10% anisic acid, magnolol 0.05 ~ 10%, 10 ~ 15% deionized water, fully mix in mixing kettle, add citric acid, its pH value is made to be 6.8 ~ 7.2, add deionized water, thus finally obtain described plant antiseptic agent.
4. prescription relate to citral, vanillic aldehyde, anisic acid, magnolol for the plant origin aseptic applications of main component is in the daily cosmetics such as facial mask, reach Antimicrobial preservative effect.
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