CN105362140B - A kind of non-cosmetics preservative composition and its application with preservative efficacy - Google Patents
A kind of non-cosmetics preservative composition and its application with preservative efficacy Download PDFInfo
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- CN105362140B CN105362140B CN201510843349.6A CN201510843349A CN105362140B CN 105362140 B CN105362140 B CN 105362140B CN 201510843349 A CN201510843349 A CN 201510843349A CN 105362140 B CN105362140 B CN 105362140B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/42—Amides
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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Abstract
The invention discloses a kind of non-cosmetics preservative compositions with preservative efficacy, it is characterised in that by forming following weight percentage components：Caprylhydroxamic acid, 1,2 ethohexadiols, Chinese medicine composition；In composition Chinese medicine composition be cloves, radix scutellariae, Chinese cassia tree by Hydrolysis kinetics be made.The production method of the composition is：By caprylhydroxamic acid, 1,2 ethohexadiols, Chinese medicine composition mixing, stirring and dissolving is uniform, you can.It is all that some safe, non-stimulated compounds overcome current preservative and injure big defect to human skin to human skin fanout free region that the composition of the present invention, which has good anti-corrosion effect, raw material used,.In addition, there is the caprylhydroxamic acid in composition good antiallergic, Green Tea Extract effect, 1,2 ethohexadiol also there is good moisture-keeping efficacy, Chinese medicine composition also to have Green Tea Extract, white-skinned face function.
Description
Technical field
The present invention relates to a kind of non-cosmetics preservative composition with preservative efficacy and its applications, belong to cosmetics neck
Domain.
Background technology
China《Cosmetics health specification》（2007）It defines the 67 kinds of preservatives that can be used in cosmetics and its makes
With limitation.Currently, common preservative has p-hydroxybenzoate, imidazolidinyl urea, interior uride, isothiazoline in cosmetics
Ketone, phenoxetol etc..These preservatives have human skin certain injury, easily cause skin allergy.
With the improvement of people's living standards, for cosmetic allergic contact dermatitis problem pay attention to day by day.In order to comply with the consumption of the people
Demand has become hot spot for not adding the research of cosmetics of preservative.But cosmetics are the productions for being very easy to microbiological contamination
How product accomplish anti-corrosionIt can only be screened, be obtained from the non-preservative raw material and natural products for being presently available for cosmetics
To the non-antiseptic composition with preservative efficacy.
Invention content
The purpose of the present invention is exactly the compound with preservative efficacy to be filtered out from common cosmetic material, and carry out excellent
Change combination, a kind of non-stimulated, safe non-antiseptic composition with preservative efficacy is finally provided.
To achieve the object of the present invention, present invention employs following technical solutions：
A kind of non-cosmetics preservative composition with preservative efficacy, it is characterised in that by the group of following weight percent
It is grouped as：Caprylhydroxamic acid 5-20%, 1,2- ethohexadiol 15-30%, Chinese medicine composition 50-80%.
Preferably, a kind of non-cosmetics preservative composition with preservative efficacy, it is characterised in that by following weight hundred
The group of ratio is divided to be grouped as：Caprylhydroxamic acid 15%, 1,2- ethohexadiols 20%, Chinese medicine composition 65%.
Preferably, a kind of non-cosmetics preservative composition with preservative efficacy, it is characterised in that by following weight hundred
The group of ratio is divided to be grouped as：Caprylhydroxamic acid 12%, 1,2- ethohexadiols 24%, Chinese medicine composition 64%.
Preferably, a kind of non-cosmetics preservative composition with preservative efficacy, it is characterised in that by following weight hundred
The group of ratio is divided to be grouped as：Caprylhydroxamic acid 10%, 1,2- ethohexadiols 25%, Chinese medicine composition 65%.
Preferably, a kind of non-cosmetics preservative composition with preservative efficacy, it is characterised in that by following weight hundred
The group of ratio is divided to be grouped as：Caprylhydroxamic acid 16%, 1,2- ethohexadiols 18%, Chinese medicine composition 66%.
Above-mentioned Chinese medicine composition is prepared by following weight percent Chinese medicine：Cloves 15-30%, radix scutellariae 45-75%, Chinese cassia tree 10-
25%.Preparation method is：After cloves, radix scutellariae, Chinese cassia tree are crushed, 40 mesh sieve is crossed, is uniformly mixed, Extraction solvent is added, it is molten with extracting
It after agent impregnates 0.5-2h together, is extracted with high pressure homogenization method machine under room temperature, extracting solution is centrifuged, and is concentrated under reduced pressure
Afterwards, then upper macroreticular resin column purification, collect the ethanol elution part that mass fraction is 30%-80%, be concentrated under reduced pressure into extracting solution with
Quality of medicinal material ratio is 1: 2, and the 1,3-BDO with extracting solution phase homogenous quantities is added, is uniformly dissolved, and Chinese medicine composition is made；It carries
It is water, ethyl alcohol, alcohol-water mixed solution to take solvent.
The preparation method of above-mentioned non-cosmetics preservative composition, it is characterised in that：By caprylhydroxamic acid, 1,2- pungent two
Alcohol, Chinese medicine composition mixing, stirring and dissolving are uniform, you can.
The second object of the present invention is by above-mentioned non-cosmetics preservative composition in cosmetics, it is steady to make property
Fixed, the good cosmetics of anti-corrosion effect.
The second purpose to realize the present invention, present invention employs following technical solutions：By above-mentioned non-cosmetics preservative
Composition is used for preparing cosmetics, it is characterised in that contain above-mentioned non-cosmetics preservative composition in anti-aging cosmetics,
Its dosage is 0.5-15%, preferable amount 2-10%.
The dosage form of cosmetics is not particularly limited, and can be solution, lotion, paste, foundation emulsion, spray, facial mask etc..
The beneficial effects of the invention are as follows：Each ingredient is all not belonging in the composition of the present invention《Cosmetics health specification》
（2007）Specified in preservative, but after optimum organization have good anti-corrosion effect.Raw material used is all makeup
Ingredient is commonly used in product, is that some safe, non-stimulated compounds overcome current preservative to people to human skin fanout free region
The big defect of body skin damage.Particularly, the caprylhydroxamic acid in composition have good antiallergic, Green Tea Extract effect, 1,
Also there is 2- ethohexadiols good moisture-keeping efficacy, Chinese medicine composition also to have Green Tea Extract, white-skinned face function.
Specific implementation mode
Below by way of specific embodiment come the present invention is further illustrated, but these embodiments simply to illustrate that,
It is not limitation of the present invention.
1 non-cosmetics preservative composition of embodiment（Ⅰ）And preparation method thereof
Non- cosmetics preservative composition（Ⅰ）It forms by weight percentage as follows：Caprylhydroxamic acid 15%, 1,2- ethohexadiols
20%, Chinese medicine composition 65%.Wherein Chinese medicine composition is prepared as follows：Cloves 25g, radix scutellariae 60g, Chinese cassia tree 15g are crushed
Afterwards, 40 mesh sieve is crossed, is uniformly mixed, the ethyl alcohol 1kg that mass fraction is 50% is added, after impregnating 1h, high pressure homogenization method is used under room temperature
Machine extracts, and extracting solution is centrifuged, and after reduced pressure, then upper macroreticular resin column purification, collection mass fraction are 50%-
80% ethanol elution part is concentrated under reduced pressure into extracting solution 50g, and 1,3-BDO 50g is added, is uniformly dissolved, and Chinese traditional medicine composition is made
Object.
Composition（Ⅰ）Preparation method is：Caprylhydroxamic acid, 1,2- ethohexadiols, Chinese medicine composition are mixed, stirring and dissolving is equal
It is even, you can.
2 non-cosmetics preservative composition of embodiment（Ⅱ）And preparation method thereof
Non- cosmetics preservative composition（Ⅱ）It forms by weight percentage as follows：Caprylhydroxamic acid 12%, 1,2- pungent two
Alcohol 24%, Chinese medicine composition 64%.Wherein Chinese medicine composition is prepared as follows：By cloves 20g, radix scutellariae 60g, Chinese cassia tree 20g powder
After broken, 40 mesh sieve is crossed, is uniformly mixed, the ethyl alcohol 1kg that mass fraction is 50% is added, after impregnating 1h, carried with high-pressure homogeneous under room temperature
Machine is taken to extract, extracting solution is centrifuged, after reduced pressure, then upper macroreticular resin column purification, collecting mass fraction is
The ethanol elution part of 50%-80% is concentrated under reduced pressure into extracting solution 50g, and 1,3-BDO 50g is added, is uniformly dissolved, and Chinese medicine is made
Composition.
Composition（Ⅱ）Preparation method is：Caprylhydroxamic acid, 1,2- ethohexadiols, Chinese medicine composition are mixed, stirring and dissolving
Uniformly, you can.
3 non-cosmetics preservative composition of embodiment（Ⅲ）And preparation method thereof
Non- cosmetics preservative composition（Ⅲ）It forms by weight percentage as follows：Caprylhydroxamic acid 8%, 1,2- ethohexadiols
28%, Chinese medicine composition 64%.Wherein Chinese medicine composition is prepared as follows：Cloves 28g, radix scutellariae 50g, Chinese cassia tree 22g are crushed
Afterwards, 40 mesh sieve is crossed, is uniformly mixed, the ethyl alcohol 1kg that mass fraction is 50% is added, after impregnating 1h, high pressure homogenization method is used under room temperature
Machine extracts, and extracting solution is centrifuged, and after reduced pressure, then upper macroreticular resin column purification, collection mass fraction are 50%-
80% ethanol elution part is concentrated under reduced pressure into extracting solution 50g, and 1,3-BDO 50g is added, is uniformly dissolved, and Chinese traditional medicine composition is made
Object.
Composition（Ⅲ）Preparation method is：Caprylhydroxamic acid, 1,2- ethohexadiols, Chinese medicine composition are mixed, stirring and dissolving
Uniformly, you can.
Comparative example 1
It forms by weight percentage as follows：Caprylhydroxamic acid 35%, deionized water 65%, mixed dissolution is uniform.
Comparative example 2
It forms by weight percentage as follows：1,2- ethohexadiol 35%, deionized water 65%, mixed dissolution is uniform.
Comparative example 3
It forms by weight percentage as follows：Chinese medicine composition 65%, deionized water 35%, mixed dissolution is uniform.Wherein Chinese medicine
Composition is prepared as follows：Preparation method is：After cloves 20g, radix scutellariae 60g, Chinese cassia tree 20g are crushed, 40 mesh sieve, mixing are crossed
Uniformly, the ethyl alcohol 1kg that mass fraction is 50% is added to be extracted with high pressure homogenization method machine under room temperature after impregnating 1h, extracts
Liquid is centrifuged, after reduced pressure, then upper macroreticular resin column purification, collect the ethanol elution portion that mass fraction is 50%-80%
Point, it is concentrated under reduced pressure into extracting solution 100g, Chinese medicine composition is made.
Comparative example 4
It forms by weight percentage as follows：Caprylhydroxamic acid 15%, 1,2- ethohexadiols 20%, deionized water 65%, mixing are molten
Solution is uniform.
4 skin care cream of embodiment
Table 1 provides the skin care cream formula of the non-cosmetics preservative composition containing the present invention.
Table 1
Preparation method：The 80 DEG C of dissolvings of A phases are uniformly mixed, and the 80 DEG C of dissolvings of B phases are uniformly mixed, cyclomethicone emulsification
Preceding addition B phases, B is added to A phases and homogeneous 5min when emulsification, C phase and homogeneous 2 minutes is added when being cooled to 50 DEG C, after being aged for 24 hours
Packaging, you can.
5 facial treatment milk of embodiment
Table 2 provides the facial treatment milk formula of the non-cosmetics preservative composition containing the present invention, and the dosage of each substance is used
Mass fraction indicates.
Table 2
Preparation method：The 80 DEG C of dissolvings of A phases are uniformly mixed, and the 80 DEG C of dissolvings of B phases are uniformly mixed, cyclomethicone emulsification
Preceding addition B phases, B is added to A phases and homogeneous 5min when emulsification, C phase and homogeneous 2 minutes is added when being cooled to 50 DEG C, after being aged for 24 hours
Packaging, you can.
The preparation of 6 surfactant of embodiment
Table 3 provides the surfactant formula of the non-cosmetics preservative composition containing the present invention, the dosage matter of each substance
Measure fraction representation.
Table 3
Preparation method：Deionized water is heated to 85 DEG C, and hydroxyethyl cellulose is added, and stirring and dissolving is uniform, and 1,2- third is added
Glycol.When stirring is cooled to 50 DEG C, other compositions are added, continues stirring and is cooled to 38 DEG C, you can.
5 common surfactant of comparative example
Table 4 provides the composition without containing the present invention, but the common surfactant formula containing Common Preservatives, each substance
Dosage is indicated with mass fraction.
Table 4
Preparation method：Deionized water is heated to 85 DEG C, and hydroxyethyl cellulose is added, and stirring and dissolving is uniform, and 1,2- third is added
Glycol.When stirring is cooled to 50 DEG C, other compositions are added, continues stirring and is cooled to 38 DEG C, you can.
1 skin irritation evaluation experimental of experimental example
Using 30 women and 20 males as object, takes 30mg samples to be placed in the coyote hole of spot examination adhesive tape, will be equipped with immediately
The spot of sample tries that adhesive tape is longitudinal since lower part to be affixed on the normal skin of left forearm, at the same one by one light pressing room to drive away sky
Gas, and trier is made to be uniformly distributed.Experiment position marks, to observe.It is primary every 24 hours patch skins, after opening patch
Half an hour, then according to CTFA guides（1981）Term checked.6 patch experiments have been carried out altogether, and patch skin terminates
Afterwards the 6th day, in order to observe delayed response, additional inspection is carried out.Data then utilize last time inspection result, are compared
Compared with.It identifies and is carried out for standard with table 5.Substances are respectively the surfactant of embodiment 6 and the common surfactant of comparative example 5, knot
Fruit is as shown in table 6.
Table 5
| Grade | Symbol | Standard of perfection |
| 0 | - | Negative reaction：It is non-stimulated, without erythema |
| 1 | ± | Suspicious reaction：Slight erythema |
| 2 | + | Weakly positive is reacted：Erythema |
| 3 | ++ | Strong positive reaction：Erythema, papule, blister |
| 4 | +++ | Extremely strong positive reaction：Serious edema, bulla |
Table 6
| Lagging number | Comparative example 5 | Blank assay | Embodiment 6 |
| 1 | 1 time ± | 0 | 0 |
| 2 | 0 | 0 | |
| 3 | 0 | 0 | |
| 4 | 1 time ± | 0 | 0 |
| 5 | 0 | 0 | |
| 6 | 0 | 0 | |
| After the 6th day | 1 time ± | 0 | 0 |
| It is total | 3 times ± | 0 | 0 |
By this test result, it can be appreciated that blank assay is non-stimulated, the stimulation of the surfactant of embodiment 6 to skin, and
Still there is the stimulate the reaction of skin in the common surfactant of comparative example 5.Illustrate non-cosmetics preservative group using the present invention
It is smaller than the cosmetics irritation prepared with common preservatives to close cosmetics prepared by object, it is safer.
2 preservation challenge evaluation experimental of experimental example
1, experimental strain
Staphylococcus aureus ATCC 6538（Staphylococcus aureus）
Escherichia coli ATCC 8739 (Escherichia coli)
Pseudomonas aeruginosa ATCC 9027 (Pseudomonas aeruginosa)
Candida albicans ATCC 10231 (candida albicans)
Aspergillus niger ATCC 9029 (black-koji mould)
2, the keeping of experimental strain and condition of culture
（1) bacterium and candida albicans
Culture medium: TSB
Maintaining requirement:4-8 DEG C of refrigeration
Maintaining requirement:2 months
（2) black-koji mould
Culture medium: PDB
Maintaining requirement:4-8 DEG C of refrigeration
Maintaining requirement:2 months
3, experiment bacterium solution manufacturing method
（1) (every gram of the sample of experiment is 10 to bacterium liquid manufacturing method7cfu )
Three kinds of bacteriums and Candida albicans respectively take 50 μ L to be added in the 5mL TSB culture solutions of sterilized processing and are inoculated with,
Then it is cultivated 48 hours in 37 DEG C of shaking tables, obtains the bacterium solution of each bacterium.According to 106, 107,108Three dilutions will with LB culture mediums
It is cultivated, and then confirms the viable count of each bacterium solution.Each bacterium solution takes in the 50mL centrifuge tubes that 1mL is added to and mixes, and obtains mixed bacteria liquid
（The a concentration of of mixed bacteria liquid is preferably controlled in 1.0 × 109Cfu/mL or so）.
（2) (every gram of the sample of experiment is 10 to the production method of fungi liquid5cfu )
By reference culture bacterium（Black-koji mould）It is inoculated on culture medium, is then placed on inside 25 DEG C of incubator and fully trains
After supporting spore, the spore of cultured black is inoculated into platinum oese in culture solution PDB10mL, fully shaking is equal
It is even, then spore is scraped off inside culture medium.After the spore scraped off and fluid nutrient medium are sufficiently mixed, take above
Bacterium solution be collected into centrifuge tube, obtain fungi liquid.By fungi liquid（About 107cfu）It is diluted in as possible after being cultivated on PDA, really
Recognize the bacterium number of survival.
4, experimental method
（1）The preparation of sample
Anticorrosive composite prepared by embodiment 1,2,3 and comparative example 1,2,3,4 is separately added into the formula of table 7, dissolving is equal
It is even that sample is made.
Table 7
（2) bacterium preservative challenge test method
This laboratory reference cosmetics, toilet articles and fragrance association（CTFA）Microbiological test methods are：Add in cosmetics
A certain amount of mixed microorganism bacteria suspension, addition is added to mix bacterium amount and be respectively：Bacterium 3.0 × 107CFU/g (CFU/m1) and mould
1.0×105CFU/g (CFU/m1)）, survival condition of the mixed sample in specific time separation detection observation microorganism：0 is small
When (inoculation after at once sample), 7 days, 14 days, 21 days and 28 days result it is required that bacterium reduction by 99.9% at the 7th day, mould
Bacterium reduces by 90%；And continuous decrease is zero to judge the anti-corrosion effect of preservative, specific judging result reference in 28 days
Table 8.
Table 8
| Strain name | 0d | 7d | 14d | 21d | 28d |
| Fungi (cfu/g) | 1.0×105 | ≤100 | 0 | 0 | 0 |
| Bacterium (cfu/g) | 3.0×107 | 0 | 0 | 0 | 0 |
5, result
It the results are shown in Table shown in 9.
Table 9
As shown in Table 9, the sample made of embodiment 1,2,3 passed preservation challenge test, have potent anti-corrosion
Effect.Over time, bacterium and total number of fungi have decline to the sample that comparative example 1,2,3 makes, and illustrate to have certain
Anti-corrosion effect, but do not tested by preservation challenge.
In addition, being also seen that the anti-corrosion effect of comparative example 4 is got well than the anti-corrosion effect of comparative example 1,2 by table 9, illustrate pungent
Acyl hydroxamic acid can improve anti-corrosion effect with 1,2- ethohexadiols compounding.And by caprylhydroxamic acid, 1,2- ethohexadiols, Chinese medicine composition
Anti-corrosion effect of the embodiment 1,2,3 than comparative example 1,2,3,4 after three kinds of substances are compounded by science is much better；Illustrate three
Compounding plays synergistic function, improves anti-corrosion ability.
Claims (2)
1. a kind of non-cosmetics preservative composition with preservative efficacy, it is characterised in that by following weight percentage components
Composition：Caprylhydroxamic acid 5-20%, 1,2- ethohexadiol 15-30%, Chinese medicine composition 50-80%；The Chinese medicine composition is by such as
It is prepared by lower weight percent Chinese medicine：Cloves 15-30%, radix scutellariae 45-75%, Chinese cassia tree 10-25%；The preparation side of the Chinese medicine composition
Method is：After cloves, radix scutellariae, Chinese cassia tree are crushed, 40 mesh sieve is crossed, is uniformly mixed, Extraction solvent is added, is impregnated together with Extraction solvent
After 0.5-2h, being extracted with high pressure homogenization method machine under room temperature, extracting solution is centrifuged, after reduced pressure, then upper macropore
Resin column purification collects the ethanol elution part that mass fraction is 30%-80%, and be concentrated under reduced pressure into extracting solution is with quality of medicinal material ratio
1: 2, the 1,3-BDO with extracting solution phase homogenous quantities is added, is uniformly dissolved, Chinese medicine composition is made；Extraction solvent is water, second
Alcohol, alcohol-water mixed solution.
2. a kind of non-cosmetics preservative composition answering in preparing cosmetics with preservative efficacy described in claim 1
With, it is characterised in that in cosmetics contain a kind of above-mentioned non-cosmetics preservative composition with preservative efficacy, dosage with
Mass fraction is calculated as 0.5-15%.
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| CN107308064A (en) * | 2017-08-08 | 2017-11-03 | 广州蜜妆生物科技有限公司 | A kind of compound natural preservative |
| CN114344226B (en) * | 2022-02-25 | 2023-03-17 | 河南科技大学 | Traditional Chinese medicine preservative, preparation method and application |
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| CN101773462A (en) * | 2010-03-03 | 2010-07-14 | 太原博义医药科技开发有限公司 | Chinese herbal skin care type natural bacteriostatic hand sanitizer and preparation method thereof |
| CN103432047A (en) * | 2013-09-12 | 2013-12-11 | 广东轻工职业技术学院 | Natural preservative composition and application thereof in cosmetics |
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| US8993641B2 (en) * | 2007-11-29 | 2015-03-31 | Innolex Investment Corporation | Preservation of cosmetics, toiletry and pharmaceutical compositions |
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| CN101773462A (en) * | 2010-03-03 | 2010-07-14 | 太原博义医药科技开发有限公司 | Chinese herbal skin care type natural bacteriostatic hand sanitizer and preparation method thereof |
| EP2807925A1 (en) * | 2013-05-26 | 2014-12-03 | Symrise AG | Antimicrobial compositions |
| CN103432047A (en) * | 2013-09-12 | 2013-12-11 | 广东轻工职业技术学院 | Natural preservative composition and application thereof in cosmetics |
| KR20150049027A (en) * | 2013-10-29 | 2015-05-08 | 주식회사 제닉 | Composition of preservatives and cosmetic composition comprising the same |
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