WO2019047004A1 - 一种天然替代的植物精油防腐剂及在化妆品中的应用 - Google Patents

一种天然替代的植物精油防腐剂及在化妆品中的应用 Download PDF

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WO2019047004A1
WO2019047004A1 PCT/CN2017/100495 CN2017100495W WO2019047004A1 WO 2019047004 A1 WO2019047004 A1 WO 2019047004A1 CN 2017100495 W CN2017100495 W CN 2017100495W WO 2019047004 A1 WO2019047004 A1 WO 2019047004A1
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oil
preservative
essential oil
weight
essential
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PCT/CN2017/100495
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English (en)
French (fr)
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赵文忠
洪盛杰
林学镁
谷志静
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拉芳家化股份有限公司
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Priority to CN201780004913.2A priority Critical patent/CN108697629B/zh
Priority to PCT/CN2017/100495 priority patent/WO2019047004A1/zh
Publication of WO2019047004A1 publication Critical patent/WO2019047004A1/zh

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    • 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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • 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
    • 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
    • A61K8/342Alcohols having more than seven atoms in an unbroken chain
    • 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
    • A61K8/347Phenols
    • 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
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • 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
    • A61K2800/10General cosmetic use
    • 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

Definitions

  • the invention belongs to the field of daily chemistry and relates to a natural substitute plant essential oil preservative.
  • the invention also relates to the use of the preservative in cosmetics.
  • cosmetic manufacturers and cosmetic formulators need to pay attention to whether the preservatives used in cosmetics are potentially toxic, whether they have an allergic reaction to the skin, whether they are facing the risks of current or future regulations, etc. during product development and production. Column problem. Therefore, in the front-end research and development of cosmetics production, formulators should not only carefully screen the raw materials of cosmetic carriers, such as whether the raw materials used are listed in the Catalogue of Used Cosmetics 2015, if there is any cosmetic raw materials. Safety data, etc., and a more important consideration is whether the preservative or bactericide selected by a certain formula meets the requirements of the cosmetics safety regulations, and whether it conforms to the trend of domestic and international mainstream regulations, specifically in cosmetics.
  • the application in the formula must also consider the effectiveness of the preservative in dealing with the following four common bacteria: (1) mold such as Aspergillus, (2) yeast such as Candida albicans, (3) Gram-positive bacteria such as Staphylococcus aureus (4) Gram-negative bacteria such as Pseudomonas aeruginosa.
  • mold such as Aspergillus
  • yeast such as Candida albicans
  • Gram-positive bacteria such as Staphylococcus aureus
  • Gram-negative bacteria such as Pseudomonas aeruginosa.
  • Another object of the invention is to provide the use of the preservative in cosmetics.
  • the object of the present invention is achieved by a natural alternative plant essential oil preservative consisting of a compound plant essential oil and an active substance, the components and the percentage by weight of which are as follows:
  • the technical solution of the present invention comprises the preservative, and further comprises a monovalent glycerol monoglyceride in an amount of 1-0.8% by weight of the preservative.
  • a natural alternative plant essential oil preservative the composition and weight percentage of which are as follows:
  • the preservative of the present invention is useful for inhibiting Aspergillus niger, Candida albicans, Staphylococcus aureus and Pseudomonas aeruginosa in cosmetics.
  • the present invention has the following advantages:
  • a natural alternative preservative composition of the present invention consisting of a compound plant essential oil having an antibacterial action and an active substance, the natural substitute preservative composition being effective against microorganisms commonly encountered in cosmetics (1) molds such as black koji Mold, (2) yeast such as Candida albicans, (3) Gram-positive bacteria such as Staphylococcus aureus, (4) Gram-negative bacteria such as Pseudomonas aeruginosa.
  • the natural replacement preservative composition of the present invention is effective for inhibiting and killing microorganisms within 72 hours in a cosmetic emulsion formulation containing no other chemical preservative at a weight percentage of 2%.
  • Natural plant essential oils are a large class of substances.
  • Essential oils also known as “aromatic oils” are oily substances with characteristic aromas obtained from certain parts of aromatic plants such as roots, skins, stems, branches, fruits, seeds, etc., which are then subjected to distillation and extraction. In general, it mainly contains olefins, aromatic hydrocarbons, alcohols, aldehydes, ketones, ethers, esters and phenols. Among them, terpenoids and their derivatives are the most common.
  • Leaf alcohol is shown in Formula III as a non-cyclic monoterpene alcohol compound.
  • the above three active ingredients belong to some terpene alcohols which may be contained in some plant essential oils.
  • Terpene alcohols have certain antibacterial activity, which can cause microbial cell membrane deformation and affect its permeability change.
  • the hydrophobic properties of the essential oils allow it to penetrate and dissolve into the cell membrane of the microorganism and destroy the function of the fungus.
  • plant essential oils act as antibacterial agents by interfering with and destroying phospholipid biofilms of microbial cells, enzyme activities and genetic resources.
  • the essential oils with high phenolic compounds in plant essential oils also exhibit relatively high antibacterial activity.
  • the carvacrol present in thyme oil is shown in formula IV, and the eugenol present in clove oil is shown in formula V.
  • 2- Isopropyl-5-methylphenol see Formula VI is a naturally occurring active substance with good antibacterial and antioxidant functions.
  • This active substance is present in thyme oil, also known as thymol
  • 2-isopropyl- 5-Methylphenol (Thymol) is a monoterpene which is a phenol derivative of p-isopropyltoluene (p-salt). Its molecular formula is C10H14O, which is an isomer with carvacrol.
  • Other essential oils containing relatively high phenolic substances include oregano, rosemary, sage, and the like.
  • terpinen-4-ol also known as 4-terpineol.
  • Linalool extracted from eucalyptus oil and eucalyptus oil is an essential oil active.
  • Geraniol extracted from natural essential oils such as rose essential oil, horse clove oil and citronella oil is an essential oil active.
  • Carvacrol is an isomer of thymol, which is similar to thymol, so it is also called iso thymol. Carvacrol is naturally present in essential oils such as thyme oil and is an essential oil active.
  • 2-isopropyl-5-methylphenol is an essential oil active found in thyme essential oils, also known as thymol. Its chemical name is as above, and Thymol is a monoterpene which is a phenol derivative of p-isopropyltoluene. Its molecular formula is C10H14O, which is an isomer with carvacrol.
  • the microorganism of the present invention adopts the Chinese Industrial Microbial Culture Collection Management Center CICC or the American Type Culture Collection ATCC strain, and the required experimental sample contains aspergillus niger Aspergillus sp. ATCC 10864, candida albicans Candida albicans Staphyloccus aureus Staphylococcus aureus ATCC 25923 and pseudamonas aeruginosa Pseudomonas aeruginosa ATCC 27853.
  • Antibacterial evaluation method Determination of antibacterial efficacy - Oxford Cup method, this method is a general method for testing antibiotic titer at home and abroad, and is also a method prescribed by national pharmacopoeia.
  • the Oxford Cup containing the bacteriostatic drug was placed on the agar plate that had been inoculated with the test bacteria, and the drug contained in the Oxford Cup continued to spread around the Oxford Cup. A decreasing gradient concentration is formed.
  • the growth of the test bacteria in the range of inhibitory concentrations around the Oxford Cup is inhibited, forming a sterile growing transparent circle (ie, the zone of inhibition).
  • the size of the inhibition zone reflects the sensitivity of the test bacteria to the measured drug, and the minimum inhibitory concentration (MIC) of the drug to be tested.
  • the inhibition zone diameter ⁇ 20mm is extremely sensitive "+++” is judged to have antibacterial effect, the inhibition zone is larger, the antibacterial effect is better; 15mm ⁇ antibacterial diameter ⁇ 20mm is high sensitivity "++ "; 10mm ⁇ antibacterial diameter ⁇ 15mm for the medium sensitive "+”; antibacterial diameter ⁇ 10mm is invalid, was judged as no bacteriostatic effect. Those who had bacteriostatic results in 3 repeated tests were judged as qualified. The negative control group had no inhibition zone, otherwise the test was ineffective.
  • Essential oils and actives are essential oils such as cinnamon oil, rosemary oil, cedar oil, lemongrass essential oil, neroli essential oil, peppermint oil, clove oil, thyme essential oil and geranium essential oil; essential oil actives such as linalool and parsley There are 15 kinds of phenol, geraniol, syringol, eugenol and 2-isopropyl-5-methylphenol.
  • MIC Minimum inhibitory concentration test
  • agar medium dilution method is used to add 0.5% by volume of Tween-20 to the agar in order to increase the tested essential oil or active substance.
  • Solubility Each essential oil or active is prepared as a series of 2-fold dilutions ranging from 0.2 mg/ml to 25.6 mg/ml.
  • the surface dish is dried at room temperature for 30 minutes and then inoculated with 3 PPM of medium.
  • Each microorganism contains 10 5 CFU/ml colony number. Inoculate at 37 ° C for 18 hours, and calculate the MIC. The experiment is performed in triplicate.
  • the surface dish containing essential oil and active substance is compared with the blank to observe the inhibition of bacteria and observe the minimum inhibition of essential oils and active substances.
  • concentration of the above 15 plant essential oils and essential oil actives has good antibacterial activity
  • selected 12 plant essential oils and their actives are essential oils such as cinnamon oil, rosemary oil, cedar oil, lemon Grass oil, neroli essential oil, peppermint oil, clove oil, geranium essential oil and thyme essential oil; and essential oil actives such as linalool, geraniol, 2-isopropyl-5-methylphenol.
  • the present invention has been experimentally and researched and found that among the known plant essential oils having bacteriostatic effects, their antibacterial properties are strong and weak, some have good effects on inhibiting fungi, and some have good effects on inhibiting bacteria.
  • the inhibitory effect on Gram-positive bacteria is higher than that of Galanz-negative bacteria.
  • suitable essential oils and essential oil active substances are combined in an appropriate weight percentage to form a compound preservative and an active preservative (corresponding to a combination of a combination of essential essential oils and active substances) and used in cosmetics.
  • the preservative composition was established, and the weight percentage of the compound essential oil and its active preservative in the cosmetic was controlled as much as 2%.
  • Tween-20 essential oil (active) was weighed in a weight ratio of 3:1, and then Tween-20 was added to the essential oil to form a mixture, which was then taken to contain 0.5%, 1%, 1.5%, 2.0%, 2.5. %, 3.0% of essential oil or active substance (the essential oil carrier or solvent is jojoba oil, essential oil or active substance can be dissolved first with jojoba oil, for example 2% rosemary essential oil composition, 2 grams of rosemary essential oil +98 g of jojoba oil), add 10 ml of petri dish containing sterile medium, and mix by shaking.
  • the essential oil carrier or solvent is jojoba oil, essential oil or active substance can be dissolved first with jojoba oil, for example 2% rosemary essential oil composition, 2 grams of rosemary essential oil +98 g of jojoba oil
  • the four cultured microorganisms Aspergillus niger, Candida albicans, Staphylococcus aureus and Pseudomonas aeruginosa were respectively dropped into the above-mentioned culture dish containing a single essential oil, Tween-20 and medium, in which each microorganism was dropped.
  • the liquid contains approximately 1 million microorganisms.
  • the culture dish is then shaken and placed under a constant temperature of 37 ° C for 72 hours. Then observe the growth of the microorganisms. The more the microorganisms grow, the worse the antibacterial effect of the essential oils and active preservatives.
  • the four cultured microorganisms Aspergillus niger, Candida albicans, Staphylococcus aureus and Pseudomonas aeruginosa are respectively dropped into liquid form with different contents.
  • Preservatives consisting of a combination of essential oils and actives (12 essential oils and actives) (see Table 1), Tween-20 and medium culture dishes, including 12 essential oils in the essential oils and actives.
  • An active wherein each drop of microbial liquid contains about 1 million microorganisms.
  • the culture dish was then shaken and placed under a constant temperature of 37 ° C for 72 hours, and then the growth of the microorganisms was observed.
  • the compound essential oil and active preservative composition of the invention is divided into 8 systems, each antiseptic system is equivalent to a preservative composition, and the weight percentage of each of the 12 plant essential oils and active substances in each preservative composition is according to the respective minimum
  • the bacterial concentration MIC is used to determine the weight percentage of 12 plant essential oils and actives.
  • jojoba oil is a carrier oil for plant essential oils and active substances, and monosilicic acid monoglyceride functions as a dispersing, dissolving and emulsifying function in the respective preservative compositions.
  • lemon grass essential oil accounts for 1-12% by weight of the preservative composition
  • rosemary essential oil accounts for 0.5-5% by weight of the preservative composition
  • neroli essential oil accounts for 0.5% by weight of the preservative composition.
  • peppermint oil accounts for 0.5-5% by weight of the preservative composition
  • geranium essential oil accounts for 0.1-0.8% by weight of the preservative composition
  • the preservative composition is present in an amount of from 0.05% to 1.5% by weight, and the balance of the preservative composition is supplemented with jojoba oil.
  • the compound essential oil and the active preservative composition (1) of the 12 plant essential oils and active substances are obtained through the compound essential oil and the active substance bacteriostatic test.
  • (8) When the bacteriostatic experiments were carried out in the examples (1) to (8), respectively, 0.5%, 1.0%, and 2.0%, and the composition of each agent was found to be against the four cultured microorganisms Aspergillus niger and Candida albicans. Staphylococcus aureus and Pseudomonas aeruginosa showed different degrees of bacteriostatic effects.
  • the plant essential oils in the above preservative composition are, for example, cinnamon oil, rosemary oil, cedar oil, lemongrass essential oil, neroli essential oil, peppermint oil, clove oil, geranium essential oil, thyme essential oil and essential oil actives such as geranium Alcohol, 2-isopropyl-5-methylphenol, linalool are commercially available pure plant essential oils and actives thereof. These plant essential oils and actives have bactericidal and bacteriostatic effects, in addition, one month
  • the glyceryl silicate acts as an emulsified and dispersed essential oil in the preservative composition of the present invention.
  • Monovalent glyceryl silicate chemical name 2,3-dihydroxypropanol dodecanoate (formula VII), also known as dodecanoic acid monoglyceride
  • formula VII also known as dodecanoic acid monoglyceride
  • the lauric acid monoglyceride is directly esterified by lauric acid and glycerin, and the appearance is generally scaly or oily, white or light yellow fine granular crystal.
  • the single-month glyceryl acrylate has a parental structure with a molecular weight of 274.21, and the presence of the lauric acid carbon chain has the effects of sterilization and bacteriostasis. Therefore, the single-month glyceryl acrylate is both an emulsifying and dispersing agent, and It is a bactericide, and in the present invention, it mainly plays the role of emulsification and dispersion of essential oils and has synergistic antibacterial effect.
  • the weight percentage of the glycerol monolaurate to the preservative composition of the present invention is further optimized to be from 0.1 to 0.8%.
  • the jojoba oil is a carrier oil of the plant essential oil in the present invention, which is a non-aromatic plant essential oil, and the jojoba oil is used up to 100% in the 1 to 8 preservative composition.
  • Table 1 Compound plant essential oils and active preservative compositions Examples 1 to 8
  • the monovalent glyceryl silicate acts as an emulsified and dispersed essential oil in the preservative composition of the present invention.
  • Jojoba oil is a carrier oil of plant essential oil in the present invention, and is a non-aromatic plant essential oil.
  • preservative compositions 1 to 8 preservative compositions (see Table 1), respectively, are 0.5%, 1%, 1.5%, 2.0%, 2.5%, 3.0% by weight, respectively. Antibacterial effect. Among them, Examples 6, 7, and 8 of the preservative composition are preferred.
  • an optimized compound essential oil and an active preservative composition thereof are selected from the examples of the 1 to 8 preservative composition, and the preservative composition is capable of treating the four microorganisms within 72 hours.
  • Maximum inhibitory effect (Aspergillus niger, Candida albicans, Staphylococcus aureus and Pseudomonas aeruginosa), in addition to comprehensive cost-effectiveness and mildness, the compound essential oil and active preservative composition is a preservative combination Example 6 (see Table 2)
  • the preservative composition 6 showed good inhibition and killing effects on four microorganisms at 72% by weight in an amount of 2% by weight.
  • the ingredients in the cleansing cream formula such as cationic guar gum are guar hydroxypropyltrimonium chloride, potassium stearate and sodium cocoyl isethionate are blowing agents and detergents, glycerin As a moisturizer, allantoin is an anti-allergic agent, monoglyceride, stearic acid, cetostearyl alcohol as emulsifier and emulsified thickener, octanoic acid/triglyceride as emollient, vitamin E acetic acid
  • the ester is an antioxidant
  • the combination essential oil and the active preservative composition 6 are preferred preservative compositions of the invention
  • Tween-20 is a solubilizing agent. All of the above materials are cosmetic grade materials and are known to those skilled in the art and are commercially available. Tween-20 and compound essential oil and active preservative composition 6 were mixed and added at a weight ratio of 3:1.
  • Premixing and dissolving of the preservative composition The Tween-20 is added to the essential oil and the active preservative composition 6 to be stirred and dissolved, and used.
  • step 75 degrees Celsius, add the substance of step 2 to step 1, stir until the emulsion is emulsified evenly, and then start to cool down to 40 degrees Celsius.
  • step 3 preservative premix is added to the material of step 4 and stirred until the preservative composition is homogeneous.
  • a lotion formula is as follows:
  • the ingredients in the moisturizer formula are guar hydroxypropyltrimonium chloride, which acts to thicken, potassium 12-alkyl phosphate and mono-glycol, cetostearyl alcohol Stearic acid is an emulsifier and an emulsion stabilizer, octanoic acid/sodium triglyceride and white oil are emollients, glycerin is a moisturizer, allantoin is an anti-allergic agent, and vitamin E acetate is an antioxidant.
  • Essential Oils and Active Preservative Compositions 6 are preferred preservative compositions of the present invention, and Tween-20 is a solubilizing agent for the preservative compositions of the present invention. All of the above materials are cosmetic grade materials and are commercially available from those skilled in the art. Tween-20 and compound essential oil and active preservative composition 6 were mixed and added at a weight ratio of 3:1.
  • Premixing and Dissolving of Preservative Composition Tween-20 is added to the compound essential oil and the active preservative composition 6 to be stirred and dissolved, and used.
  • B is added to A, stirred until the emulsion is uniformly emulsified, then cooled while stirring, and triethanolamine is added when the temperature is lowered to 60 degrees Celsius, and stirring is continued.
  • the pre-mixed C preservative composition is added to D in a long time and stirred for 15-30 minutes until the preservative composition is homogeneous.
  • the lotion (1) and the lotion (2) were placed in four sizes of 150 mm. In the culture dish, four kinds of microorganisms of about 1 million counts were placed in each of the four culture dishes, and 1 gram of the inoculated product was diluted with 9 ml of the sterile diluent, cultured, observed, and found to be moist after 5 days. The microorganisms of the formula (1) and the lotion formula (2) were reduced from the initial 1.5*10 6 to ⁇ 10. See Table 6
  • the present invention has the following advantages:
  • a natural alternative preservative composition of the present invention consisting of a compound plant essential oil having an antibacterial action and an active substance, the natural replacement preservative composition being effective against microorganisms commonly encountered in cosmetics (1) Molds such as Aspergillus, (2) yeast such as Candida albicans, (3) Gram-positive bacteria such as Staphylococcus aureus, (4) Gram-negative bacteria such as Pseudomonas aeruginosa.
  • the natural replacement preservative composition of the present invention is effective for inhibiting and killing microorganisms within 72 hours in a cosmetic emulsion formulation containing no other chemical preservative at a weight percentage of 2%.

Abstract

一种天然替代的植物精油防腐剂,由复方植物精油及活性物组成,其组分及重量百分比含量为:占防腐剂重量百分比为2-17%的芳樟醇(含量比下同)、0.5-5%的香叶醇、2-20%的百里香精油、0.5-6%的丁香油、0.1-0.8%的2-异丙基-5-甲基苯酚、0.1-2%的桂皮精油、2-19%的香柏精油、1-12%的柠檬草精油、0.5-5%的迷迭香精油、0.5-5%的橙花精油、0.5-5%的薄荷油、0.1-0.8%的天竺葵精油、0.05-1.5%的单月桂酸甘油酯和余量的霍霍巴油。所述防腐剂在化妆品抑制黑曲霉菌、白色念珠菌、金黄色葡萄球菌和绿脓杆菌中应用。所述防腐剂不含其它化学防腐剂,在化妆品乳液配方中能有效抑制并杀灭其中的微生物。

Description

一种天然替代的植物精油防腐剂及在化妆品中的应用 技术领域
本发明属日化领域,涉及一种天然替代的植物精油防腐剂。
本发明还涉及该防腐剂在化妆品中的应用。
背景技术
在日化领域,有关化妆品配方的研发和生产一直离不开一个重要的技术环节,那就是配方防腐的研究及应用。因此化妆品配方设计中将考虑一系列的防腐杀菌剂并用于有效对抗微生物。目前化妆品所使用的防腐剂和杀菌剂如卡松,DMDMH,尼泊金酯类等大都是化学合成的化合物成份。虽说这些化学合成的防腐剂在法规规定的用量下是安全的,但在全球化妆品走向天然有机的大背景下,这些合成类的防腐剂愈来愈面临着诸多的来自消费者和科学研究领域的质疑。各国尤其是来自美国和欧盟的化妆品法规也愈来愈提出更严格的防腐剂使用标准。因此,化妆品生产制造商和化妆品配方师在产品研发和生产过程中需要时常关注化妆品所采用的防腐剂是否有潜在的毒性,是否会对皮肤产生过敏反应,是否面临当下或未来法规的风险等一些列问题。因此,在化妆品生产的前端研发环节,配方师不但要对化妆品载体原料经过认真的筛选如,所使用原料是否在《已使用化妆品目录2015》中有载录,如有载录是否有化妆品原料的安全数据等,还有一个更重要的考量点是某一个配方所选择的防腐剂或杀菌剂是否符合化妆品安全规范的要求,是否符合国内外主流法规的走向,具体到在化妆品 配方中的应用还必须考虑防腐剂应对如下四种常见菌的有效性(1)霉菌如黑曲霉菌,(2)酵母菌如白色念珠菌,(3)革兰氏阳性菌如金黄色葡萄球菌,(4)革兰氏阴性菌如绿脓杆菌。
发明内容
本发明的目的是提供一种天然替代的植物精油防腐剂。
本发明的另一目的提供该防腐剂在化妆品中的应用。
本发明的目的是这样实现的:一种天然替代的植物精油防腐剂,由复方植物精油及活性物组成,其组分及重量百分比含量如下:
(a)占防腐剂重量百分比为2-17%的芳樟醇,
(b)占防腐剂重量百分比为0.5-5%的香叶醇,
(c)占防腐剂重量百分比为2-20%的百里香精油,
(d)占防腐剂重量百分比为0.5-6%的丁香油,
(e)占防腐剂重量百分比为0.1-0.8%的2-异丙基-5-甲基苯酚,
(f)占防腐剂重量百分比为0.1-2%的桂皮精油,
(g)占防腐剂重量百分比为2-19%的香柏精油,
(h)占防腐剂重量百分比为,1-12%的柠檬草精油,
(i)占防腐剂重量百分比为0.5-5%的迷迭香精油,
(j)占防腐剂重量百分比为0.5-5%的橙花精油,
(k)占防腐剂重量百分比为0.5-5%的薄荷油,
(l)占防腐剂重量百分比为0.1-0.8%的天竺葵精油,
(m)占防腐剂重量百分比为0.05-1.5%的单月硅酸甘油酯,
(n)余量的霍霍巴油。
本发明技术方案包括所述的防腐剂,还含有占防腐剂重量百分比1-0.8%的单月硅酸甘油酯。
一种天然替代的植物精油防腐剂,其组分及重量百分比含量如下:
组分 含量 重量(%)
芳樟醇 15
香叶醇 4
百里香精油 18
丁香油 5
2-异丙基-5-甲基苯酚 0.6
桂皮精油 1.5
香柏精油 19
柠檬草精油 10
迷迭香精油 4.5
橙花精油 4.5
薄荷油 4.5
天竺葵精油 0.6
月硅酸单甘油酯 0.6
霍霍巴油 加至100%
本发明所述防腐剂在化妆品抑制黑曲霉菌、白色念珠菌、金黄色葡萄球菌和绿脓杆菌中的应用。
与现有技术相比,本发明具有以下优点:
1、本发明一种天然替代防腐剂组合物是由具有抑菌作用的复方植物精油及活性物组成,该天然替代防腐剂组合物能有效对抗抗化妆品中常见的微生物(1)霉菌如黑曲霉菌,(2)酵母菌如白色念珠菌,(3)革兰氏阳性菌如金黄色葡萄球菌,(4)革兰氏阴性菌如绿脓杆菌。
2、本发明天然替代防腐剂组合物,以2%的重量百分比用于不含其它化学防腐剂的化妆品乳液配方中能在72小时内有效抑制并杀灭其中的微生物。
具体实施方式
下面结合实施例对本发明作进一步的详细说明。
为了获得安全与有效的化妆品防腐剂,工程师们一直研究将天然来源的物质用于化妆品的防腐以期获得防御和杀灭微生物的效果,天然植物精油就是其中的一大类物质。
精油也称为“芳香精油”,是从芳香植物体的某个部位如,根、皮、茎、枝、果实、种子等采取,然后经过蒸馏提取等方法制得的具有特征香气的油状物质的总称,主要含有萜烯烃类,芳香烃类、醇类、醛类、酮类、醚类、酯类和酚类等化合物,其中以萜类化合物及其衍生物最为常见。
精油品种有3000种以上,其中有商业价值约百种。人类使用植物精油如在医药,食品储存以及个人护理方面的应用已经有上千年的历史,人们对于植物精油的科学研究也从来没有停止过,除了芳香疗法之外,植物精油在防腐和抗菌方面的研究与应用具有可深究的潜力,精油及精油中所含有的活性成份及化学结构与精油的抑菌能力有直接关联性。根据文献《精油的化学表征与抗菌特性》巴西微生物学杂志ISSN 1517-8382,Braz.J.Microbiol.vol.42no.4 
Figure PCTCN2017100495-appb-000001
 Paulo Oct./Dec.2011,的研究,植物精油抑菌的机理在于其能够改变微生物细 胞膜的结构和功能,如马郁兰精油中含有的主要活性成份松油烯-4-醇,又名4-萜烯醇见式Ⅰ属于链状萜烯醇类,从芳樟木油,芳樟叶油中提取的芳樟醇见式Ⅱ,以及从玫瑰油、马丁香油和香茅油等天然精油中提取的香叶醇见式Ⅲ是一个非环单萜醇类化合物。上述三种活性成份均属于一些植物精油中可以含有的萜烯醇类物质。萜烯醇类物质具有一定的抗菌活性,能致使微生物细胞膜变形进而影响其渗透性的变化。此外,精油的疏水特性能使其渗透并溶入微生物的细胞膜并使菌类功能遭到破坏。概况一句话,植物精油是通过干扰与破坏微生物细胞的磷脂生物膜,酶活性和基因资源起到抑菌作用的。植物精油中酚类化合物含量高的精油也呈现出相对较高的抑菌活性,存在于百里香油中的香芹酚见式Ⅳ,存在于丁香油中的丁香酚见式Ⅴ,此外,2-异丙基-5-甲基苯酚见式Ⅵ是一种天然存在的具有较好抗菌和抗氧化功能的活性物,该活性物存在于百里香油中,也叫百里香酚,2-异丙基-5-甲基苯酚(百里香酚Thymol)是一个单萜,是对异丙基甲苯(对撒花烃)的酚衍生物。其分子式为C10H14O,与香芹酚是同分异构体。其它含有比较高的酚类物质的精油还包括牛至,迷迭香,鼠尾草等。
Figure PCTCN2017100495-appb-000002
式Ⅰ 4-萜烯醇化学结构式
马郁兰精油中含有的主要活性成份为松油烯-4-醇,又名4-萜烯醇(4-terpineol)
Figure PCTCN2017100495-appb-000003
式Ⅱ 芳樟醇化学结构式
从芳樟木油,芳樟叶油中提取的芳樟醇(Linalool)为精油活性物。
Figure PCTCN2017100495-appb-000004
式Ⅲ 香叶醇化学结构式
从玫瑰精油、马丁香油和香茅油等天然精油中提取的香叶醇(Geraniol)为精油活性物。
Figure PCTCN2017100495-appb-000005
式Ⅳ 香芹酚化学结构式2-甲基-5-异丙基苯酚
香芹酚是百里香酚的同分异构体,香气与百里香酚类似,故又称为异百里香酚。香芹酚天然存在于百里香油等精油中,为精油活性物。
Figure PCTCN2017100495-appb-000006
式Ⅴ 丁香酚化学结构式
从丁香油、丁香罗勒油以及肉桂油等精油中提取获得,化学名为2-甲氧基-4-(2-丙烯基)苯酚(EUGENOL),为精油活性物。
Figure PCTCN2017100495-appb-000007
式Ⅵ 2-异丙基-5-甲基苯酚化学结构式
2-异丙基-5-甲基苯酚为精油活性物,存在于百里香精油中,也叫百里香酚。其化学名称为如上式,百里香粉(Thymol)是一个单萜,是对异丙基甲苯(对撒花烃)的酚衍生物。其分子式为C10H14O,与香芹酚是同分异构体。
此外,在个人护理方面。许多国内外科学文献的报道如,柯克-奥思默Kirk-Othmer百科全书中对精油的组成及生产有描述,以及《植物精油对微生物的抑菌效果评估研究》食品科学2008 Vol 209,No.12,p83-86,一些植物精油能有效对抗通常涉及的微生物如,黑曲霉菌,白色念珠菌,金黄色葡萄球菌和绿脓杆菌四种微生物等方面的文献。
根据柯克-奥思默Kirk-Othmer百科全书中对精油的记载以及《植物精油对微生物的抑菌效果评估研究》食品科学2008 Vol 209,No.12,p83-86,所记载植物精油的抑菌研究,以及国内外植物精油相关抑菌杀菌文献的记录,目前可能具有抑菌和杀菌效果的植物,精油及源于精油的活性物大约有:罗勒,芳樟木 油,芳樟叶油,伽罗木油、玫瑰木油、天竺葵精油,胡荽子油,雪松,肉桂,桂皮油,香茅,丁香叶,香柏油,丝柏,尤加利,茴香,天竺葵,姜,薰衣草,肉豆蔻,甜橙,广藿香,欧薄荷,迷迭香油,檀香,茶树,月桂,樟树,芹菜,橄榄油,桔油,山鸡椒,松树,冬青,白兰花,依兰,茶树溶水油,马乔莲(牛至),芫荽籽精油,柠檬桉叶油,山苍子油,薄荷油,艾草,巴西玫瑰木油,香菜,豆蔻,柏木油,桂皮油,芫荽,龙蒿油,甜茴香油,柠檬草油,香茅醇(玫瑰草油等中提取),杜松子油,芳樟醇(巴西玫瑰木油,芳樟油中提取),马乔莲,薄荷脑,橙花油,栎扁枝衣,玫瑰奥托油,百里香油,香子兰,冬青油,香叶醇,香芹酚,百里香精油,2-异丙基-5-甲基苯酚(百里香精油中提取),丁香油酚,多香果精油,苦杏仁油,杂醇油,西班牙胡薄荷油,山苍子油,圆叶当归精油,布枯叶油,芳樟醇,羟基香茅醛(桉树中提取),金雀花油,羟基香茅醛(提取自香茅油),异丁香酚,霍霍巴油,萜烯醇等等80多种,其中橄榄油和霍霍巴油为植物精油的载体油脂。
具有杀菌抑菌效果的植物精油及其活性物的筛选:
实验用微生物:本发明微生物采用中国工业微生物菌种保藏管理中心CICC或美国典型培养物保藏中心ATCC菌种,所需实验用样品包含aspergillus niger黑曲霉菌ATCC 10864,candida albicans白色念珠菌
Figure PCTCN2017100495-appb-000008
staphyloccus aureus金黄色葡萄球菌ATCC 25923和pseudamonas aeruginosa绿脓杆菌ATCC 27853。
具有较优抑菌效果的植物精油及活性物的筛选。
抗菌评价方法:抑菌效力的测定—牛津杯法,此方法是国内外检验抗生素效价的通用方法,也是各国药典规定的方法。将含有定量抑菌药物的牛津杯放在已接种待检菌的琼脂平板上,牛津杯中所含的药物不断向牛津杯周围扩散, 形成递减的梯度浓度。在牛津杯周围抑菌浓度范围内待检菌的生长被抑制,形成无菌生长的透明圈(即抑菌圈)。抑菌圈的大小反映待检菌对测定药物的敏感程度,并与该药对待检菌的最低或最小抑菌浓度(minimal inhibitory concentration,简称MIC)
抑菌作用的判断:抑菌圈直径≥20mm为极敏感“+++”判为有抑菌作用,抑菌圈越大抑菌效果越好;15mm≥抑菌直径<20mm为高敏“++”;10mm≥抑菌直径<15mm为中敏“+”;抑菌直径<10mm为无效,判为无抑菌作用。3次重复试验均有抑菌作用结果者,判为合格。阴性对照组无抑菌环产生,否则试验无效。
通过常规的抗菌评价方法和抑菌能力的分析,将以上80多种植物精油及其活性物经过抑菌圈测试,选取其中抑菌圈超过19毫米的对四种微生物均有有明显抑制效果的精油及活性物为精油如,桂皮精油、迷迭香油、香柏精油、柠檬草精油、橙花精油、薄荷油、丁香油、百里香精油和天竺葵精油;精油活性物如,芳樟醇、香芹酚、香叶醇、丁香醇、丁香酚、2-异丙基-5-甲基苯酚等共15种。
最低抑菌浓度测试(MIC)。
根据以上抑菌圈的实验筛选并同时确定各自的最低抑菌浓度MIC,采用琼脂培养基稀释方法,将体积百分比0.5%的吐温-20加入琼脂中,目的是为了增加所测试精油或活性物的溶解性。每种精油或活性物制备成一系列2倍的稀释液,浓度范围为0.2毫克/毫升至25.6毫克/毫升,表面皿在室温下干燥30分钟后,用3PPM的培养基现场接种,每种微生物含有105CFU/ml菌落数。在摄氏37度温度下接种18小时,并计算MIC.实验一式三份,含有精油及活性物的表面皿与空白进行对比,观察抑菌的情况,并观察精油及活性物的最低抑菌所对应的浓度,确定上述15种植物精油及精油活性物具有较好的抑菌活性,并最终 选出12种植物精油及其活性物分别为精油如,桂皮精油、迷迭香油、香柏精油、柠檬草油、橙花精油、薄荷油、丁香油、天竺葵精油和百里香精油;以及精油活性物,如:芳樟醇、香叶醇、2-异丙基-5-甲基苯酚。
此外,本发明经过实验和研究发现,在已知的具有抑菌效果的植物精油中,它们的抗菌特性有强弱之分,有的对抑制真菌效果好,有的对抑制细菌效果好,有的对革兰氏阳性菌比格兰仕阴性菌的抑制效果好等等。为了获得精油在化妆品中有效应用,将适合的精油和精油活性物质以适当的重量百分比进行组合形成复方精油及活性物的防腐剂(相当于复方精油及活性物混合组成的组合物)并用于化妆品防腐剂组合物的建立,并且复方精油及其活性物防腐剂在化妆品中所占重量百分比尽量控制在2%。
抗菌实验(单方精油及活性物,复方精油及活性物)。
1、单方精油或活性物抑菌试验(12种精油及活性物)。
将吐温-20:精油(活性物)以3:1的重量比称取,然后将吐温-20加入精油搅拌形成混合物,然后分别取含有0.5%,1%,1.5%,2.0%,2.5%,3.0%单方精油或活性物(精油的载体或溶剂为霍霍巴油,精油或活性物可以先用霍霍巴油溶解,举例如2%迷迭香精油其组成为,2克迷迭香精油+98克霍霍巴油),加入10毫升含有无菌培养基的培养皿中,然后震荡混合。将四种培养好的微生物黑曲霉菌,白色念珠菌,金黄色葡萄球菌和绿脓杆菌以液体形式分别滴入上述含有单个精油,吐温-20和培养基的培养皿中,其中每滴微生物液体含有大约1百万个微生物。之后将培养皿震荡,放置在37摄氏度的恒温条件下培养72小时,然后注意观察微生物的生长情况,微生物生长的越多表明精油及活性物防腐剂的抑菌效果越差;反之,微生物生长的越少表明精油及活性物防腐剂的抑菌效果越好,实验证明,将0.5%,1.0%,2.0%浓度的单方植物精油及活性物(分别 为桂皮油,迷迭香油,香柏精油,柠檬草油,橙花精油,薄荷油,丁香油,天竺葵精油,百里香精油,芳樟醇,香叶醇,2-异丙基-5-甲基苯酚)等12种分别测试结果表明,所述12种植物精油及活性物在单方精油及活性物浓度分别为0.5%,1.0%,2.0%的浓度条件下,抑菌效果较弱或无抑菌效果。说明单方精油或活性成分在0.5%,1.0%,2.0%的浓度下的抑菌效果较低。
2、复方精油及活性物抑菌试验(12种精油及活性物以不同重量百分比组成的混合物)
与采用单方精油或活性物抑菌实验同样的接种方法不同的是,将四种培养好的微生物黑曲霉菌,白色念珠菌,金黄色葡萄球菌和绿脓杆菌以液体形式分别滴入含有不同配比的复方精油及活性物(由12种精油及活性物)组成的防腐剂(见表1),吐温-20和培养基的培养皿中,其中复方精油及活性物中含12种精油及活性物,其中每滴微生物液体含有大约1百万个微生物。之后将培养皿震荡,放置在37摄氏度的恒温条件下培养72小时,然后注意观察微生物的生长情况。
本发明复方精油及活性物防腐剂组合物分8个体系,每个防腐体系相当于一个防腐组合物,各个防腐剂组合物中12种植物精油及活性物各自的重量百分比是根据各自的最低抑菌浓度MIC来确定12种植物精油及活性物的重量百分比。其中霍霍巴油为植物精油及活性物的载体油脂,月硅酸单甘油酯在各自的防腐剂组合物中充当分散,溶解和乳化的功能。
经过筛选,设计形成8个复方植物精油及活性物防腐剂组合物组合物(见表1),其中的12种植物精油及活性物如,芳樟醇占防腐剂组合物重量百分比为2-17%,香叶醇占防腐剂组合物重量百分比为0.5-5%,百里香精油占防腐剂组合物重量百分比为2-20%,丁香油占防腐剂组合物重量百分比为0.5-6%,2- 异丙基-5-甲基苯酚占防腐剂组合物重量百分比为0.1-0.8%,桂皮精油占防腐剂组合物重量百分比为0.1-2%,香柏精油占防腐剂组合物重量百分比为2-19%,柠檬草精油占防腐剂组合物重量百分比为,1-12%,迷迭香精油占防腐剂组合物重量百分比为0.5-5%,橙花精油占防腐剂组合物重量百分比为0.5-5%,薄荷油占防腐剂组合物重量百分比为0.5-5%,天竺葵精油占防腐剂组合物重量百分比为0.1-0.8%,此外还含有单月硅酸甘油酯,单月硅酸甘油酯占防腐剂组合物重量百分比为0.05-1.5%,防腐剂组合物中余量用霍霍巴油补齐。
与单方精油及活性物抑菌实验效果不同的是,经过复方精油及活性物抑菌实验发现:所述12种植物精油及活性物所组成的复方精油及活性物防腐剂组合物(1)至(8),当(1)至(8)实施例分别取0.5%,1.0%,2.0%进行抑菌实验时,发现各剂组合物对对四种培养好的微生物黑曲霉菌、白色念珠菌、金黄色葡萄球菌和绿脓杆菌均表现出不同程度的抑菌效果。
以上防腐剂组合物中所述植物精油如,桂皮精油,迷迭香油,香柏精油,柠檬草精油,橙花精油,薄荷油,丁香油,天竺葵精油,百里香精油以及精油活性物如,香叶醇,2-异丙基-5-甲基苯酚,芳樟醇均为市售的纯的植物精油及其活性物,这些植物精油及活性物均具有杀菌和抑菌的效果,此外,单月硅酸甘油酯在本发明防腐剂组合物中充当乳化和分散精油的作用。单月硅酸甘油酯,化学名为2,3-二羟基丙醇十二酸酯(式Ⅶ),又名十二酸单甘油酯,是一种亲脂性的非离子型表面活性剂,是天然存在于一些植物中的化合物。提取之后经常作为杀菌剂及消炎剂添加到食品、日用品或化妆品中。月桂酸单甘油酯由月桂酸和甘油直接酯化合成,外观一般为鳞片状或油状、白色或浅黄色的细粒状结晶。从结构式可以看出单月硅酸甘油酯具有双亲的结构,分子量274.21,月桂酸碳链的存在具有杀菌和抑菌的效果,因此,单月硅酸甘油酯既是乳化分散剂,又 是一个杀菌剂,在本发明中主要起到精油的乳化分散作用并兼有协同抑菌的效果。本发明复方精油及活性物防腐剂组合物中,单月桂酸甘油酯占本发明防腐剂组合物重量百分比进一步优化为0.1-0.8%。
Figure PCTCN2017100495-appb-000009
式Ⅶ 单月硅酸甘油酯
此外,霍霍巴油在本发明中为植物精油的载体油脂,为非芳香植物精油类,霍霍巴油在1至8防腐剂组合物中用量补齐到100%。
表1:复方植物精油及活性物防腐剂组合物实施例1至8
Figure PCTCN2017100495-appb-000010
Figure PCTCN2017100495-appb-000011
单月硅酸甘油酯在本发明防腐剂组合物中充当乳化和分散精油的作用。霍霍巴油在本发明中为植物精油的载体油脂,为非芳香植物精油类。
制作方法:
1、先将单月硅酸甘油酯分散和溶解在霍霍巴油中,然后加入香叶醇,芳樟醇,2-异丙基-5-甲基苯酚并搅拌直到溶解,
2、边搅拌边加入桂皮精油,迷迭香油,香柏精油,柠檬草油,橙花精油,薄荷油,丁香油,天竺葵油,百里香精油,注意容器封闭性。
3、继续搅拌直到全部分散和溶解。
以上所述8个防腐剂组合物,1至8的防腐剂组合物(见表1),分别取各自重量百分比0.5%、1%、1.5%、2.0%、2.5%、3.0%,则均呈现抑菌效果。其中防腐剂组合物实施例6、7、8比较理想。
通过实验和分析,从1至8防腐剂组合物实施例中选择一种最优化的复方精油及其活性物防腐剂组合物,该防腐剂组合物能够在72小时之内对所述四种微生物起到最大的抑制效果(黑曲霉菌,白色念珠菌,金黄色葡萄球菌和绿脓杆菌),此外,再综合性价比和温和性等因素,该复方精油及活性物防腐剂组合物为防腐剂组合物实施例6(见表2)
表2,精油及活性物防腐剂组合物6
Figure PCTCN2017100495-appb-000012
Figure PCTCN2017100495-appb-000013
-::无微生物或微生物消失
+:轻度至中度微生物
++:中度至重度微生物
防腐剂组合物6在重量百分比2%的用量下,72小时对四种微生物显示良好的抑制和杀灭效果。
----------------------------------------------------------
精油及活性物防腐剂组合物的应用
为了验证精油及活性物防腐剂组合物6在常规化妆品组合物中的应用及效果,一种洁面霜配方如下表3:
表3 洁面霜配方
Figure PCTCN2017100495-appb-000014
Figure PCTCN2017100495-appb-000015
本洁面霜配方中的成分如,阳离子瓜尔胶为瓜尔胶羟丙基三甲基氯化铵,硬脂酸钾和椰油基羟乙基磺酸钠为发泡剂和清洁剂,甘油为保湿剂,尿囊素为抗过敏剂,单甘脂、硬脂酸、十六十八醇为乳化剂和乳化增稠剂,辛酸/葵酸三甘油酯为润肤剂,维生素E乙酸酯为抗氧化剂,复方精油及活性物防腐剂组合物6为本发明优选的防腐剂组合物,吐温-20是增溶剂。所有上述原料都是属于化妆品级原料,是本领域的人已知并在市面上可以购买到的。吐温-20与复方精油及活性物防腐剂组合物6以重量比3:1的比例混合并添加。
工艺
1、将水相成份中的阳离子瓜尔胶溶于去离子水,然后在搅拌下加入甘油,硬脂酸钾,尿囊素和椰油基羟乙基磺酸钠,边搅拌边加热,直到温度升到75摄氏度,保持恒温。
2、将油相成份中的单甘脂,辛酸/葵酸三甘油酯,硬脂酸,十六十八醇,维生素E乙酸酯加在一起,然后加热并搅拌直到溶解,当温度到达75摄氏度时保持恒温。
3、防腐剂组合物的预混合溶解:将吐温-20漫漫加入到精油及活性物防腐剂组合物6搅拌溶解,备用。
4、在75摄氏度的温度下,将步骤2物质加入到步骤1中,搅拌直到乳液乳化均匀,之后开始降温到40摄氏度,
5、将步骤3物质防腐剂预混合物漫漫加入到步骤4物质中,搅拌直到防腐剂组合物均匀。
抑菌试验
为了验证洁面霜配方(1)和洁面霜配方(2)的抑菌效果:将洁面霜(1)和洁面霜(2)分别放入四个规格为150毫米的培养皿中,然后每四个培养皿中分别放入四种约1百万计数的微生物,将1克接种过的产品用9毫升无菌稀释液稀释,培养,观察,结果发现,5天后洁面霜配方(1)和洁面霜配方(2)的微生物从起初的1*106降低到<10.见表4
表4
Figure PCTCN2017100495-appb-000016
为了验证精油及活性物防腐配方剂组合物6在常规化妆品组合物中的应用及效果,一种润肤乳配方如下表5:
表5 润肤乳,
Figure PCTCN2017100495-appb-000017
Figure PCTCN2017100495-appb-000018
本润肤乳配方中的成分如,阳离子瓜尔胶为瓜尔胶羟丙基三甲基氯化铵,起到增稠作用,12烷基磷酸酯钾和单甘脂、十六十八醇、硬脂酸为乳化剂和乳化稳定剂,辛酸/葵酸三甘油酯和白油为润肤剂,甘油为保湿剂,尿囊素为抗过敏剂,维生素E乙酸酯为抗氧化剂,复方精油及活性物防腐剂组合物6为本发明优选的防腐剂组合物,吐温-20是本发明防腐剂组合物的增溶剂。所有上述原料都是属于化妆品级原料,是本领域的人已知的在市面上可以购买到的。吐温-20与复方精油及活性物防腐剂组合物6以重量比3:1的比例混合并添加。
工艺
A、将水相成份中的阳离子瓜尔胶溶于去离子水,然后在搅拌下加入甘油,尿囊素和12烷基磷酸酯钠,边搅拌边加热,直到温度升到75摄氏度,保持恒温。
B、将油相成份中的单甘脂,辛酸/葵酸三甘油酯,白油,硬脂酸,十六十八醇,维生素E乙酸酯加在一起,然后加热并搅拌直到溶解,当温度到达75摄氏度时保持恒温。
C、防腐剂组合物的预混合溶解:将吐温-20漫漫加入到复方精油及活性物防腐剂组合物6搅拌溶解,备用。
D、在75摄氏度的温度下,将B加入到A中,搅拌直到乳液乳化均匀,之后边搅拌边降温,当温度降到60摄氏度时加入三乙醇胺,继续搅拌。
E、当温度降温到40摄氏度,将预先混合好的C防腐剂组合物漫漫加入到D中,搅拌15-30分钟直到防腐剂组合物均匀。
抑菌试验:为了验证润肤乳配方(1)和润肤乳配方(2)的抑菌效果:将润肤乳(1)和润肤乳(2)分别放入四个规格为150毫米的培养皿中,然后每四个培养皿中分别放入四种约1百万计数的微生物,将1克接种过的产品用9毫升无菌稀释液稀释,培养,观察,结果发现,5天后润肤乳配方(1)和润肤乳配方(2)的微生物从起初的1.5*106降低到<10.见表6
表6
Figure PCTCN2017100495-appb-000019
与现有技术相比,本发明具有以下优点:
1、本发明一种天然替代防腐剂组合物是由具有抑菌作用的复方植物精油及活性物组成,该天然替代防腐剂组合物能有效对抗抗化妆品中常见的微生物(1) 霉菌如黑曲霉菌,(2)酵母菌如白色念珠菌,(3)革兰氏阳性菌如金黄色葡萄球菌,(4)革兰氏阴性菌如绿脓杆菌。
2、本发明天然替代防腐剂组合物,以2%的重量百分比用于不含其它化学防腐剂的化妆品乳液配方中能在72小时内有效抑制并杀灭其中的微生物。

Claims (4)

  1. 一种天然替代的植物精油防腐剂,由复方植物精油及活性物组成,其组分及重量百分比含量如下:
    (a)占防腐剂重量百分比为2-17%的芳樟醇;
    (b)占防腐剂重量百分比为0.5-5%的香叶醇;
    (c)占防腐剂重量百分比为2-20%的百里香精油;
    (d)占防腐剂重量百分比为0.5-6%的丁香油;
    (e)占防腐剂重量百分比为0.1-0.8%的2-异丙基-5-甲基苯酚;
    (f)占防腐剂重量百分比为0.1-2%的桂皮精油;
    (g)占防腐剂重量百分比为2-19%的香柏精油;
    (h)占防腐剂重量百分比为,1-12%的柠檬草精油;
    (i)占防腐剂重量百分比为0.5-5%的迷迭香精油;
    (j)占防腐剂重量百分比为0.5-5%的橙花精油;
    (k)占防腐剂重量百分比为0.5-5%的薄荷油;
    (l)占防腐剂重量百分比为0.1-0.8%的天竺葵精油;
    (m)占防腐剂重量百分比为0.05-1.5%的单月硅酸甘油酯;
    (n)余量的霍霍巴油。
  2. 根据权利要求1所述的防腐剂,还含有占防腐剂重量百分比0.1-0.8%的单月硅酸甘油酯。
  3. 一种天然替代的植物精油防腐剂,其组分及重量百分比含量如下:
    组分 含量 重量(%) 芳樟醇 15 香叶醇 4 百里香精油 18 丁香油 5 2-异丙基-5-甲基苯酚 0.6 桂皮精油 1.5 香柏精油 19 柠檬草精油 10 迷迭香精油 4.5 橙花精油 4.5 薄荷油 4.5 天竺葵精油 0.6 月硅酸单甘油酯 0.6 霍霍巴油 加至100%。
  4. 权利要求1所述防腐剂在化妆品中抑制黑曲霉菌、白色念珠菌、金黄色葡萄球菌和绿脓杆菌的应用。
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