WO2022228268A1 - 虾青素组合物及其制备方法和应用 - Google Patents

虾青素组合物及其制备方法和应用 Download PDF

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WO2022228268A1
WO2022228268A1 PCT/CN2022/088180 CN2022088180W WO2022228268A1 WO 2022228268 A1 WO2022228268 A1 WO 2022228268A1 CN 2022088180 W CN2022088180 W CN 2022088180W WO 2022228268 A1 WO2022228268 A1 WO 2022228268A1
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astaxanthin
oil
present disclosure
composition
astaxanthin composition
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PCT/CN2022/088180
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English (en)
French (fr)
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张金金
林娜妹
张慧
李传茂
张伟杰
张楚标
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广州市科能化妆品科研有限公司
广东丹姿集团有限公司
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Publication of WO2022228268A1 publication Critical patent/WO2022228268A1/zh

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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
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • 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
    • A61K8/35—Ketones, e.g. benzophenone
    • 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
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/522—Antioxidants; Radical scavengers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions
    • A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18

Definitions

  • the present disclosure relates to an astaxanthin composition, a preparation method and application thereof, in particular to an efficient and stable astaxanthin composition, a preparation method and application thereof, and belongs to the field of cosmetics.
  • Astaxanthin is one of the carotenoids, which has strong antioxidants and is highly recognized by consumers in skin care products. .
  • the molecular structure of astaxanthin contains many long conjugated unsaturated double bonds, which is sensitive to light and heat, and its properties are extremely unstable and easy to fade, which affects its stability in cosmetic applications and reduces its antioxidant properties.
  • Citation 1 discloses a highly efficient and stable photoresist and antioxidant composition and its application.
  • the composition includes the following components in parts by weight: 0.0001-0.2 parts of astaxanthin; 0.01-2.0 parts of glucosyl rutin .
  • it is a compound of glucosyl rutin and water-soluble astaxanthin, which has good photothermal stability when used in skin care products. Prolonged time will cause the color of the material to turn yellow.
  • Citation 2 discloses an astaxanthin-containing aqueous composition, a cosmetic, and a method for inhibiting the decomposition of astaxanthin, wherein the astaxanthin-containing aqueous composition contains at least (A) astaxanthin, (B) 20 ⁇ g/ L or more iron and (C) an iron chelating agent; and a method for inhibiting the decomposition of astaxanthin, wherein (C) an iron chelating agent is contained in an aqueous composition, which is said to contain at least (A) ) astaxanthin and (8) iron above 20 ⁇ g/L.
  • the astaxanthin-containing water-based composition contains a certain concentration of iron ions, which may have poor compatibility with the thickener in cosmetic formulations or cause discoloration of active ingredients, etc. At the same time, the water-based composition protects astaxanthin from being degraded. The mechanism is to block the influence of the components in the water system of skin care products on astaxanthin.
  • the present disclosure first provides an astaxanthin composition, which is compounded by microalgae oil and oat kernel oil, so that astaxanthin has good heat resistance in skin care products or cosmetics and lightfast stability, maintaining its antioxidant activity in skin care products.
  • the present disclosure also provides an emulsification system with strong antioxidant activity and excellent thermal stability and light stability.
  • an astaxanthin composition which, based on the total mass of the astaxanthin composition, includes the following components:
  • Microalgal oil 25-50%
  • Astaxanthin 0.01-5%.
  • an astaxanthin composition wherein, based on the total mass of the astaxanthin composition, the added amount of the microalgal oil is 30-50%, and the added amount of the oat kernel oil is 30-50%. is 50-70%, and the added amount of the astaxanthin is 0.05-5%.
  • an astaxanthin composition wherein the weight ratio of the microalgae oil, oat kernel oil and astaxanthin is 1:(0.9-2.8):(0.0002-0.2); preferably 1:( 1 to 2.3): (0.0017 to 0.2).
  • the present disclosure also provides a preparation method of the astaxanthin composition according to the present disclosure, including the step of mixing the components of the astaxanthin composition.
  • the present disclosure also provides an emulsification system comprising the astaxanthin composition described in the present disclosure; preferably, based on the total mass of the emulsification system, the astaxanthin composition is added in an amount of 0.01-10% .
  • the emulsification system further comprises one or a combination of two or more of emulsifiers, oils, thickeners, moisturizing agents, and preservatives.
  • the added amount of the emulsifier is 0.01-5%; the added amount of the oil is 0.1-40%; the thickening
  • the addition amount of the agent is 0.01-5%; the addition amount of the moisturizing agent is 0.01-20%; the addition amount of the preservative is 0.01-2%.
  • the present disclosure also provides a preparation method of the emulsion system according to the present disclosure, which includes the step of mixing each component of the emulsion system.
  • the present disclosure further provides an application of the astaxanthin composition according to the present disclosure or the emulsification system according to the present disclosure in skin care products or cosmetics.
  • the skin care product or cosmetic comprises one or a combination of two or more of lotions, essences, sleeping masks, face creams, moisturizing oils, massage creams, lip balms, and lipsticks.
  • the beneficial effect of the present disclosure is at least as follows: the efficient and stable astaxanthin composition provided by the present disclosure is compounded with microalgae oil and oat kernel oil in astaxanthin-containing antioxidant skin care products, Astaxanthin has good light stability and thermal stability, and maintains the antioxidant activity of astaxanthin in skin care products.
  • the astaxanthin composition of the present disclosure is added to the emulsification system of the present disclosure, and the emulsification system of the present disclosure has excellent antioxidant activity, and has excellent thermal stability and light stability.
  • compositions of the present disclosure can be used in skin care products or cosmetics.
  • FIG. 1 shows the DPPH clearance rate of the emulsions prepared by the application examples 1, 3-4 and application comparative examples 1-3 of the present disclosure and the control group emulsion under various conditions.
  • references to “some specific/preferred embodiments”, “other specific/preferred embodiments”, “embodiments”, etc. refer to the specific elements described in relation to the embodiment (eg, features, structures, properties, and/or characteristics) are included in at least one embodiment described herein, and may or may not be present in other embodiments. Additionally, it should be understood that the described elements may be combined in any suitable manner in the various embodiments.
  • numerical range represented by "numerical value A to numerical value B” means a range including numerical values A and B at the endpoints.
  • the "water” includes deionized water, distilled water, ion-exchanged water, double-distilled water, high-purity water, purified water and any other feasible water that can be used in the cosmetic field.
  • the specific temperature may be 10-40°C.
  • a first aspect of the present disclosure provides an astaxanthin composition, based on the total mass of the astaxanthin composition, comprising the following components:
  • Microalgal oil 25-50%
  • Astaxanthin 0.01-5%.
  • the astaxanthin composition of the present disclosure enables astaxanthin to have good photostability and thermal stability in skin care products, while maintaining good antioxidant activity.
  • the microalgae oil in the astaxanthin composition of the present disclosure is a natural oil extracted from microalgae organisms, rich in Omega-9 unsaturated fatty acids beneficial to the human body, stable in properties and strong in anti-oxidation.
  • the microalgal oil of the present disclosure is a kind of microalgae separated and screened from chestnut tree sap, using dry sucrose as a transparent light yellow liquid oil extracted after carbonic fermentation, rich in more than 90% Omega-9 Monounsaturated fatty acid (oleic acid), with excellent antioxidant properties, stable properties and not easy to change color.
  • the added amount of the microalgae oil is 25-50%, preferably 30-50%, for example: the added amount of the microalgae oil can be 26%, 27%, 28%, 29%, 30%, 32%, 33%, 35%, 36%, 38%, 40%, 42%, 43%, 45%, etc.
  • the added amount of the microalgae oil is 25-50%, the light resistance and heat resistance properties of astaxanthin in the application of skin care products can be significantly improved, and excellent antioxidant activity can be maintained.
  • the oat kernel oil in the astaxanthin composition of the present disclosure is an oil refined from oat kernels.
  • the oat kernel oil of the present disclosure can be obtained by using CO 2 supercritical extraction and is a natural pure vegetable oil without introducing a solvent, which is yellow and transparent, rich in more than 80% unsaturated fatty acids and various active ingredients, such as Omega-6 Natural antioxidants like Oleic Acid, Omega-3 Linolenic Acid, Omega-9 Oleic Acid and Vitamin E.
  • the added amount of the oat kernel oil is 45-70%, preferably 50-70%, for example: can be 46%, 48%, 50%, 52%, 55% %, 58%, 60%, 62%, 63%, 65%, 68%, 69%, etc.
  • the added amount of the oat kernel oil is 45-70%, which can synergize with the microalgae oil, thereby improving the UV protection stability of astaxanthin in the application of skin care products, and can exert excellent antioxidant activity.
  • astaxanthin in the present disclosure includes derivatives such as astaxanthin and an ester of astaxanthin (hereinafter, also referred to as “astaxanthin” as appropriate).
  • any astaxanthin may be used as long as it is obtained by a conventional method other than astaxanthin derived from natural products such as plants, algae, and bacteria.
  • natural products such as plants, algae, and bacteria.
  • the natural product include Phaffia rhodochrous, Haematococcus, marine bacteria, krill, and the like.
  • the extract etc. derived from the culture are also mentioned.
  • the astaxanthin in the astaxanthin composition of the present disclosure is astaxanthin extracted from Haematococcus as a raw material.
  • Haematococcus include Haematococcus pluvialis, Haematococcus lacustrine, and the like.
  • the astaxanthin of the present disclosure is a dark red oily extract obtained from Haematococcus pluvialis as a raw material without introducing a solvent through CO 2 supercritical extraction, and contains not less than 5.5% total carotenoids, of which natural The total astaxanthin content is not less than 5%, and the all-trans astaxanthin content is not less than 3.5%.
  • the astaxanthin of the present disclosure has antioxidant effects, anti-inflammatory effects, skin anti-aging effects, whitening effects, and the like, as can impart excellent emollient effects, anti-aging effects to skin, and antioxidant effects.
  • the added amount of astaxanthin is 0.01-5%, preferably 0.05-5%, for example: can be 0.03%, 0.06%, 0.08%, 0.1%, 0.12% , 0.2%, 0.5%, 0.8%, 1%, 1.2%, 1.5%, 1.8%, 2.0%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2 %, 4.5%, etc.
  • the added amount of astaxanthin is 0.01-5%, it can be used in combination with microalgae oil and oat kernel oil, used in cosmetics and skin care products, has good light and temperature stability, is not easy to fade, and maintains well antioxidant activity.
  • the weight ratio of the microalgal oil, oat kernel oil and astaxanthin of the present disclosure is 1:(0.9-2.8):(0.0002-0.2); preferably 1:(1-2.3 ):(0.0017 ⁇ 0.2), for example: 1:(1.1 ⁇ 2.2):(0.002 ⁇ 0.18), 1:(1.2 ⁇ 2.1):(0.004 ⁇ 0.15), 1:(1.3 ⁇ 2):(0.007 ⁇ 0.14 ), 1:(1.4 ⁇ 1.9):(0.01 ⁇ 0.12), 1:(1.5 ⁇ 1.8):(0.02 ⁇ 0.1), 1:(1.6 ⁇ 1.7):(0.04 ⁇ 0.0.08).
  • the efficacy of each component can be exerted most effectively, so as to make astaxanthin
  • the composition can obtain more excellent antioxidant activity, photostability and thermal stability.
  • the present disclosure also provides a preparation method of an astaxanthin composition, which includes the step of mixing each component of the astaxanthin composition.
  • the preparation method includes: mixing microalgal oil, oat kernel oil and astaxanthin at room temperature, and stirring at 100-1000 rpm/min for 1-20 min to obtain the astaxanthin composition.
  • a second aspect of the present disclosure provides an emulsifying system comprising the astaxanthin composition of the first aspect of the present disclosure.
  • the emulsification system can have excellent antioxidant activity under high temperature and light conditions.
  • the astaxanthin composition is added in an amount of 0.01-10%, for example: 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, etc.
  • 0.01-10% 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, etc.
  • the addition amount of the astaxanthin composition is less than 0.01%, the effect of antioxidant activity cannot be achieved, or the effect of antioxidant activity is poor; when the addition amount of the astaxanthin composition is greater than 10%, the astaxanthin composition The content of the substance is too high, the cost is too high, the concentration in skin care products is too high, and it is yellow and easy to color when applied to the skin.
  • the emulsification system of the present disclosure further comprises one or a combination of two or more of emulsifiers, oils, thickeners, moisturizing agents, and preservatives.
  • the added amount of the emulsifier is 0.1-5%; the added amount of the oil is 0.1-40%; the added amount of the thickener is 0.01-5%;
  • the added amount of the moisturizing agent is 0.01-20%; the added amount of the preservative is 0.01-2%.
  • the formulation composition of the emulsification system of the present disclosure is mild, so that the efficacy of the astaxanthin composition of the present disclosure can be fully exerted. in particular:
  • the added amount of the emulsifier is 0.01-5%, for example: it may be 0.1-5%, it may be 1-5%, it may be 1-4% , can be 1-3%, etc., for example: 0.5%, 0.8%, 1.5%, 2%, 2.5%, 3.5%, 4.5%, etc.
  • the dosage of the emulsifier in the present application is less than 0.01%, the emulsification is insufficient and the system is unstable; when the dosage of the emulsifier is more than 5%, it may cause skin discomfort, and adverse reactions such as acne and irritation may occur, which will affect the stability of the product. will also have some impact.
  • the emulsifier may include cetearyl alcohol, cetearyl glucoside, PEG-100 stearate, polyglycerol-10 stearate, glyceryl stearate/PEG- 100 stearate, sorbitan sesquioleate, isosteareth-20, PEG-10 rapeseed sterol, laureth-7, polyglycerol-3 methyl glucodistearate , PEG/PPG-10/1 dimethicone, polyglycerol-3 diisostearate, glyceryl stearate, steareth-20, ceteth-20, poly One or a combination of one or two or more of Sorbitan Ester-60.
  • the added amount of the oil is 0.1-40%; for example, the added amount of the oil can be 1%, 5%, 10%, 15%, 20% , 25%, 30%, 35%, etc.
  • the added amount of the oil can be 1%, 5%, 10%, 15%, 20% , 25%, 30%, 35%, etc.
  • the oils and fats may include isopropyl myristate, dimethicone, caprylic/capric triglycerides, dioctyl carbonate, hydrogenated polyisobutylene, shea butter, ethyl palmitate One or a combination of two or more selected from the group consisting of methylhexyl ester, hydrogenated polydecene, isononyl isononanoate, ethylhexyl cetyl alcohol, phytosterols, sunflower oil, and olive oil unsaponifiable matter.
  • the added amount of the thickener is 0.01-5%.
  • the consistency of the emulsification systems of the present disclosure can be tailored by adding thickeners.
  • the added amount of the thickener of the present disclosure can be 0.05-4%, 0.1-3%, 1-3%, etc., for example: 0.02%, 0.08%, 0.3%, 0.5%, 0.8% %, 1.5%, 2%, 2.5%, 3.5%, 4.5%, etc.
  • the thickeners include carbomer, carbomer salt, xanthan gum, sodium polyacrylate, carrageenan, gellan gum, hydroxyethyl cellulose, acryloyldimethyltaurine One or a combination of two or more of ammonium/VP copolymer and hydroxyethyl acrylate/sodium acryloyldimethyltaurate copolymer.
  • the added amount of the moisturizing agent is 0.01-20%.
  • the added amount of the moisturizing agent can play a moisturizing effect.
  • the added amount of the moisturizing agent of the present disclosure can be 1-18%, can be 3-16%, can be 5-14%, can be 6-12%, for example: 2% , 3%, 6%, 8%, 10%, 12%, 15%, 17%, 19%, etc.
  • the humectants include butanediol, panthenol, dipropylene glycol, glycerin, betaine, xylitol, sodium hyaluronate, trehalose, pentylene glycol, hexylene glycol, 1,3 - One or a combination of two or more propylene glycols.
  • the emulsifying system of the present disclosure may also contain a preservative, and based on the total mass of the emulsifying system, the preservative is added in an amount of 0.01-2%; specifically, the preservative may include phenoxyethanol, hydroxybenzene One or a combination of two or more of methyl ester, propylparaben, ethylhexylglycerol, benzoic acid and salts thereof.
  • the emulsification system of the present disclosure is not limited to the above components, and other feasible ingredients that can be used in cosmetics or skin care products can also be added, such as: whitening additives, skin conditioning agents, sensitizers, pH adjusters, chelating agents, other Antioxidants and more.
  • the present disclosure also provides a preparation method of the emulsification system, the preparation method includes the step of mixing each component of the emulsification system.
  • the preparation method comprises the following steps:
  • phase A Mix the emulsifier and oil at a temperature of 75-85°C, and keep moisturizing for 1-20min to obtain phase A;
  • phase B After mixing the thickener, moisturizing agent and water, and homogenizing for 1-5min, heat to 75-85°C, keep the temperature for 5-30min, fully stir until the dissolution is complete, and obtain phase B;
  • phase A to phase B and homogenize for 1-10min, then stir for 1-10min;
  • the astaxanthin composition of the present disclosure is added, and the temperature is lowered to 35-45° C. after mixing evenly, and the material is discharged.
  • a third aspect of the present disclosure provides an application of the astaxanthin composition according to the present disclosure or the emulsification system according to the present disclosure in skin care products or cosmetics.
  • the astaxanthin composition or emulsification system described in the present application is applied in skin care products or cosmetics, so that the skin care products or cosmetics have the effect of antioxidant activity, and can still have stable antioxidant under high temperature or light conditions active.
  • the skin care products or cosmetics may include one or a combination of two or more of lotions, essences, sleeping masks, face creams, moisturizing oils, massage balms, lip balms, and lipsticks.
  • microalgae oil Lubrizol company, model, HSHO microalgae oil;
  • microalgae oil Take 25 parts by weight (25%) of microalgae oil, 70 parts by weight (70%) of oat kernel oil and 5 parts by weight (5%) of astaxanthin, wherein microalgae oil: oat kernel oil: astaxanthin
  • the weight percentage is 1:2.8:0.2.
  • the components were sequentially added to a clean container, stirred at 500 rpm/min for 10 min and mixed uniformly to obtain astaxanthin composition I, which was sealed and stored at room temperature for later use.
  • microalgae oil Take 30 parts by weight (30%) of microalgae oil, 69.99 parts by weight (69.99%) of oat kernel oil and 0.01 part by weight (0.01%) of astaxanthin, wherein microalgae oil: oat kernel oil: astaxanthin
  • the weight percentage is about 1:2.33:0.0003.
  • the components were sequentially added to a clean container, stirred at 300 rpm/min for 2 min and mixed evenly to obtain astaxanthin composition II, which was sealed and stored at room temperature for later use.
  • microalgae oil Take 38 parts by weight (38%) of microalgae oil, 60.5 parts by weight (60.5%) of oat kernel oil and 1.5 parts by weight (1.5%) of astaxanthin, wherein microalgae oil: oat kernel oil: astaxanthin
  • the weight percentage is about 1:1.6:0.039.
  • the components were sequentially added to a clean container, stirred at 400 rpm/min for 4 min and mixed uniformly to obtain astaxanthin composition III, which was sealed and stored at room temperature for later use.
  • microalgae oil Take 50 parts by weight (50%) of microalgae oil, 45 parts by weight (45%) of oat kernel oil and 5 parts by weight (5%) of astaxanthin, wherein microalgae oil: oat kernel oil: astaxanthin
  • the weight percentage is 1:0.9:0.1.
  • the components were sequentially added to a clean container, and the mixture was stirred at 500 rpm/min for 10 min and mixed uniformly to obtain astaxanthin composition IV, which was sealed and stored at room temperature for later use.
  • microalgae oil Take 42 parts by weight (42%) of microalgae oil, 54.8 parts by weight (54.8%) of oat kernel oil and 3.2 parts by weight (3.2%) of astaxanthin, wherein microalgae oil: oat kernel oil: astaxanthin
  • the weight percentage is about 1:1.3:0.076.
  • the components were sequentially added to a clean container, stirred at 350 rpm/min for 5 min and mixed evenly to obtain astaxanthin composition V, which was sealed and stored at room temperature for later use.
  • microalgae oil Take 40 parts by weight (40%) of microalgae oil, 58 parts by weight (58%) of oat kernel oil and 2 parts by weight (2%) of astaxanthin, wherein microalgae oil: oat kernel oil: astaxanthin
  • the weight percentage is 1:1.45:0.05.
  • the components were sequentially added to a clean container, and the mixture was stirred at 300 rpm/min for 4.5 minutes to obtain an astaxanthin composition VI, which was sealed and stored for later use at room temperature.
  • Comparative Example 1 Take 15 parts by weight (about 16.67%) of microalgae oil, 70 parts by weight (about 77.78%) of oat kernel oil and 5 parts by weight (about 5.55%) of astaxanthin, add each component in turn to clean In the container, the mixture was stirred at 500 rpm/min for 10 min to obtain the astaxanthin composition VII, which was sealed and stored for later use at room temperature.
  • the astaxanthin compositions I-VI samples of Examples 1-6 were added to the emulsion formulation in Table 1 according to 1% mass fraction, and the astaxanthin compositions VII-XI samples of Comparative Examples 1-5 were calculated according to 1% mass fraction Added to the emulsion formulation in Table 2, the formulation without the astaxanthin composition was used as a control group. 12 emulsions were prepared according to the following method.
  • Deionized water, sodium carbomer, ammonium acryloyldimethyltaurate/VP copolymer, 1,3-propanediol, panthenol, trehalose, and sodium hyaluronate in phase B were sequentially added to a clean emulsification pot, Homogenize at high speed for 3 minutes, then heat to 80°C, keep warm for 15 minutes, and stir thoroughly until the dissolution is complete;
  • the cooling water is cooled to 45°C, and the phenoxyethanol and ethylhexylglycerol in phase C are added in turn;
  • High temperature acceleration The test condition is 50°C ⁇ 1°C, 25%RH ⁇ 5%RH for 1 month.
  • Xenon lamp illumination test the illumination intensity is 0.35W/M 2 , the test is 26.4 hours, the blackboard temperature is 45°C (not the cabinet temperature), and the humidity is 50%.
  • Outdoor light Place under natural light for 10 days.
  • control sample emulsion without astaxanthin composition does not change its appearance at high temperature because it does not contain any antioxidants, but the sunflower oil is accelerated to oxidize to produce peculiar smell; at the same time, xenon lamp and outdoor light also accelerate. Sunflower oil is oxidized, which changes the color of the lotion and produces an unpleasant odor.
  • the emulsions containing astaxanthin compositions I-VI prepared by application examples 1-6 did not change in color and odor under room temperature, high temperature, xenon lamp and outdoor light conditions.
  • the microalgae oil content in the application example 1 is relatively small, and the content of oat kernel oil and astaxanthin is too high, which is not within the scope of the present disclosure, so that the astaxanthin composition is
  • the color of the emulsion of VII changed from reddish-orange to pale orange at high temperature, xenon lamp and outdoor light, that is, astaxanthin was mostly degraded.
  • Application Example 3 is compared with Application Comparative Example 2, the content of oat kernel oil in Application Comparative Example 2 is relatively small, resulting in excessive content of microalgae oil, which is not within the scope of the present disclosure, and astaxanthin-containing composition VIII under high temperature conditions
  • the color and odor of the emulsion are the same as room temperature, but the color of xenon lamp and outdoor light is light orange compared with room temperature, that is, astaxanthin has degraded to a certain extent.
  • Application example 4 is compared with application comparative example 3, and the astaxanthin content in application comparative example 3 is high, causing the content of oat kernel oil to be too low, not within the scope of the present disclosure, and under each condition, the astaxanthin-containing composition IX is high.
  • the color of the emulsion became lighter, but the odor did not change, that is, the microalgae oil and oat kernel oil in this concentration range could only protect part of the astaxanthin from being degraded.
  • the mixing of the astaxanthin composition IX requires a longer stirring time.
  • Application example 5 is compared with application comparative example 4, in the application comparative example 4, microalgae oil is replaced with olive oil, and the emulsion containing astaxanthin composition X becomes lighter in color at high temperature and can protect part of astaxanthin from being degraded. , but the color of xenon lamps and outdoor light faded, that is, astaxanthin was completely degraded.
  • Application Example 5 is compared with Application Comparative Example 5.
  • Application Comparative Example 5 microalgal oil and oat kernel oil are replaced with tocopherol acetate, and the emulsion of astaxanthin composition XI is degraded under various conditions. The color faded but no odor was produced, however, the emulsions all had a yellow appearance due to the reaction of tocopheryl acetate under xenon lamp and light.
  • DPPH is a stable free radical in organic solvent, its alcoholic solution is purple, has a single electron, can capture other free radicals, and has a maximum absorption at the wavelength of 517nm. In the presence of free radical scavengers, the single electron of DPPH is captured to make its color lighter, and the absorbance value decreases at the maximum light absorption wavelength, and the degree of decrease is linear.
  • the antioxidant capacity is expressed by the inhibition rate, the greater the inhibition rate, the stronger the antioxidant activity.
  • compositions I, III-IV emulsions prepared by application examples 1, 3-4 and astaxanthin-containing compositions VI-IX emulsion prepared by application comparative examples 1-3 and the control group did not contain astaxanthin
  • the composition emulsion was tested under the three conditions of normal temperature, high temperature and outdoor light test samples to observe the scavenging effect of DPPH free radicals, and to evaluate the changes in the antioxidant properties of astaxanthin.
  • a sample group absorbance values of sample solution and DPPH alcohol solution
  • a blank group absorbance values of sample solution and absolute ethanol
  • a control group absorbance values of DPPH alcohol solution and water.
  • the DPPH free radical scavenging rate of the emulsions containing astaxanthin compositions I, III-VI prepared by application examples 1, 3-4 is very small after the test at room temperature, high temperature and outdoor light conditions, that is, astaxanthin can Maintains good antioxidant activity under high temperature and outdoor light conditions.
  • application example 1 is compared with application comparative example 1, and the microalgae oil content in application comparative example 1 is relatively small, and causes the content of oat kernel oil and astaxanthin to be excessive, which is not within the scope of the present disclosure,
  • the DPPH free radical scavenging rate of the emulsion of astaxanthin composition VII decreases after high temperature and outdoor illumination, that is, astaxanthin is degraded and its antioxidant activity is significantly reduced.
  • Application Example 3 is compared with Application Comparative Example 2, the content of oat kernel oil in Application Comparative Example 2 is relatively small, resulting in excessive content of microalgae oil, which is not within the scope of the present disclosure, and astaxanthin-containing composition VIII under high temperature conditions
  • the DPPH free radical scavenging rate did not change significantly in the emulsion and room temperature, but it can be seen that the astaxanthin was degraded to a certain extent under outdoor illumination and room temperature.
  • Application example 4 is compared with application comparative example 3, and the astaxanthin content in application comparative example 3 is high, causing the content of oat kernel oil to be too low, not within the scope of the present disclosure, and under each condition, the astaxanthin-containing composition IX is high.
  • Both the emulsions maintain a certain free radical scavenging effect, that is, the microalgae oil and oat kernel oil within this concentration range can only protect part of the astaxanthin from being degraded and maintain part of the antioxidant activity.

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Abstract

本公开涉及一种虾青素组合物及其制备方法和应用。以所述虾青素组合物的总质量计，所述虾青素组合物包括以下组分：微藻油：25-50％；燕麦仁油：45-70％；虾青素：0.01-5％。相比现有技术，本公开的有益效果至少在于：本公开所提供的高效稳定的虾青素组合物，将微藻油和燕麦仁油复配用于含虾青素抗氧化护肤产品中，使得虾青素具有良好的光稳定性和热稳定性，保持虾青素在护肤品中的抗氧化活性。

Description

虾青素组合物及其制备方法和应用 技术领域
本公开涉及一种虾青素组合物及其制备方法和应用，具体涉及一种高效稳定的虾青素组合物及其制备方法和应用，属于化妆品领域。
背景技术
随着皮肤衰老问题受消费者高度重视，抗氧化护肤品需求不断持续增加，而虾青素属于类胡萝卜素中的一种，具有强抗氧化剂，在护肤品中备受成分党消费者的认可。然而虾青素分子结构中含有很多长共轭不饱和双键，对光和热比较敏感，其性质极不稳定，容易褪色，使得其在化妆品应用中稳定性受影响，抗氧化性能降低。
近年来对虾青素的稳定性研究比较多，但都是针对虾青素原料保存过程而言，有报道显示采用冻干法干燥、低温密封保存、真空冷藏等有助于保持虾青素的活性。然而对虾青素应用在护肤品中在耐热和光照下维持良好活性的研究比较少。因而如何保持虾青素在抗氧化护肤品中应用，在光照和热条件下不褪色，货架期内保持良好的活性成为一大技术难点。
引用文献1公开了一种高效稳定的抗光抗氧化组合物及其应用，该组合物包括按照重量份计的以下组分：虾青素0.0001-0.2份；葡糖基芦丁0.01-2.0份。但是其将葡糖基芦丁和水溶性虾青素复配，应用于护肤品中具有良好的光热稳定性，但葡糖基芦丁自身原料因在光照下可吸收蓝光，随着货架期时间延长会引起料体颜色变黄。
引用文献2公开了一种含虾青素的水系组合物、化妆品和虾青素的分解抑制方法，该含虾青素的水系组合物中至少含有(A)虾青素、(B)20μg/L以上的铁和(C)铁螯合剂；并且，涉及一种虾青素的分解抑制方法，其中，在水 系组合物中含有(C)铁螯合剂，所述水系组合物叫至少含有(A)虾青素和(8)20μg/L以上的铁。该含虾青素的水系组合物中含一定浓度的铁离子，可能与化妆品配方中增稠剂兼容性不佳或引起活性成分出现变色等，同时该水系组合物保护虾青素不被降解的机理是阻隔护肤品水系中的组分对虾青素的影响。
引用文献
引用文献1：CN111557861A
引用文献2：CN103025306A
发明内容
发明要解决的问题
鉴于现有技术存在的技术问题，本公开首先提供了一种虾青素组合物，其采用微藻油和燕麦仁油复配，使得虾青素在护肤品或化妆品中的具有良好的耐热和耐光的稳定性，保持其在护肤品中的抗氧化活性。
本公开还提供了一种乳化体系，其抗氧化活性强，且具有优异的热稳定性、光照稳定性。
用于解决问题的方案
本公开提供一种虾青素组合物，以所述虾青素组合物的总质量计，包括以下组分：
微藻油：25-50％；
燕麦仁油：45-70％；
虾青素：0.01-5％。
根据本公开所述的是虾青素组合物，其中，以所述虾青素组合物的总质量计，所述微藻油的加入量为30-50％，所述燕麦仁油的加入量为50-70％，所述虾青素的加入量为0.05-5％。
根据本公开所述的是虾青素组合物，其中，所述微藻油、燕麦仁油和虾青素的重量比为1:(0.9～2.8):(0.0002～0.2)；优选1:(1～2.3):(0.0017～0.2)。
本公开还提供一种根据本公开所述的虾青素组合物的制备方法，包括将所述虾青素组合物各组分混合的步骤。
本公开还提供一种乳化体系，其包括本公开所述的虾青素组合物；优选地，以所述乳化体系的总质量计，所述虾青素组合物的加入量为0.01-10％。
根据本公开所述的乳化体系，其中，所述乳化体系还包含乳化剂、油脂、增稠剂、保湿剂、防腐剂中的一种或两种以上的组合。
根据本公开所述的乳化体系，其中，以所述乳化体系的总质量计，所述乳化剂的加入量为0.01-5％；所述油脂的加入量为0.1-40％；所述增稠剂的加入量为0.01-5％；所述保湿剂的加入量为0.01-20％；所述防腐剂的加入量为0.01-2％。
本公开还提供一种根据本公开所述的乳化体系的制备方法，其包括将所述乳化体系的各组分混合的步骤。
本公开又提供一种根据本公开所述的虾青素组合物或者根据本公开所述的乳化体系在护肤品或化妆品中的应用。
根据本公开所述的应用，其中，所述护肤品或化妆品包括乳液、精华液、睡眠面膜、面霜、润肤油、按摩膏、唇膏、口红中的一种或两种以上的组合。
发明的效果
相比现有技术，本公开的有益效果至少在于：本公开所提供的高效稳定的虾青素组合物，将微藻油和燕麦仁油复配用于含虾青素抗氧化护肤产品中，使得虾青素具有良好的光稳定性和热稳定性，保持虾青素在护肤品中的抗氧化活性。
本公开的乳化体系中添加有本公开的虾青素组合物，本公开的乳化体系具有优异的抗氧化活性，且具有优异的热稳定性、光照稳定性。
本公开的虾青素组合物可以在护肤品或化妆品中应用。
附图说明
图1示出了本公开应用实施例1、3-4和应用对比例1-3制备的乳液和对照组乳液在各条件下对DPPH的清除率。
具体实施方式
以下将详细说明本公开的各种示例性实施例、特征和方面。在这里专用的词“示例性”意为“用作例子、实施例或说明性”。这里作为“示例性”所说明的任何实施例不必解释为优于或好于其它实施例。
另外，为了更好地说明本公开，在下文的具体实施方式中给出了众多的具体细节。本领域技术人员应当理解，没有某些具体细节，本公开同样可以实施。在另外一些实例中，对于本领域技术人员熟知的方法、手段、器材和步骤未作详细描述，以便于凸显本公开的主旨。
如无特殊声明，本说明书中所使用的单位均为国际标准单位，并且本公开中出现的数值，数值范围，均应当理解为包含了工业生产中所不可避免的系统性误差。
本说明书中，如没有特别说明，则“％”均表示质量百分含量。
本说明书中，使用“可以”表示的含义包括了进行某种处理以及不进行某种处理两方面的含义。
本说明书中，所提及的“一些具体/优选的实施方案”、“另一些具体/优选的实施方案”、“实施方案”等是指所描述的与该实施方案有关的特定要素(例如，特征、结构、性质和/或特性)包括在此处所述的至少一种实施方案中，并且可存在于其它实施方案中或者可不存在于其它实施方案中。另外，应理解，所述要素可以任何合适的方式组合在各种实施方案中。
本说明书中，使用“数值A～数值B”表示的数值范围是指包含端点数值A、B的范围。
另外，本说明书中，所述“水”包含去离子水、蒸馏水、离子交换水、双蒸水、高纯水、纯净水等化妆品领域能够使用的任何可行的水。
本说明书中，如有涉及“室温”、“常温”等，其具体温度可以是10-40℃。
<第一方面>
本公开的第一方面提供了一种虾青素组合物，以所述虾青素组合物的总质量计，包括以下组分：
微藻油：25-50％；
燕麦仁油：45-70％；
虾青素：0.01-5％。
本公开的虾青素组合物使得虾青素在护肤品中具有良好的光稳定性和热稳定性，同时保持良好的抗氧化活性。
微藻油
本公开的虾青素组合物中的微藻油，微藻油是从微藻生物中提炼获得的天然油脂，富含有益人体的Omega-9不饱和脂肪酸，性状稳定、抗氧化强。作为优选，本公开的微藻油是由栗树汁液分离筛选的一种微藻，利用干蔗蔗糖作为碳酸发酵后提取得到的一种透明淡黄色液体油脂，富含超过90％的Omega-9单不饱和脂肪酸(油酸)，具有优异的抗氧化性，性状稳定不易变色。
以所述虾青素组合物总质量计，所述的微藻油加入量为25-50％，优选30-50％，例如：所述微藻油的加入量可以是26％、27％、28％、29％、30％、32％、33％、35％、36％、38％、40％、42％、43％、45％等。所述的微藻油加入量为25-50％时，能够显著提升虾青素在护肤品应用中的耐光照和耐热性能，保持优异的抗氧化活性。
燕麦仁油
本公开的虾青素组合物中的燕麦仁油，是从燕麦仁中精炼而成的油脂。作为优选，本公开的燕麦仁油可以使用CO 2超临界萃取得到且不引入溶剂的天然纯植物油，呈黄色透明状，富含超过80％不饱和脂肪酸及多种活性成分，如Omega-6亚油酸、Omega-3亚麻酸、Omega-9油酸和维生素E等天然抗氧化成分。
以所述虾青素组合物总质量计，所述的燕麦仁油的加入量为45-70％，优选50-70％，例如：可以是46％、48％、50％、52％、55％、58％、60％、62％、63％、65％、68％、69％等。所述的燕麦仁油加入量为45-70％，能够与微藻油产生协同增效的作用，从而提升虾青素在护肤品应用中的UV防护稳定性，能够发挥优异的抗氧化活性。
虾青素
需要说明的是，本公开中“虾青素”包含虾青素和虾青素的酯等衍生物(以下，也适宜称为“虾青素类”)。
作为本公开中的虾青素，除了来自植物类、藻类和细菌等天然物的虾青素以外，只要是根据常规方法获得的虾青素，则可以为任意的虾青素。作为所述天然物，例如，可以举出红法夫酵母、红球藻、海洋性细菌、磷虾等。另外，还可以举出来自其培养物的提取物等。
作为优选，本公开的虾青素组合物中的虾青素，是以红球藻为原料，从其中提取得到的虾青素。可列举的红球藻包括雨生红球藻、湖生红球藻等。进一步，本公开的虾青素是以雨生红球藻为原料，经过CO 2超临界萃取不引入溶剂制得的呈暗红色油状提取物，含有不低于5.5％总类胡萝卜素，其中天然总虾青素含量不低于5％，全反式虾青素含量不低于3.5％。本公开的虾青素具有抗氧化效果、抗炎效果、皮肤抗老化效果、美白效果等，作为能够赋予优异的润肤剂效果、皮肤的抗老化效果及抗氧化效果。
以所述虾青素组合物总质量计，所述的虾青素加入量为0.01-5％，优选 0.05-5％，例如：可以是0.03％、0.06％、0.08％、0.1％、0.12％、0.2％、0.5％、0.8％、1％、1.2％、1.5％、1.8％、2.0％、2.2％、2.5％、2.8％、3％、3.2％、3.5％、3.8％、4％、4.2％、4.5％等。当所述的虾青素加入量为0.01-5％时，能够与微藻油和燕麦仁油复配使用，应用于化妆品护肤品中，具有良好的光照和温度稳定性，不易褪色，保持良好的抗氧化活性。
在一些具体的实施方案中，本公开的所述微藻油、燕麦仁油和虾青素的重量比为1:(0.9～2.8):(0.0002～0.2)；优选为1:(1～2.3):(0.0017～0.2)，例如：1:(1.1～2.2):(0.002～0.18)、1:(1.2～2.1):(0.004～0.15)、1:(1.3～2):(0.007～0.14)、1:(1.4～1.9):(0.01～0.12)、1:(1.5～1.8):(0.02～0.1)、1:(1.6～1.7):(0.04～0.0.08)。当所述微藻油、燕麦仁油和虾青素的重量比为1:(0.9～2.8):(0.0002～0.2)时，各个组分的功效能够获得最有效的发挥，从而使虾青素组合物能够获得更优异的抗氧化活性、光稳定性以及热稳定性。
另外，本公开还提供了一种虾青素组合物的制备方法，其包括将所述虾青素组合物的各组分混合的步骤。具体地，所述制备方法包括：于常温下将微藻油、燕麦仁油以及虾青素于常温下混合，并在100-1000rpm/min下，搅拌1-20min，得到虾青素组合物。
<第二方面>
本公开的第二方面提供了一种乳化体系，所述乳化体系中包含有本公开第一方面所述的虾青素组合物。通过在乳化体系中添加本公开虾青素组合物，能够使该乳化体系在高温、光照条件下，均具有优异的抗氧化活性。
在一些具体的具体地实施方案中，以所述乳化体系的总质量计，所述虾青素组合物的加入量为0.01-10％，例如：0.5％、1％、2％、3％、4％、5％、6％、7％、8％、9％等。当虾青素组合物的加入量在0.01-10％之间时，其使用效果最佳。当虾青素组合物的加入量小于0.01％时，不能起到抗氧化活性的作用，或抗氧化活性的效果较差；当虾青素组合物的加入量大于10％时，虾 青素组合物的含量过高，成本过高，在护肤品中浓度太高，涂抹于皮肤上发黄易着色。
进一步，本公开的所述乳化体系还包含乳化剂、油脂、增稠剂、保湿剂、防腐剂中的一种或两种以上的组合。以所述乳化体系的总质量计，所述乳化剂的加入量为0.1-5％；所述油脂的加入量为0.1-40％；所述增稠剂的加入量为0.01-5％；所述保湿剂的加入量为0.01-20％；所述防腐剂的加入量为0.01-2％。本公开的乳化体系的配方组成温和，可以使本公开的虾青素组合物的功效得到充分发挥。具体而言：
在本公开中，以所述乳化体系的总质量计，所述乳化剂的加入量为0.01-5％，例如：可以是0.1-5％，可以是1-5％，可以是1-4％，可以是1-3％等，例如：0.5％、0.8％、1.5％、2％、2.5％、3.5％、4.5％等。本申请的乳化剂用量小于0.01％时，导致乳化不充分使得体系不稳定；乳化剂用量大于5％时，可能会引起皮肤不适感，出现致痘、刺激等不良反应，会对产品的稳定性也会造成一定的影响。
在本公开中，所述乳化剂可以包括鲸蜡硬脂醇、鲸蜡硬脂基葡糖苷、PEG-100硬脂酸酯、聚甘油-10硬脂酸酯、甘油硬脂酸酯/PEG-100硬脂酸酯、山梨坦倍半油酸酯、异硬脂醇聚醚-20、PEG-10油菜籽甾醇、月桂醇聚醚-7、聚甘油-3甲基葡糖二硬脂酸酯、PEG/PPG-10/1聚二甲基硅氧烷、聚甘油-3二异硬脂酸酯、甘油硬脂酸酯、硬脂醇聚醚-20、鲸蜡醇聚醚-20、聚山梨醇酯-60中的一种或两种以上的组合中的一种或两种以上的组合。
在本公开中，以所述乳化体系的总质量计，所述油脂的加入量为0.1-40％；例如所述油脂的加入量可以是1％、5％、10％、15％、20％、25％、30％、35％等。通过在乳化体系中添加油脂，可以减少皮肤表面水分的蒸发，防止皮肤干裂。另外，通过添加油脂，可以在皮肤表面形成疏水性薄膜，防止外部有害物质的侵入。当油脂的含量小于0.1％时，不能减少皮肤表面水分的蒸发， 且不能有效防止有害物质的侵入；当油脂的含量大于40％时，使乳化体系过于油腻，使用感会有所下降。
在本公开中，所述油脂可以包括肉豆蔻酸异丙酯、聚二甲基硅氧烷、辛酸/癸酸甘油三酯、碳酸二辛酯、氢化聚异丁烯、牛油果树果脂、棕榈酸乙基己酯、氢化聚癸烯、异壬酸异壬酯、鲸蜡醇乙基己酯、、植物甾醇类、葵花籽油、油橄榄油不皂化物中的一种或两种以上的组合。
以所述乳化体系的总质量计，所述增稠剂的加入量为0.01-5％。通过添加增稠剂，可以使本公开的乳化体系的稠度合适。作为优选，本公开的增稠剂的加入量可以是0.05-4％，可以是0.1-3％，还可以是1-3％等，例如：0.02％、0.08％、0.3％、0.5％、0.8％、1.5％、2％、2.5％、3.5％、4.5％等等。
在本公开中，所述增稠剂包括卡波姆、卡波姆盐、黄原胶、、聚丙烯酸钠、卡拉胶、结冷胶、羟乙基纤维素、丙烯酰二甲基牛磺酸铵/VP共聚物、丙烯酸羟乙酯/丙烯酰二甲基牛磺酸钠共聚物中的一种或两种以上的组合。
以所述乳化体系的总质量计，所述保湿剂的加入量为0.01-20％。当保湿剂的加入量在0.01-20％时，能够起到保湿作用。为了使保湿剂的功效能够进一步发挥，本公开的保湿剂的加入量可以是1-18％，可以是3-16％，可以是5-14％，可以是6-12％，例如：2％、3％、6％、8％、10％、12％、15％、17％、19％等等。
在本公开中，所述保湿剂包括丁二醇、泛醇、双丙甘醇、甘油、甜菜碱、木糖醇、透明质酸钠、海藻糖、戊二醇、己二醇、1,3-丙二醇中的一种或两种以上的组合。
本公开的乳化体系中还可以包含防腐剂，以所述乳化体系的总质量计，所述防腐剂的加入量为0.01-2％；具体地，所述防腐剂可以包括苯氧乙醇、羟苯甲酯、羟苯丙酯、乙基己基甘油、苯甲酸及其盐中的一种或两种以上的组合。
另外，本公开乳化体系不限于以上各组分，还可以添加其它可行的化妆品或护肤品中能够使用的成分，例如：美白添加剂、皮肤调理剂、舒敏剂、pH调节剂、螯合剂、其它抗氧化剂等等。
本公开还提供了一种乳化体系的制备方法，所述制备方法包括将所述乳化体系的各组分混合的步骤。
具体地，所述制备方法包括以下步骤：
将乳化剂和油脂于75-85℃的温度下混合，并保湿1-20min，得到A相；
将增稠剂、保湿剂以及水混合后，并均质1-5min后，加热至75-85℃，保温5-30min，充分搅拌至溶解完全，得到B相；
将A相加入B相中均质1-10min后，搅拌1-10min；
降温至40-50℃，然后加入防腐剂；
最后加入本公开的虾青素组合物，混合均匀后降温至35-45℃，出料。
<第三方面>
本公开的第三方面提供了一种根据本公开所述的虾青素组合物或者根据本公开所述的乳化体系在护肤品或化妆品中的应用。将本申请的所述的虾青素组合物或乳化体系应用在护肤品或化妆品中，以使得护肤品或化妆品具有抗氧化活性的功效，且在高温或光照条件下依然能够具有稳定的抗氧化活性。
具体地，所述护肤品或化妆品可以包括乳液、精华液、睡眠面膜、面霜、润肤油、按摩膏、唇膏、口红中的一种或两种以上的组合。
实施例
下面将结合实施例对本公开的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施例仅用于说明本公开，而不应视为限定本公开的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售获得的常规产品。
实施例中，微藻油的生产厂家：路博润公司，型号，HSHO微藻油；
虾青素的生产厂家：美国Cyanotech(西亚诺泰克)公司，型号BioAstin；
燕麦仁油的生产厂家：芬兰(Fazer)食品公司。
实施例1
取25重量份(25％)的微藻油、70重量份(70％)的燕麦仁油和5重量份(5％)的虾青素，其中微藻油:燕麦仁油:虾青素的重量百分比为1:2.8:0.2。将各组分依次加入洁净容器中，于500rpm/min下搅拌10min混合均匀，得到虾青素组合物I，常温下密闭存储备用。
实施例2
取30重量份(30％)的微藻油、69.99重量份(69.99％)的燕麦仁油和0.01重量份(0.01％)的虾青素，其中微藻油:燕麦仁油:虾青素的重量百分比约为1:2.33:0.0003。将各组分依次加入洁净容器中，于300rpm/min下搅拌2min混合均匀得到虾青素组合物II，常温下密闭存储备用。
实施例3
取38重量份(38％)的微藻油、60.5重量份(60.5％)的燕麦仁油和1.5重量份(1.5％)的虾青素，其中微藻油:燕麦仁油:虾青素的重量百分比约为1:1.6:0.039。将各组分依次加入洁净容器中，于400rpm/min下搅拌4min混合均匀，得到虾青素组合物III，常温下密闭存储备用。
实施例4
取50重量份(50％)的微藻油、45重量份(45％)的燕麦仁油和5重量份(5％)的虾青素，其中微藻油:燕麦仁油:虾青素的重量百分比为1:0.9:0.1。将各组分依次加入洁净容器中，于500rpm/min下搅拌10min混合均匀，得到虾青素组合物IV，常温下密闭存储备用。
实施例5
取42重量份(42％)的微藻油、54.8重量份(54.8％)的燕麦仁油和3.2 重量份(3.2％)的虾青素，其中微藻油:燕麦仁油:虾青素的重量百分比约为1:1.3:0.076。将各组分依次加入洁净容器中，于350rpm/min下搅拌5min混合均匀，得到虾青素组合物V，常温下密闭存储备用。
实施例6
取40重量份(40％)的微藻油、58重量份(58％)的燕麦仁油和2重量份(2％)的虾青素，其中微藻油:燕麦仁油:虾青素的重量百分比为1:1.45:0.05。将各组分依次加入洁净容器中，于300rpm/min下搅拌4.5min混合均匀，得到虾青素组合物VI，常温下密闭存储备用。
对比例1取15重量份(约16.67％)的微藻油、70重量份(约77.78％)的燕麦仁油和5重量份(约5.55％)的虾青素，将各组分依次加入洁净容器中，于500rpm/min下搅拌10min混合均匀，得到虾青素组合物VII，常温下密闭存储备用。
对比例2
取38重量份(约58.91％)的微藻油、25重量份(约38.76％)的燕麦仁油和1.5重量份(约2.33％)的虾青素，将各组分依次加入洁净容器中，于400rpm/min下搅拌4min混合均匀，得到虾青素组合物VIII，常温下密闭存储备用。
对比例3
取50重量份(约47.62％)的微藻油、45重量份(约42.86％)的燕麦仁油和10重量份(约9.52％)的虾青素，将各组分依次加入洁净容器中，于500rpm/min下搅拌25min混合均匀，得到虾青素组合物IX，常温下密闭存储备用。
对比例4
取42重量份(42％)的橄榄油、54.8重量份(54.8％)的燕麦仁油和3.2重量份(3.2％)的虾青素，将各组分依次加入洁净容器中，于350rpm/min 下搅拌5min混合均匀，得到虾青素组合物X，常温下密闭存储备用。
对比例5
取96.8重量份(96.8％)的生育酚乙酸酯和3.2重量份(3.2％)的虾青素，将各组分依次加入洁净容器中，于350rpm/min下搅拌5min混合均匀，得到虾青素组合物XI，常温下密闭存储备用。
应用实施例1-6及应用对比例1-5
将实施例1-6的虾青素组合物I-VI样品按照1％质量分数计加入表1乳液配方中，对比例1-5的虾青素组合物VII-XI样品按照1％质量分数计加入表2的乳液配方中，其中不添加虾青素组合物的配方作为对照组。按照以下方法制备得到12款乳液。
乳液的制备步骤如下：
将A相中的聚甘油-10硬脂酸酯、甘油硬脂酸酯/PEG-100硬脂酸酯、辛酸/癸酸甘油三酯、聚二甲基硅氧烷和葵花籽油依次加入洁净油相锅升温至80℃，保温10min；
B相中的去离子水、卡波姆钠、丙烯酰二甲基牛磺酸铵/VP共聚物、1,3-丙二醇、泛醇、海藻糖、透明质酸钠依次加入洁净乳化锅中，高速均质3min后加热至80℃，保温15min，充分搅拌至溶解完全；
将A相抽入乳化锅，高速均质4min后，继续搅拌5min；
冷却水降温至45℃依次加入C相中的苯氧乙醇和乙基己基甘油；
最后加入D相中的虾青素组合物(对照组不加该相)；
充分搅拌均匀后降温至38℃出料过滤，送检合格后，得到乳液样品。
表1 应用实施例1-6的乳液组成
Figure PCTCN2022088180-appb-000001
表2 应用对比例1-5和对照组乳液组成
Figure PCTCN2022088180-appb-000002
性能测试
1、稳定性测试
将应用实施例1-6制备的含虾青素组合物I-VI和应用对比例1-5制备的含虾青素组合物VII-XI的11款乳液样品和不加虾青素组合物的对照组乳液，分别置于透明PET瓶中储存于4种条件下进行测试，观察各条件下样品颜色和气味变化情况，测试结果如下表3所示。
测试条件：
常温样品于25℃，60％RH静置，进行对比测试。
高温加速：测试条件为50℃±1℃，25％RH±5％RH放置1个月。
氙灯光照测试：光照强度0.35W/M 2，测试26.4小时，黑板温度45℃(非箱体温度)，湿度50％。
室外光：放置自然光照射10天。
表3 应用实施例1-6及应用对比例1-5和对照组制备的乳液的稳定性测试结果
Figure PCTCN2022088180-appb-000003
由表3可以看出，不含虾青素组合物的对照样品乳液因不含任何抗氧化剂在高温下外观虽未发生变化，因葵花籽油被加速氧化产生异味；同时氙灯和室外光照也加速葵花籽油被氧化，使得乳液颜色发生变化同时产生异味。应用实施例1-6制备的含虾青素组合物I-VI的乳液在室温、高温、氙灯和室外光条件下均未发生颜色和气味变化。
应用实施例1和应用对比例1相比，应用对比例1中微藻油含量比较少，且导致燕麦仁油和虾青素的含量过多，不在本公开范围内，使得虾青素组合物VII的乳液在高温、氙灯和室外光照颜色均由红橙色变浅呈淡橙色，也即虾青素被大部分降解。
应用实施例3和应用对比例2相比，应用对比例2中燕麦仁油的含量比较 少，导致微藻油的含量过多，不在本公开范围内，高温条件下含虾青素组合物VIII的乳液颜色和气味与室温保持一致，但氙灯和室外光颜色与室温比较变浅呈浅橙色，即虾青素出现一定程度的降解。
应用实施例4和应用对比例3相比，应用对比例3中的虾青素含量高，导致燕麦仁油的含量过低，不在本公开范围内，各条件下含虾青素组合物IX的乳液颜色均变浅，但气味未发生变化，也即该浓度范围内的微藻油和燕麦仁油只能保护部分的虾青素不被降解。同时由于虾青素含量高，虾青素组合物IX混匀需要更长的搅拌时间。
应用实施例5和应用对比例4相比，应用对比例4中微藻油用橄榄油替换，含虾青素组合物X的乳液在高温下颜色变浅即可以保护部分虾青素不被降解，但氙灯和室外光颜色褪色即虾青素被完全降解。
应用实施例5和应用对比例5相比，应用对比例5中微藻油和燕麦仁油用生育酚乙酸酯替换，含虾青素组合物XI的乳液在各条件下虾青素被降解褪色但无异味产生，然而氙灯和光照下因生育酚乙酸酯发生反应，使得乳液均出现发黄外观。
2、DPPH自由基清除试验----抗氧化测试
使用应用实施例1、3-4及应用对比例1-3进行相关测试
DPPH在有机溶剂中是一种稳定性的自由基，其醇溶液呈紫色，具有单一电子，可以捕获其他自由基，在波长517nm处有最大吸收。有自由基清除剂存在时，DPPH的单电子被捕捉而使其颜色变浅，在最大光吸收波长处吸光值下降，且下降程度呈线性关系，吸光度水平的降低表明抗氧化性能的增加，从而以评价试验样品的抗氧化能力。抗氧化能力用抑制率来表示，抑制率越大，抗氧化性越强。
将应用实施例1、3-4制备的含虾青素组合物I、III-IV乳液及应用对比例1-3制备的含虾青素组合物VI-IX乳液和对照组不含虾青素组合物乳液在三个条件下常温、高温和室外光测试结束的样品进行测试，观察对DPPH自由基清除效果，评估虾青素的抗氧化性能的变化。
将0.2mM的DPPH醇溶液和配制好的30mg/mL的各条件测试的含虾青素组合物和对照组的水溶液，按照1:1混合，上96孔板，每组3个复孔，37℃水浴恒温避光反应30min后，测517nm处的吸光度，计算每个样品的DPPH清除率，测试结果如图1所示。
清除率＝[1-(A 样品组-A 空白组)/A 对照组]×100％
A 样品组：样品溶液和DPPH醇溶液的吸光值；
A 空白组：样品溶液和无水乙醇的吸光值；
A 对照组：DPPH醇溶液和水的吸光值。
由图1可以看出，不含虾青素组合物的对照样品乳液因不含任何抗氧化剂，对DPPH自由基清除效果很差，也即对照样品无抗氧化活性。
应用实施例1、3-4制备的含虾青素组合物I、III-VI的乳液在室温、高温和室外光条件测试后其DPPH自由基清除率变化幅度很小，也即虾青素能在高温和室外光照条件下保持良好的抗氧化活性。
由图1所示，应用实施例1和应用对比例1相比，应用对比例1中微藻油含量比较少，且导致燕麦仁油和虾青素的含量过多，不在本公开范围内，使得虾青素组合物VII的乳液在高温和室外光照后DPPH自由基清除率下降，也即虾青素被降解其抗氧化活性明显下降。
应用实施例3和应用对比例2相比，应用对比例2中燕麦仁油的含量比较少，导致微藻油的含量过多，不在本公开范围内，高温条件下含虾青素组合物VIII的乳液和常温下DPPH自由基清除率变化不明显，但室外光照和室温比较可见，虾青素出现一定程度的降解。
应用实施例4和应用对比例3相比，应用对比例3中的虾青素含量高，导致燕麦仁油的含量过低，不在本公开范围内，各条件下含虾青素组合物IX的乳液均保持一定的自由基清除效果，也即该浓度范围内的微藻油和燕麦仁油只能保护部分的虾青素不被降解，保持一部分的抗氧化活性。
本公开的上述实施例仅仅是为清楚地说明本公开所作的举例，而并非是 对本公开的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本公开的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本公开权利要求的保护范围之内。

Claims (10)

  1. 一种虾青素组合物，其特征在于，以所述虾青素组合物的总质量计，包括以下组分：
    微藻油：25-50％；
    燕麦仁油：45-70％；
    虾青素：0.01-5％。
  2. 根据权利要求1所述的是虾青素组合物，其特征在于，以所述虾青素组合物的总质量计，所述微藻油的加入量为30-50％，所述燕麦仁油的加入量为50-70％，所述虾青素的加入量为0.05-5％。
  3. 根据权利要求1或2所述的虾青素组合物，其特征在于，所述微藻油、燕麦仁油和虾青素的重量比为1:(0.9～2.8):(0.0002～0.2)；优选1:(1～2.3):(0.0017～0.2)。
  4. 一种根据权利要求1-3任一项所述的虾青素组合物的制备方法，其特征在于，包括将所述虾青素组合物各组分混合的步骤。
  5. 一种乳化体系，其特征在于，包括权利要求1-3任一项所述的虾青素组合物；优选地，以所述乳化体系的总质量计，所述虾青素组合物的加入量为0.01-10％。
  6. 根据权利要求5所述的乳化体系，其特征在于，所述乳化体系还包含乳化剂、油脂、增稠剂、保湿剂、防腐剂中的一种或两种以上的组合。
  7. 根据权利要求6所述的乳化体系，其特征在于，以所述乳化体系的总质量计，所述乳化剂的加入量为0.01-5％；所述油脂的加入量为0.1-40％；所述增稠剂的加入量为0.01-5％；所述保湿剂的加入量为0.01-20％；所述防腐剂的加入量为0.01-2％。
  8. 根据权利要求5-7任一项所述的乳化体系的制备方法，其特征在于，包括将所述乳化体系的各组分混合的步骤。
  9. 一种根据权利要求1-3任一项所述的虾青素组合物或者根据权利要求 5-7任一项所述的乳化体系在护肤品或化妆品中的应用。
  10. 根据权利要求9所述的应用，其特征在于，所述护肤品或化妆品包括乳液、精华液、睡眠面膜、面霜、润肤油、按摩膏、唇膏、口红中的一种或两种以上的组合。
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