WO2021104144A1 - 一种基于植物甾醇稳定的油包水型Pickering乳液的制备方法 - Google Patents

一种基于植物甾醇稳定的油包水型Pickering乳液的制备方法 Download PDF

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WO2021104144A1
WO2021104144A1 PCT/CN2020/130009 CN2020130009W WO2021104144A1 WO 2021104144 A1 WO2021104144 A1 WO 2021104144A1 CN 2020130009 W CN2020130009 W CN 2020130009W WO 2021104144 A1 WO2021104144 A1 WO 2021104144A1
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phytosterol
water
oil
pickering emulsion
ethanol
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PCT/CN2020/130009
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English (en)
French (fr)
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刘付
蓝漫钰
欧仕益
汪勇
郑洁
黄才欢
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暨南大学
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Publication of WO2021104144A1 publication Critical patent/WO2021104144A1/zh
Priority to ZA2022/00292A priority Critical patent/ZA202200292B/en

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • A23L33/11—Plant sterols or derivatives thereof, e.g. phytosterols
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/28—Steroids, e.g. cholesterol, bile acids or glycyrrhetinic acid
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • A61K8/064—Water-in-oil emulsions, e.g. Water-in-silicone emulsions
    • 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
    • A61K8/63—Steroids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/10—Dispersions; Emulsions
    • A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
    • 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
    • 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
    • A61K2800/10—General cosmetic use

Definitions

  • the invention belongs to the field of water-in-oil emulsions, and particularly relates to a water-in-oil Pickering emulsion based on phytosterol stability, and a preparation method and application thereof.
  • Water-in-oil emulsion is an important type of emulsion system, which has broad application prospects in food, chemical and other related fields.
  • margarine is a water-in-oil emulsion used to replace animal butter, and most cosmetic creams are also water-in-oil emulsions.
  • Water-in-oil emulsions are also good embedding carriers for water-soluble active substances.
  • the emulsion based on particle stability (ie Pickering emulsion) has the advantages of small amount of emulsifier, high emulsion stability and no surfactant.
  • Most of the particles used to stabilize Pickering emulsions are inorganic and organic synthetic particles, and their applications in food, medicine and other industries are very limited.
  • some food-grade or bio-derived particles have been found to be used to stabilize Pickering emulsions, they are used to stabilize oil-in-water emulsions.
  • Phytosterols are a series of natural compounds that have a cholesterol-like structure and lower blood cholesterol. It is generally believed that taking 2-3g of plant sterols daily can effectively reduce blood low-density lipoprotein by 10-15%. However, its low water solubility and even fat solubility greatly limit its application in food and pharmaceutical oral preparations. At present, the following methods are mainly used to improve its solubility and bioavailability: 1) esterification with fatty acids to increase its fat solubility; 2) forming nanoparticles in the presence of stabilizers; 3) embedding in an oil-in-water emulsion.
  • phytosterols as emulsion (especially water-in-oil type) stabilizers, except for a few protein-stabilized phytosterol particles.
  • the water-in-oil Pickering emulsion based on phytosterol stability is not only natural and safe, but also functional in itself, and can be used to embed water-soluble active substances. It has great application prospects in the food, medicine and cosmetic industries.
  • the particles used to stabilize the water-in-oil Pickering emulsion are mainly synthetic particles, such as hydrophobic silicon particles, modified cellulose, polystyrene colloidal particles, microgels, etc.
  • the particles used to stabilize the water-in-oil Pickering emulsion are mainly synthetic particles, such as hydrophobic silicon particles, modified cellulose, polystyrene colloidal particles, microgels, etc.
  • biocompatibility such as food, medicine, cosmetics, etc.
  • the primary purpose of the present invention is to provide a method for preparing a water-in-oil Pickering emulsion based on phytosterol stability.
  • Another object of the present invention is to provide a water-in-oil Pickering emulsion based on phytosterol stabilized by the above method.
  • a preparation method of water-in-oil Pickering emulsion based on phytosterol stability which comprises the following steps:
  • step (3) Mix the aqueous dispersion of phytosterol particles obtained in step (2) with the oil phase, and obtain a water-in-oil Pickering emulsion through homogenization;
  • step (2) Dry the aqueous dispersion of the phytosterol particles obtained in step (2) to obtain phytosterol powder, disperse the phytosterol powder in the oil phase, and mix with water to obtain a water-in-oil Pickering emulsion through homogenization.
  • the plant sterols described in step (1) preferably refer to plant sterols with a total sterol content of ⁇ 95%.
  • the sterol is a mixture of one or more of ⁇ -sitosterol, campesterol, rapeseed sterol and stigmasterol, preferably a mixture of ⁇ -sitosterol, campesterol, rapeseed sterol and stigmasterol.
  • the commercial price of mixed sterols is significantly lower than that of high-purity sterols, so the use of mixed phytosterols has more industrial and commercial significance.
  • the heating and dissolving in step (1) is preferably heating at 45-85°C for 5-10 minutes to obtain an ethanol solution of phytosterol, preferably heating at 45°C for 10 minutes;
  • step (1) The amount of phytosterol and ethanol mentioned in step (1) meets the following requirements: 0.05 ⁇ 0.12kg of phytosterol powder is added to each 10L of absolute ethanol, preferably 0.08 ⁇ 0.10kg is added to every 10L of absolute ethanol.
  • Phytosterol powder 0.05 ⁇ 0.12kg of phytosterol powder is added to each 10L of absolute ethanol, preferably 0.08 ⁇ 0.10kg is added to every 10L of absolute ethanol.
  • step (2) The amount of the ethanol solution of phytosterol and water in step (2) meets that the volume ratio of the ethanol solution of phytosterol and water is 1-8:9-2;
  • step (2) The mixing described in step (2) is preferably carried out by homogenizing for 1 to 4 minutes under the condition of 1000 to 10000 revolutions per minute;
  • the removal of ethanol in step (2) is preferably to remove ethanol by rotary evaporation and concentrate to 2 to 4% (kg phytosterol/L water);
  • the oil phases described in step (3) and step (4) are relatively independently non-polar solvents or vegetable oils; the vegetable oils are preferably at least one of soybean oil, corn oil and blended oil.
  • the non-polar solvent is preferably at least one of n-hexane, dodecane and ethyl acetate;
  • the volume ratio of the aqueous dispersion of phytosterol particles to the oil phase in step (3) is 3-7:7-3;
  • step (3) and step (4) refers to homogenization for 1 to 3 minutes under the condition of 1,000 to 10,000 revolutions per minute;
  • the amount of the phytosterol powder and the oil phase for dispersing the phytosterol powder in the oil phase in step (4) meets: set the saturation concentration of the phytosterol in the oil phase at room temperature to X% w/v, where w is The unit is kg, and the unit of v is L, then (X+0.5) kg or more of phytosterol powder is added to each 100L of the oil phase to form a dispersion; the amount of water described in step (4) meets: phytosterol
  • the volume ratio of the dispersion liquid formed by dispersing the powder in the oil phase to water is 3-7:7-3, preferably 3-5:7-5.
  • a water-in-oil Pickering emulsion based on phytosterol stabilized prepared by the above method.
  • the above-mentioned phytosterol-stabilized water-in-oil Pickering emulsion can be used not only as a nutritious food product, but also as an embedding carrier for many water-soluble active substances, and is widely used in the development of functional (health) foods, medicines and cosmetics, etc. .
  • the present invention can be used to produce a water-in-oil Pickering emulsion containing a polypeptide active substance to improve the stability of the active substance.
  • the mechanism of the present invention is:
  • the anti-solvent precipitation method is used to prepare water-dispersed phytosterol particles.
  • the phytosterol undergoes self-assembly (partially hydrophilic groups are exposed) to achieve a slight change in surface wettability, from extremely hydrophobic to relatively hydrophobic, thereby stabilizing the oil Water-in-water Pickering emulsion.
  • Water-dispersible phytosterol particles can also be freeze-dried to form phytosterol particle powder, which still has a certain degree of amphiphilicity (mainly hydrophobic) and can be used for the stabilization of water-in-oil Pickering emulsions.
  • the present invention has the following advantages and beneficial effects:
  • the present invention uses a new production process without any additional stabilizers to produce a stable water-in-oil Pickering emulsion.
  • the process solves the shortcomings of the existing water-in-oil Pickering emulsion stabilizer preparation process.
  • the production process involved in the present invention is not only simple, efficient, and low in production cost, but also environmentally friendly, safe, and suitable for industrialized production.
  • the water-in-oil Pickering emulsion produced by the present invention can be used not only as a nutritious food product, but also as an embedding carrier for many water-soluble active substances, and is widely used in the development of functional (health) foods, medicines, and cosmetics.
  • the water-in-oil Pickering emulsion containing a polypeptide active substance produced by the present invention is expected to greatly improve the stability of the active substance.
  • the quality of the water-in-oil Pickering emulsion produced by the present invention can be adjusted by the sterol particle concentration, water phase ratio and oil phase type, and its specific formula can also be easily adjusted according to actual needs, so as to produce a series of properties Different water-in-oil Pickering emulsions.
  • Figure 1 is a schematic diagram of the mechanism of the present invention
  • Example 2 is the appearance and optical microscope image of the water-in-oil Pickering emulsion prepared in Example 1;
  • Example 3 is the appearance and optical microscope image of the water-in-oil Pickering emulsion prepared in Example 2;
  • Example 4 is the appearance and optical microscope image of the water-in-oil Pickering emulsion prepared in Example 3;
  • Example 5 is the appearance and optical microscope image of the water-in-oil Pickering emulsion prepared in Example 4.
  • reagents used in the examples can be conventionally purchased from the market unless otherwise specified.
  • Plant sterols (purchased from Shaanxi Haisifu Biological Engineering Co., Ltd., with a solid-liquid ratio of 1:100 at room temperature, with total sterol content ⁇ 95%, ⁇ -sitosterol 55%, campesterol 30%, and stigmasterol 10 %, rapeseed sterol 0.49%) was dispersed in absolute ethanol, and then heated at 45°C for 5 minutes to obtain an ethanol solution of plant sterols; the solid-liquid ratio in the solid dosage unit is kilograms, and the liquid dosage unit is liters.
  • the obtained emulsion sample is a water-in-oil emulsion, and particle size analysis shows that it is The average particle size is 88.3 microns, and the appearance and particle size of the emulsion do not change significantly after being left for one month.
  • Plant sterols (purchased from Shaanxi Haisifu Biological Engineering Co., Ltd., with a solid-liquid ratio of 1:100 at room temperature, total sterol content ⁇ 95%, ⁇ -sitosterol 55%, campesterol 30%, stigmasterol 10 %, rapeseed sterol 0.49%) was dispersed in anhydrous ethanol, and then heated at 85°C for 5 minutes to obtain an ethanol solution of plant sterols; the solid dosage unit in the solid-liquid ratio is kilograms, and the liquid dosage unit is liters.
  • the appearance and optical microscope picture of the water-in-oil Pickering emulsion prepared in Example 2 after being left for 1 day are shown in Figure 3.
  • the obtained emulsion sample is a water-in-oil emulsion, and particle size analysis shows it The average particle size is 33.3 microns, and there is no significant change in the appearance and particle size of the emulsion after 1 month.
  • Plant sterols (purchased from Shaanxi Haisifu Biological Engineering Co., Ltd., with a solid-liquid ratio of 1:100 at room temperature, total sterol content ⁇ 95%, ⁇ -sitosterol 55%, campesterol 30%, stigmasterol 10 %, rapeseed sterol 0.49%) was dispersed in absolute ethanol, and then heated at 45°C for 5 minutes to obtain an ethanol solution of plant sterols; the solid-liquid ratio in the solid dosage unit is kilograms, and the liquid dosage unit is liters.
  • the obtained emulsion sample is a water-in-oil emulsion; particle size analysis shows it The average particle size is 27.4 microns; there is no significant change in the appearance and particle size of the emulsion after 1 month.
  • Plant sterols (purchased from Shaanxi Haisifu Biological Engineering Co., Ltd., with a solid-liquid ratio of 1:100 at room temperature, with total sterol content ⁇ 95%, ⁇ -sitosterol 55%, campesterol 30%, and stigmasterol 10 %, rapeseed sterol 0.49%) was dispersed in absolute ethanol, and then heated at 45°C for 5 minutes to obtain an ethanol solution of plant sterols; the solid-liquid ratio in the solid dosage unit is kilograms, and the liquid dosage unit is liters.
  • the phytosterol granules obtained above are dispersed in dodecane at a concentration of 2% w/v (the saturated concentration of sterol in dodecane at room temperature is 0.55% w/v), and the volume ratio is 5:5 with water. After mixing, homogenously dispersing by a high-speed shearing machine for 2 minutes at a rotation speed of 5000 rpm, to obtain a water-in-oil Pickering emulsion.
  • the unit of w is kilogram, and the unit of v is liter.
  • the obtained emulsion sample is a water-in-oil emulsion; particle size analysis shows it The average particle size is 41.9 microns; there is no significant change in the appearance and particle size of the emulsion after 1 month.

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Abstract

一种基于植物甾醇稳定的油包水型Pickering乳液及其制备方法和应用。油包水型Pickering乳液由以下方法制备得到：将植物甾醇分散于无水乙醇中，加热溶解得到植物甾醇的乙醇溶液，然后与水混合再除去乙醇，得到植物甾醇颗粒的水分散液，将水分散液与油相混合均质即得到油包水Pickering乳液；或者将水分散液干燥得到植物甾醇粉末，将植物甾醇粉末分散于油相中，再与水混合，通过均质得到油包水Pickering乳液。

Description

一种基于植物甾醇稳定的油包水型Pickering乳液的制备方法 技术领域
本发明属于油包水乳液领域，特别涉及一种基于植物甾醇稳定的油包水型Pickering乳液及其制备方法和应用。
背景技术
油包水型乳液是一类重要的乳浊液体系类型，在食品、化工及其他相关领域具有广泛的应用前景。譬如，人造黄油就是一种油包水型乳液用于替代动物性黄油，而大多数的化妆霜也是油包水型乳液。油包水乳液也是很好的水溶活性物质包埋载体。
传统上形成油包水乳液需要使用大量的表面活性剂，会产生环境问题及安全问题。基于颗粒稳定的乳液(即Pickering乳液)具有乳化剂用量少、乳液稳定性高且无表面活性剂等优点。目前用于Pickering乳液稳定的颗粒多为无机及有机合成颗粒，在食品、医药等行业应用十分受限。尽管一些食品级或生物来源颗粒已被发现可以用于Pickering乳液稳定，但用于稳定水包油型乳液。能用于油包水型Pickering乳液的食品级颗粒非常少，仅有脂肪结晶、多酚晶体等。
植物甾醇是具有类似胆固醇结构具有降血液胆固醇的一系列天然化合物。一般认为每天服用2-3g的植物甾醇可以有效降低血液低密度脂蛋白10-15％。然而其低水溶性甚至脂溶性极大地限制了其在食品及医药口服制剂中的应用。目前主要通过以下手段来提高其溶解度及生物利用度：1)与脂肪酸酯化提高其脂溶性；2)在稳定剂存在下形成纳米颗粒；3)包埋于水包油乳液当中。然而利用植物甾醇作为乳液(尤其是油包水型)稳定剂的研究非常少，除了少数蛋白稳定的植物甾醇颗粒外。基于植物甾醇稳定的油包水型Pickering乳液不仅天然安全，而且本身具有功能性，且可以用于包埋水溶活性物质，在食品、 医药及化妆品等行业均有巨大的应用前景。
尽管如此，国内外在食品级油包水型Pickering乳液方面研究仍进展不大。究其原因，是可以用于稳定油包水型Pickering乳液的食品级颗粒的缺乏。目前用于油包水型Pickering乳液稳定的颗粒主要是合成颗粒，如疏水性硅颗粒、改性纤维素、聚苯乙烯胶粒、微胶等。然而对于要求生物兼容性的软材料应用领域如食品、医药、化妆品等，亟需开发一类基于天然、可降解及可再生资源得到的Pickering乳液稳定剂。
发明内容
为了克服上述现有技术的缺点与不足，本发明的首要目的在于提供一种基于植物甾醇稳定的油包水型Pickering乳液的制备方法。
本发明另一目的在于提供上述方法制备的基于植物甾醇稳定的油包水型Pickering乳液。
本发明的目的通过下述方案实现：
一种基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其包括以下步骤：
(1)将植物甾醇分散于无水乙醇中，加热溶解得到植物甾醇的乙醇溶液；
(2)将步骤(1)中得到的植物甾醇的乙醇溶液和水混合，然后除去乙醇，得到植物甾醇颗粒的水分散液；
(3)将步骤(2)中得到的植物甾醇颗粒的水分散液与油相混合，通过均质得到油包水Pickering乳液；
或者，
(4)将步骤(2)中得到的植物甾醇颗粒的水分散液干燥得到植物甾醇粉末，将植物甾醇粉末分散于油相中，再与水混合，通过均质得到油包水Pickering乳液。
植物甾醇是从植物中经过物理提纯而得的，来源及甾醇纯度对终产品品质影响不明显。相对而言，在总甾醇含量相同情况下，采用高纯度甾醇生产的乳液粒径更加均匀，因此步骤(1)中所述的植物甾醇优选指总甾醇含量≥95％ 的植物甾醇，其中的植物甾醇为β-谷甾醇、菜油甾醇、菜籽甾醇和豆甾醇中的一种或多种混合，优选为β-谷甾醇、菜油甾醇、菜籽甾醇和豆甾醇的混合物。但是，混合甾醇的商用价格明显低于高纯度甾醇，因而选用混合植物甾醇更具有工业及商业意义。
步骤(1)中所述的加热溶解优选为在45～85℃加热5～10min至得到植物甾醇的乙醇溶液，优选为在45℃加热10min；
步骤(1)中所述的植物甾醇和乙醇的用量满足：每10L的无水乙醇中对应加入0.05～0.12kg的植物甾醇粉末，优选为每10L的无水乙醇中对应加入0.08～0.10kg的植物甾醇粉末；
步骤(2)中所述的植物甾醇的乙醇溶液和水的用量满足植物甾醇的乙醇溶液和水的体积比为1～8:9～2；
步骤(2)中所述的混合优选为通过在1000～10000转/分的条件下均质1～4分钟进行混合；
步骤(2)中所述的除去乙醇优选为通过旋转蒸发除去乙醇并浓缩至2～4％(kg植物甾醇/L水)；
步骤(3)和步骤(4)中所述的油相均相对独立地为非极性溶剂或植物油；所述的植物油优选为大豆油、玉米油和调和油中的至少一种，所述的非极性溶剂优选为正己烷、十二烷和乙酸乙酯中的至少一种；
步骤(3)中所述的植物甾醇颗粒的水分散液与油相的体积比为3～7:7～3；
步骤(3)和步骤(4)中所述的均质是指在1000～10000转/分的条件下均质1～3分钟；
步骤(4)中所述的将植物甾醇粉末分散于油相中植物甾醇粉末和油相的用量满足：设定常温下植物甾醇在油相中的饱和浓度为X％w/v，其中w的单位为kg，v的单位为L，则每100L的油相中对应加入大于等于(X+0.5)kg的植物甾醇粉末形成分散液；步骤(4)中所述的水的用量满足：植物甾醇粉末分散于油相中形成的分散液与水的体积比为3～7:7～3，优选为3～5:7～5。
一种由上述方法制备得到的基于植物甾醇稳定的油包水型Pickering乳液。
上述的基于植物甾醇稳定的油包水型Pickering乳液不仅可作为一种营养 食品制品，而且还可作为诸多水溶活性物质的包埋载体，广泛用于功能(保健)食品、药品及化妆品等的开发。例如，本发明可以用于生产含多肽类活性物质的油包水Pickering乳液，以提高该活性物质的稳定性。
本发明的机理为：
利用反溶剂沉淀法制备水分散植物甾醇颗粒，在此过程中植物甾醇经过自组装(部分亲水基团暴露)实现表面润湿性的轻微改变，由极其疏水变得相对疏水，进而能够稳定油包水型Pickering乳液。水分散植物甾醇颗粒也可以通过冷冻干燥形成植物甾醇颗粒粉末，该粉末仍然具有一定的两亲性(疏水性为主)，能够用于油包水型Pickering乳液的稳定。
本发明相对于现有技术，具有如下的优点及有益效果：
1.本发明以一种新的生产工艺，不需要任何额外的稳定剂，生产出稳定性好的油包水型Pickering乳液。该工艺解决了现有油包水Pickering乳液稳定剂制备工艺存在的不足。
2.本发明涉及的生产工艺不仅简单、高效，生产成本低，而且环保、安全，适合工业化生产。
3.本发明生产的油包水型Pickering乳液不仅可作为一种营养食品制品，而且还可作为诸多水溶活性物质的包埋载体，广泛用于功能(保健)食品、药品及化妆品等的开发。例如本发明可以生产的含多肽类活性物质的油包水Pickering乳液，预计能极大的提高该活性物质的稳定性。
4.本发明生产的油包水型Pickering乳液的品质可以通过甾醇颗粒浓度、水相比例及油相种类进行调节，其具体配方也可以方便地根据实际需求进行调整，从而可以生产出一系列性质不同的油包水型Pickering乳液。
附图说明
图1为本发明的机理示意图；
图2为实施例1制备得到的油包水型Pickering乳液的外观和光学显微镜图；
图3为实施例2制备得到的油包水型Pickering乳液的外观和光学显微镜 图；
图4为实施例3制备得到的油包水型Pickering乳液的外观和光学显微镜图；
图5为实施例4制备得到的油包水型Pickering乳液的外观和光学显微镜图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例中所用试剂如无特殊说明均可从市场常规购得。
实施例1
(1)常温下按照固液比1:100将植物甾醇(购买自陕西海斯夫生物工程有限公司，其中总甾醇含量≥95％，β-谷甾醇55％，菜油甾醇30％，豆甾醇10％，菜籽甾醇0.49％)分散于无水乙醇中，然后45℃加热5min，得到植物甾醇的乙醇溶液；所述固液比中固体用量单位为千克，液体用量单位为升。
(2)对上述植物甾醇的乙醇溶液按体积比5:5与水混合，同时加以剪切均质10000转/分2min，通过旋转蒸发去除乙醇，并浓缩至3％w/v得到高浓度植物甾醇颗粒的水分散液；所述w单位为千克，v单位为升；
(3)上述植物甾醇颗粒的水分散液以体积比5:5与玉米油混合，在转速为5000转/分钟的条件下，经高速剪切机均质分散2分钟，即得到油包水型Pickering乳液。经染色实验及光学显微镜观察，实施例1制备得到的油包水型Pickering乳液放置1天后的外观和光学显微镜图如图2所示，所得乳液样品为油包水型乳液，粒径分析表明其平均粒径为88.3微米，且乳液放置1月外观和粒径无明显变化。
实施例2
(1)常温下按照固液比1:100将植物甾醇(购买自陕西海斯夫生物工程 有限公司，其中总甾醇含量≥95％，β-谷甾醇55％，菜油甾醇30％，豆甾醇10％，菜籽甾醇0.49％)分散于无水乙醇中，然后85℃加热5min，得到植物甾醇的乙醇溶液；所述固液比中固体用量单位为千克，液体用量单位为升。
(2)上述植物甾醇的乙醇溶液按体积比5:5与水混合，同时加以剪切均质8000转/分4min，通过旋转蒸发去除乙醇，并浓缩至2％w/v得到高浓度植物甾醇颗粒的水分散液；所述w单位为千克，v单位为升。
(3)上述得到高浓度植物甾醇颗粒的水分散液以体积比5:5与十二烷混合，在转速为5000转/分钟的条件下，经高速剪切机均质分散2分钟，即得到油包水型Pickering乳液。
经染色实验及光学显微镜观察，实施例2制备得到的油包水型Pickering乳液放置1天后的外观和光学显微镜图如图3所示，所得乳液样品为油包水型乳液，粒径分析表明其平均粒径为33.3微米，且乳液放置1月外观和粒径无明显变化。
实施例3
(1)常温下按照固液比1:100将植物甾醇(购买自陕西海斯夫生物工程有限公司，其中总甾醇含量≥95％，β-谷甾醇55％，菜油甾醇30％，豆甾醇10％，菜籽甾醇0.49％)分散于无水乙醇中，然后45℃加热5min，得到植物甾醇的乙醇溶液；所述固液比中固体用量单位为千克，液体用量单位为升。
(2)上述植物甾醇的乙醇溶液按体积比3:7与水混合，同时加以剪切均质1000转/分2min，通过旋转蒸发去除乙醇，并浓缩至3％w/v得到高浓度植物甾醇颗粒的水分散液；所述w单位为千克，v单位为升。
(3)上述得到高浓度植物甾醇颗粒的水分散液以体积比7:3与十二烷混合，在转速为7000转/分钟的条件下，经高速剪切机均质分散2分钟，即得到油包水型Pickering乳液。
经染色实验及光学显微镜观察，实施例3制备得到的油包水型Pickering乳液放置1天后的外观和光学显微镜图如图4所示，所得乳液样品为油包水型乳液；粒径分析表明其平均粒径为27.4微米；乳液放置1月外观和粒径无 明显变化。
实施例4
(1)常温下按照固液比1:100将植物甾醇(购买自陕西海斯夫生物工程有限公司，其中总甾醇含量≥95％，β-谷甾醇55％，菜油甾醇30％，豆甾醇10％，菜籽甾醇0.49％)分散于无水乙醇中，然后45℃加热5min，得到植物甾醇的乙醇溶液；所述固液比中固体用量单位为千克，液体用量单位为升。
(2)上述植物甾醇的乙醇溶液按5:5与水混合，同时加以剪切均质10000转/分2min，通过旋转蒸发去除乙醇，并浓缩至3.5％w/v得到高浓度植物甾醇颗粒的水分散液；所述w单位为千克，v单位为升。
(3)将上述分散液经冷冻干燥，得到植物甾醇颗粒粉末。
(4)上述得到植物甾醇颗粒粉末以2％w/v(室温下甾醇在十二烷中的饱和浓度为0.55％w/v)浓度分散于十二烷中，以体积比5:5与水混合，在转速为5000转/分钟的条件下，经高速剪切机均质分散2分钟，即得到油包水型Pickering乳液。所述w单位为千克，v单位为升。
经染色实验及光学显微镜观察，实施例4制备得到的油包水型Pickering乳液放置1天后的外观和光学显微镜图如图5所示，所得乳液样品为油包水型乳液；粒径分析表明其平均粒径为41.9微米；乳液放置1月外观和粒径无明显变化。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

  1. 一种基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于包括如下步骤：
    (1)将植物甾醇分散于无水乙醇中，加热溶解得到植物甾醇的乙醇溶液；
    (2)将步骤(1)中得到的植物甾醇的乙醇溶液和水混合，然后除去乙醇，得到植物甾醇颗粒的水分散液；
    (3)将步骤(2)中得到的植物甾醇颗粒的水分散液与油相混合，通过均质得到油包水Pickering乳液；
    或者，
    (4)将步骤(2)中得到的植物甾醇颗粒的水分散液干燥得到植物甾醇粉末，将植物甾醇粉末分散于油相中，再与水混合，通过均质得到油包水Pickering乳液。
  2. 根据权利要求1所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    步骤(1)中所述的植物甾醇为总甾醇含量≥95％的植物甾醇。
  3. 根据权利要求2所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    步骤(1)中所述的植物甾醇为β-谷甾醇、菜油甾醇、菜籽甾醇和豆甾醇中的至少一种。
  4. 根据权利要求1所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    步骤(1)中所述的加热溶解指在45～85℃加热5～10min至得到植物甾醇的乙醇溶液；
    步骤(1)中所述的植物甾醇和乙醇的用量满足：每10L的无水乙醇中对应加入0.05～0.12kg的植物甾醇粉末。
  5. 根据权利要求1所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    步骤(2)中所述的植物甾醇的乙醇溶液和水的用量满足植物甾醇的乙醇 溶液和水的体积比为1～8:9～2；
    步骤(2)中所述的混合指通过在1000～10000转/分的条件下均质1～4分钟进行混合；
    步骤(2)中所述的除去乙醇指通过旋转蒸发除去乙醇并浓缩至2～4kg植物甾醇/100L水。
  6. 根据权利要求1所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    步骤(3)中所述的油相为非极性溶剂或植物油；
    步骤(3)中所述的植物甾醇颗粒的水分散液与油相的体积比为3～7:7～3；
    步骤(3)中所述的均质是指在1000～10000转/分的条件下均质1～3分钟。
  7. 根据权利要求1所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    步骤(4)中所述的油相为非极性溶剂或植物油；
    步骤(4)中所述的均质是指在1000～10000转/分的条件下均质1～3分钟；
    步骤(4)中所述的将植物甾醇粉末分散于油相中植物甾醇粉末和油相的用量满足：设定常温下植物甾醇在油相中的饱和浓度为X％w/v，其中w的单位为kg，v的单位为L，则每100L的油相中对应加入大于等于(X+0.5)kg的植物甾醇粉末形成分散液；步骤(4)中所述的水的用量满足：植物甾醇粉末分散于油相中形成的分散液与水的体积比为3～7:7～3。
  8. 根据权利要求6或7所述的基于植物甾醇稳定的油包水型Pickering乳液的制备方法，其特征在于：
    所述的植物油为大豆油、玉米油和调和油中的至少一种，所述的非极性溶剂为正己烷、十二烷和乙酸乙酯中的至少一种。
  9. 一种根据权利要求1～8任一项所述的方法制备得到的基于植物甾醇稳定的油包水型Pickering乳液。
  10. 根据权利要求9所述的基于植物甾醇稳定的油包水型Pickering乳液作为营养食品制品以及水溶活性物质的包埋载体的应用。
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