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CN111616366A - A kind of preparation method of nervonic acid nanoemulsion - Google Patents

A kind of preparation method of nervonic acid nanoemulsion Download PDF

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CN111616366A
CN111616366A CN202010317471.0A CN202010317471A CN111616366A CN 111616366 A CN111616366 A CN 111616366A CN 202010317471 A CN202010317471 A CN 202010317471A CN 111616366 A CN111616366 A CN 111616366A
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nervonic acid
emulsifier
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李梅
靳毓
徐怀德
宗浩
雷宏杰
王军
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Tengzhou Qiangqiang Guoren Food Co ltd
Northwest A&F University
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
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    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract

本发明提供了一种神经酸纳米乳液的制备方法,包括以下步骤:1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相;2)制备油相:分别称量神经酸和载油,将神经酸充分溶解于载油中形成油相;3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌,然后高速剪切,形成粗乳液;4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液。本发明的制备方法,不破坏神经酸本身营养、功能价值,同时又能提高神经酸水溶性的纳米乳液,以提高其在功能食品中的应用。The invention provides a preparation method of nervonic acid nanoemulsion, which includes the following steps: 1) preparing water phase: weighing emulsifier, adding the emulsifier into deionized water for stirring, and fully hydrating to form a water phase; 2) preparing oil Phase: respectively weigh nervonic acid and carrier oil, and fully dissolve nervonic acid in carrier oil to form an oil phase; 3) Prepare crude milk: add the oil phase obtained in step 2) dropwise to the water obtained in step 1) while stirring In the phase, continue stirring after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion; 4) Preparation of nanoemulsion: The coarse emulsion obtained in step 3) is subjected to high pressure homogenization, and then cooled to room temperature after homogenization to obtain nervonic acid Nanoemulsion. The preparation method of the invention does not destroy the nutritional and functional value of the nervonic acid itself, and at the same time can improve the water-soluble nano-emulsion of the nervonic acid, so as to improve its application in functional foods.

Description

一种神经酸纳米乳液的制备方法A kind of preparation method of nervonic acid nanoemulsion

技术领域technical field

本发明涉及纳米微乳的制备领域,具体涉一种神经酸纳米乳液的制备方法。The invention relates to the field of preparation of nano-microemulsion, in particular to a preparation method of nervonic acid nano-emulsion.

背景技术Background technique

神经酸(Nervonic acid, NA)因最早发现于哺乳动物的神经组织中而被命名为神经酸,其化学名称为二十四碳烯酸。我国老龄化日趋严峻,神经退行性疾病的发病率也将急剧增加,而神经酸是人体大脑发育的必须营养物质,有望成为新型的益脑益智功能性成分。由于人体自身很难合成神经酸,一般需要体外摄取,而神经酸的熔点为39 ~ 40 ℃,常温下为白色粉末,不宜直接摄取;此外神经酸是一种长链不饱和脂肪酸,能溶于醇,不溶于水,在肠道水环境中的扩散性较差,限制了其通过口服方式摄取的生物利用率;而目前神经酸的营养补充剂为功能性油的系列产品,载体形式较单一,不适应油脂限制摄入的人群,从而极大地限制了神经酸在功能食品中的应用。Nervonic acid (NA) is named nervonic acid because it was first discovered in mammalian nerve tissue, and its chemical name is tetracosenoic acid. my country's aging is becoming more and more severe, and the incidence of neurodegenerative diseases will also increase sharply. Nervous acid is an essential nutrient for human brain development, and is expected to become a new functional ingredient for brain and intelligence. Since it is difficult for the human body to synthesize nervonic acid, it generally needs to be ingested in vitro, while the melting point of nervonic acid is 39 ~ 40 ℃, and it is a white powder at room temperature, so it should not be ingested directly; Alcohol, insoluble in water, has poor diffusivity in the intestinal water environment, which limits its bioavailability through oral intake; while the current nutritional supplements of nervonic acid are a series of functional oil products, and the carrier form is relatively simple , which are not suitable for people with restricted intake of fats, thus greatly limiting the application of nervonic acid in functional foods.

纳米乳液是一种由水、油、表面活性剂组成、利用高能乳化法(高速剪切、高压均质、超声等)或低能乳化法(转相乳化法)制备而成的热力学稳定制剂。与传统乳液相比,纳米乳液中的小液滴使其具有更好的功能特性,例如改善聚集和乳析稳定性、小尺寸效应和表面效应、较高的光学清晰度、以及更好的控释及靶向性功能。其中水包油型(O/W)纳米乳液广泛用于包埋疏水性活性物质,以提高活性成分的溶解度、稳定性及生物利用度。Nanoemulsion is a thermodynamically stable preparation composed of water, oil and surfactant, prepared by high-energy emulsification (high-speed shearing, high-pressure homogenization, ultrasound, etc.) or low-energy emulsification (phase inversion emulsification). Compared with traditional emulsions, the small droplets in nanoemulsions enable them to have better functional properties, such as improved aggregation and emulsion stability, small size and surface effects, higher optical clarity, and better control. release and targeting functions. Among them, oil-in-water (O/W) nanoemulsions are widely used to embed hydrophobic active substances to improve the solubility, stability and bioavailability of active ingredients.

因此亟需一种在制备过程中不破坏神经酸自身营养、功能价值,同时又能提高神经酸水溶性的纳米乳液,以提高其在功能食品中的应用。Therefore, there is an urgent need for a nanoemulsion that does not destroy the nutritional and functional value of nervonic acid itself during the preparation process, and at the same time can improve the water-solubility of nervonic acid, so as to improve its application in functional foods.

发明内容SUMMARY OF THE INVENTION

要解决的技术问题:本发明的目的是提供神经酸纳米乳液的制备方法,不破坏神经酸本身营养、功能价值,同时又能提高神经酸水溶性的纳米乳液,以提高其在功能食品中的应用。Technical problem to be solved: the purpose of the present invention is to provide the preparation method of nervonic acid nanoemulsion, which does not destroy the nutrition and functional value of nervonic acid itself, and simultaneously can improve the water-soluble nanoemulsion of nervonic acid, so as to improve its performance in functional food. application.

技术方案:一种神经酸纳米乳液的制备方法,包括以下步骤:Technical scheme: a preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相;1) Prepare the water phase: weigh the emulsifier, add the emulsifier into deionized water and stir, and form the water phase after fully hydrating;

2)制备油相:分别称量神经酸和载油,将神经酸充分溶解于载油中形成油相;2) Preparation of the oil phase: Weigh the nervonic acid and the carrier oil respectively, and fully dissolve the nervonic acid in the carrier oil to form an oil phase;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌,然后高速剪切,形成粗乳液;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液。4) Preparation of nanoemulsion: the crude emulsion obtained in step 3) is subjected to high-pressure homogenization, and after homogenization, it is cooled to room temperature to obtain a nervonic acid nanoemulsion.

优选的,所述步骤1)中乳化剂包括水溶性乳化剂,所述水溶性乳化剂为动物蛋白、植物蛋白或非离子型乳化剂中任意一种。Preferably, in the step 1), the emulsifier includes a water-soluble emulsifier, and the water-soluble emulsifier is any one of animal protein, vegetable protein or non-ionic emulsifier.

优选的,所述动物蛋白为乳清分离蛋白,所述植物蛋白为大豆分离蛋白,所述非离子型乳化剂为吐温20。Preferably, the animal protein is whey protein isolate, the vegetable protein is soybean protein isolate, and the nonionic emulsifier is Tween 20.

优选的,所述步骤1)中乳化剂的浓度为0.5-2.0 w/v%,搅拌时间为10-12 h。Preferably, the concentration of the emulsifier in the step 1) is 0.5-2.0 w/v%, and the stirring time is 10-12 h.

优选地,所述步骤1)中乳化剂的浓度为1.5 w/v%Preferably, the concentration of the emulsifier in the step 1) is 1.5 w/v%

优选的,所述步骤2)中载油为中链甘油三酸酯。Preferably, the carrier oil in step 2) is medium chain triglyceride.

优选的,所述步骤2)中神经酸在油相中的浓度为0.1-3.0 mg/mL。Preferably, in the step 2), the concentration of nervonic acid in the oil phase is 0.1-3.0 mg/mL.

优选的,所述步骤2)中神经酸在油相中的浓度为0.5 mg/mL。Preferably, the concentration of nervonic acid in the oil phase in the step 2) is 0.5 mg/mL.

优选的,所述步骤2)中神经酸溶解于载油中的方式为超声波溶解,由于神经酸的熔点在39-40℃之间,常温下为固体粉末,采用超声波溶解的方式能够使得神经酸在载油中溶解。Preferably, in the step 2), the method of dissolving the nervonic acid in the carrier oil is ultrasonic dissolution. Since the melting point of the nervonic acid is between 39-40 °C, and it is a solid powder at room temperature, the method of ultrasonic dissolution can make the nervonic acid dissolve. Soluble in carrier oil.

优选的,所述步骤3)中油相和水相的质量比为1:9,滴加完成后继续搅拌时间为10min,高速剪切机的转速为30000 rpm。Preferably, in the step 3), the mass ratio of the oil phase to the water phase is 1:9, the stirring time is 10 min after the dropwise addition is completed, and the rotational speed of the high-speed shearing machine is 30,000 rpm.

优选的,所述步骤4)中均质压力设定为 90~130 MPa,均质的循环次数为3~5次。Preferably, in the step 4), the homogenization pressure is set to 90-130 MPa, and the number of cycles of homogenization is 3 to 5 times.

优选的,所述步骤4)中均质压力设定为120 MPa,均质的循环次数为5次。Preferably, in the step 4), the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is 5 times.

上述制备方法得到神经酸纳米乳液在功能食品领域的应用。The above preparation method obtains the application of the nervonic acid nanoemulsion in the field of functional food.

有益效果:本发明的神经酸纳米乳液的制备方法具有以下优点:Beneficial effect: the preparation method of the nervonic acid nanoemulsion of the present invention has the following advantages:

(1)本发明中的乳化剂可以提高神经酸的溶解度、稳定性和生物利用度;(1) The emulsifier in the present invention can improve the solubility, stability and bioavailability of nervonic acid;

(2)本发明中所使用的大豆分离蛋白价格低廉,来源于植物,乳化效率高,相比于动物来源的乳清分离蛋白和化学合成的吐温20更具有优势;(2) The soybean protein isolate used in the present invention is low in price, derived from plants, and has high emulsification efficiency, which is more advantageous than animal-derived whey protein isolate and chemically synthesized Tween 20;

(3)制备工艺简单,过程可控,安全环保,有利于形成水溶性好、神经酸负载率高、粒径较小、分散性较好的神经酸纳米乳液;(3) The preparation process is simple, the process is controllable, safe and environmentally friendly, and is conducive to the formation of a nervonic acid nanoemulsion with good water solubility, high nervonic acid loading rate, smaller particle size and better dispersibility;

(4)本发明为神经酸在功能性食品生产中的高值化应用提供新的视角;(4) The present invention provides a new perspective for the high-value application of nervonic acid in the production of functional food;

(5)本发明的制备方法不添加有毒有害试剂,绿色安全。(5) The preparation method of the present invention does not add toxic and harmful reagents, and is green and safe.

附图说明Description of drawings

图1为实施例1-3中不同乳化剂浓度对神经酸纳米乳液粒径的影响;Fig. 1 is the influence of different emulsifier concentration on the particle size of nervonic acid nanoemulsion in embodiment 1-3;

图2为实施例4-8中不同神经酸浓度对神经酸纳米乳液粒径的影响;Fig. 2 is the influence of different nervonic acid concentrations on the particle size of nervonic acid nanoemulsion in Examples 4-8;

图3为实施例9-13中不同均质压力条件对神经酸纳米乳液粒径的影响。Figure 3 shows the effect of different homogeneous pressure conditions on the particle size of the nervonic acid nanoemulsion in Examples 9-13.

具体实施方式Detailed ways

实施例1Example 1

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例2Example 2

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.0 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier into deionized water and stir, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.0 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例3Example 3

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为2.0 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier into deionized water and stir, and form a water phase after full hydration, wherein the concentration of the emulsifier is 2.0 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例1-3中,每个实施例均对不同类型的乳化剂进行试验,步骤1)中的乳化剂为乳清分离蛋白,大豆分离蛋白和吐温20中的任意一种。图1为不同浓度的乳化剂对神经酸乳液粒径的影响,不同字母表示在相同浓度条件下添加不同乳化剂的神经酸乳液粒径有显著性差异 (p < 0.05),在各浓度条件下,均得到稳定的神经酸纳米乳液。在相同浓度条件下,添加乳清分离蛋白的神经酸纳米乳液的粒径均大于添加大豆分离蛋白的神经酸纳米乳液,添加吐温20的神经酸纳米乳液粒径最小。除大豆分离蛋白神经酸纳米乳液的粒径随浓度增加而减小外,乳清分离蛋白和吐温20在其浓度为1.5 %时神经酸纳米乳液的粒径均最小,因此选取乳化剂浓度为1.5 %。In Examples 1-3, different types of emulsifiers are tested in each example, and the emulsifier in step 1) is any one of whey protein isolate, soybean protein isolate and Tween 20. Figure 1 shows the effect of different concentrations of emulsifiers on the particle size of nervonic acid emulsions. Different letters indicate that the particle sizes of nervonic acid emulsions with different emulsifiers added under the same concentration are significantly different (p < 0.05). , stable nervonic acid nanoemulsions were obtained. Under the same concentration conditions, the particle size of the nervonic acid nanoemulsion added with whey protein isolate was larger than that of the soy protein isolate, and the particle size of the nervonic acid nanoemulsion with Tween 20 was the smallest. Except that the particle size of soybean protein isolate nervonic acid nanoemulsion decreases with the increase of concentration, the particle size of whey protein isolate and Tween 20 is the smallest when its concentration is 1.5%, so the emulsifier concentration is selected as 1.5%.

实施例4Example 4

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.1 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.1 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例5Example 5

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例6Example 6

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为1.0 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 1.0 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例7Example 7

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为2.0 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 2.0 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of crude emulsion: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a crude emulsion, wherein the oil phase The mass ratio of the water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

实施例8Example 8

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为10 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 10 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为3.0 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 3.0 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为120 MPa,均质的循环次数为5次。4) Preparation of nanoemulsion: perform high pressure homogenization on the crude emulsion obtained in step 3), and then cool to room temperature after homogenization to obtain a nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa, and the number of cycles of homogenization is set to 120 MPa. for 5 times.

根据实施例4-8,步骤2)中的神经酸浓度为 0.1-3.0 mg/mL,每个实施例均使用乳清分离蛋白作为乳化剂进行试验。图2为添加不同浓度神经酸对神经酸纳米乳液粒径的影响,不同字母表示添加不同浓度神经酸制得的神经酸纳米乳液粒径有显著性差异 (p <0.05),在不同浓度神经酸条件下,均得到分散性较好的神经酸纳米乳液。当神经酸浓度为0.5 mg/mL时,制得的神经酸纳米乳液粒径最小,因此选取神经酸浓度为0.5 mg/mL。According to Examples 4-8, the nervonic acid concentration in step 2) was 0.1-3.0 mg/mL, and each example was tested using whey protein isolate as the emulsifier. Figure 2 shows the effect of adding different concentrations of nervonic acid on the particle size of nervonic acid nanoemulsion. Different letters indicate that the particle size of nervonic acid nanoemulsion prepared by adding different concentrations of nervonic acid is significantly different (p < 0.05). Under the same conditions, nervonic acid nanoemulsions with good dispersibility were obtained. When the nervonic acid concentration was 0.5 mg/mL, the obtained nervonic acid nanoemulsion had the smallest particle size, so the nervonic acid concentration was selected as 0.5 mg/mL.

实施例9Example 9

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为12 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 12 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为90 MPa。4) Preparation of nanoemulsion: the crude emulsion obtained in step 3) is subjected to high pressure homogenization, and after homogenization is cooled to room temperature, the nervonic acid nanoemulsion can be obtained, wherein the homogenization pressure is set to 90 MPa.

实施例10Example 10

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为12 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 12 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 100 MPa。4) Preparation of nanoemulsion: the crude emulsion obtained in step 3) is subjected to high pressure homogenization, and then cooled to room temperature after homogenization to obtain nervonic acid nanoemulsion, wherein the homogenization pressure is set to 100 MPa.

实施例11Example 11

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为12 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 12 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 110 MPa。4) Preparation of nanoemulsion: the crude emulsion obtained in step 3) is subjected to high pressure homogenization, and then cooled to room temperature after homogenization to obtain the nervonic acid nanoemulsion, wherein the homogenization pressure is set to 110 MPa.

实施例12Example 12

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为12 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 12 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 120 MPa。4) Preparation of nanoemulsion: the crude emulsion obtained in step 3) is subjected to high pressure homogenization, and then cooled to room temperature after homogenization to obtain nervonic acid nanoemulsion, wherein the homogenization pressure is set to 120 MPa.

实施例13Example 13

一种神经酸纳米乳液的制备方法,包括以下步骤:A preparation method of nervonic acid nanoemulsion, comprising the following steps:

1)制备水相:称量乳化剂,将乳化剂加入去离子水中进行搅拌,充分水合后形成水相,其中,乳化剂的浓度为1.5 w/v%,搅拌时间为12 h;1) Prepare the water phase: weigh the emulsifier, add the emulsifier to deionized water for stirring, and form a water phase after full hydration, wherein the concentration of the emulsifier is 1.5 w/v%, and the stirring time is 12 h;

2)制备油相:分别称量神经酸和中链甘油三酸酯,将神经酸通过超声波溶解的方式溶解于中链甘油三酸酯中形成油相,其中神经酸在中链甘油三酸酯中的浓度为0.5 mg/mL;2) Preparation of oil phase: Nervous acid and medium-chain triglyceride were weighed respectively, and nervonic acid was dissolved in medium-chain triglyceride by ultrasonic dissolving to form an oil phase, wherein nervonic acid was in medium-chain triglyceride. The concentration in 0.5 mg/mL;

3)制备粗乳:将步骤2)得到的油相边搅拌边逐滴加入步骤1)得到的水相中,滴加完成后继续搅拌10 min,然后高速剪切,形成粗乳液,其中,油相和水相的质量比为1:9;3) Preparation of coarse milk: add the oil phase obtained in step 2) dropwise to the water phase obtained in step 1) while stirring, continue to stir for 10 min after the dropwise addition is completed, and then shear at high speed to form a coarse emulsion, in which the oil The mass ratio of phase and water phase is 1:9;

4)制备纳米乳液:将步骤3)得到的粗乳液进行高压均质,均质后冷却至室温,即可得神经酸纳米乳液,其中,均质压力设定为 130 MPa。4) Preparation of nanoemulsion: the crude emulsion obtained in step 3) is subjected to high pressure homogenization, and then cooled to room temperature after homogenization to obtain the nervonic acid nanoemulsion, wherein the homogenization pressure is set to 130 MPa.

实施例9-13中,每个实施例均使用乳清分离蛋白作为乳化剂进行试验。步骤4)中均质的循环次数分别设置为3、4、5次,根据不同的均质压力重复以上实施例实验。图3为不同均质压力及循环次数对神经酸纳米乳液粒径的影响,不同字母表示在不同均质条件下神经酸纳米乳液粒径有显著性差异 (p < 0.05),在不同均质条件下,均得到分散性较好的神经酸纳米乳液。从图3可以看出,从100 MPa起,神经酸纳米乳液的粒径随均质压力增大及循环次数的增多而减小。当循环次数为5次时,均质压力在120 MPa和130 MPa下神经酸纳米乳液粒径均较小,且无显著性差异,因此选取120 MPa均质压力下循环5次进行神经酸纳米乳液的制备。In Examples 9-13, each example was tested using whey protein isolate as the emulsifier. In step 4), the number of cycles of homogenization is set to 3, 4, and 5 times, respectively, and the experiments of the above embodiments are repeated according to different homogenization pressures. Figure 3 shows the effect of different homogenization pressure and cycle times on the particle size of nervonic acid nanoemulsion. Different letters indicate significant differences in particle size of nervonic acid nanoemulsion under different homogenization conditions ( p < 0.05). Under both conditions, nervonic acid nanoemulsions with better dispersibility were obtained. It can be seen from Figure 3 that from 100 MPa, the particle size of the nervonic acid nanoemulsion decreases with the increase of the homogenization pressure and the increase of the number of cycles. When the number of cycles was 5, the particle size of the nervonic acid nanoemulsion was smaller at 120 MPa and 130 MPa, and there was no significant difference. preparation.

Claims (10)

1. A preparation method of nervonic acid nanoemulsion is characterized by comprising the following steps:
1) preparing an aqueous phase: weighing an emulsifier, adding the emulsifier into deionized water, stirring, and forming a water phase after sufficient hydration;
2) preparing an oil phase: respectively weighing nervonic acid and carrier oil, and fully dissolving the nervonic acid in the carrier oil to form an oil phase;
3) preparing coarse milk: dropwise adding the oil phase obtained in the step 2) into the water phase obtained in the step 1) while stirring, continuously stirring after the dropwise adding is finished, and then shearing at a high speed to form a coarse emulsion;
4) preparing a nano emulsion: homogenizing the crude emulsion obtained in the step 3) under high pressure, and cooling to room temperature after homogenizing to obtain the nervonic acid nano emulsion.
2. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: the emulsifier in the step 1) comprises a water-soluble emulsifier, wherein the water-soluble emulsifier is any one or a mixture of several of animal protein, plant protein and non-ionic emulsifier.
3. The method for preparing a nervonic acid nanoemulsion according to claim 2, wherein: the animal protein is whey protein isolate, the plant protein is soybean protein isolate, and the nonionic emulsifier is tween 20.
4. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: the concentration of the emulsifier in the step 1) is 0.5-2.0 w/v%, and the stirring time is 10-12 h.
5. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: the oil loading in the step 2) is medium-chain triglyceride.
6. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: the concentration of the nervonic acid in the oil phase in the step 2) is 0.1-3.0 mg/mL.
7. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: the mode of dissolving the nervonic acid in the carrier oil in the step 2) is ultrasonic dissolution.
8. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: the mass ratio of the oil phase to the water phase in the step 3) is 1: 9, after the dripping is finished, the stirring time is continued for 10min, and the rotating speed of the high-speed shearing machine is 30000 rpm.
9. The method for preparing a nervonic acid nanoemulsion according to claim 1, wherein: in the step 4), the homogenizing pressure is set to be 90-130 MPa, and the homogenizing cycle time is 3-5 times.
10. The use of the nervonic acid nanoemulsion obtained by the preparation method according to claims 1-9 in the field of functional foods.
CN202010317471.0A 2020-04-21 2020-04-21 A kind of preparation method of nervonic acid nanoemulsion Pending CN111616366A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112602875A (en) * 2020-12-24 2021-04-06 吉林大学 Method for preparing food-grade nano emulsion coated with photosensitizer
CN115120559A (en) * 2022-07-22 2022-09-30 江南大学 Method for improving embedding rate of ginsenoside Rg3 and CK and stability of nano emulsion
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CN116326703A (en) * 2023-01-10 2023-06-27 沈阳信康药物研究有限公司 A kind of phospholipid emulsion drink containing seabuckthorn seed oil and preparation method thereof

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