CN116584652A - A kind of nanoscale DHA algae oil freeze-dried instant tablet and preparation method thereof - Google Patents
A kind of nanoscale DHA algae oil freeze-dried instant tablet and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种纳米级DHA藻油冻干速溶片及其制备方法。其中,一种纳米级DHA藻油冻干速溶片,以重量份数计,其原料包括:DHA藻油10‑40份、蛋白5‑15份、冻干保护剂40‑70份、稳定剂0.1‑5份、乳化剂0.1‑5份、矫味剂0‑0.2份、纯化水285‑667份。本发明公开的一种纳米级DHA藻油冻干速溶片及其制备方法,具有良好风味、口感好、食用方便、易吸收且有较高载油量,复水后能较好保持原乳液粒径,改善吸收率及生物利用度。
The invention discloses a nano-scale DHA algae oil freeze-dried instant tablet and a preparation method thereof. Wherein, a kind of nanoscale DHA algae oil freeze-dried instant tablet, its raw material comprises: DHA algae oil 10-40 parts, protein 5-15 parts, lyoprotectant 40-70 parts, stabilizer 0.1 parts by weight. ‑5 parts, emulsifier 0.1‑5 parts, flavoring agent 0‑0.2 parts, purified water 285‑667 parts. The invention discloses a nano-scale DHA algae oil freeze-dried instant tablet and a preparation method thereof, which has good flavor, good taste, convenient eating, easy absorption and high oil loading capacity, and can better maintain the original emulsion particles after rehydration diameter, improving absorption and bioavailability.
Description
技术领域technical field
本发明涉及食品加工技术领域,尤其涉及一种纳米级DHA藻油冻干速溶片及其制备方法。The invention relates to the technical field of food processing, in particular to a nano-scale DHA algae oil freeze-dried instant tablet and a preparation method thereof.
背景技术Background technique
DHA,学名二十二碳六烯酸,俗称脑黄金。是一种对人体非常有益的Omega-3不饱和脂肪酸。DHA是神经系统细胞生长及维持的一种主要元素,是大脑和视网膜的重要构成脂肪酸,在人体大脑皮层中含量高达20%,对智力和视力发育至关重要。DHA, scientific name docosahexaenoic acid, commonly known as brain gold. It is an Omega-3 unsaturated fatty acid that is very beneficial to the human body. DHA is a main element for the growth and maintenance of cells in the nervous system. It is an important constituent fatty acid of the brain and retina. The content of DHA in the human cerebral cortex is as high as 20%, and it is very important for the development of intelligence and vision.
DHA日推荐摄入量不高于300mg,而现有DHA产品主要以凝胶糖果、软胶囊、固体饮料、压片糖果等形式存在,由于DHA主要来源于藻油,会有一定的腥味,藻油直接入口会带来油腻感,影响人体的可接受度。现有产品中的藻油大多都是直接加在糖果或软胶囊中,存在吸收不充分、口味差、油腻难接受等缺陷。The recommended daily intake of DHA is not higher than 300mg, and the existing DHA products mainly exist in the form of gel candy, soft capsule, solid drink, tablet candy, etc. Since DHA is mainly derived from algae oil, it will have a certain fishy smell. Direct intake of algae oil will bring a greasy feeling and affect the acceptability of the human body. Most of the algae oils in existing products are directly added to candies or soft capsules, which have defects such as insufficient absorption, poor taste, and unacceptable greasy.
纳米食品是指在生产、加工或包装过程中采用了纳米技术的食品,从狭义角度来说,只有对食品成分本身利用纳米技术改造和加工的产品,才称得上是纳米食品。纳米乳液一般是热力学稳定、各向同性,透明或半透明的均相分散体系,可以用于承载脂质,从而改善在消化道中的吸收率,提高生物利用度。DHA纳米乳长时间常温放置会发生破乳及降解等,将纳米乳制成干乳剂能显著提高其常温放置稳定性,为更方便储存和食用,将纳米乳液冻干,但冻干后在口中复水可能会造成液滴聚集,粒径发生变化,不利于吸收,有待改善。Nano-food refers to food that adopts nanotechnology in the process of production, processing or packaging. From a narrow perspective, only products that use nanotechnology to transform and process food ingredients themselves can be called nano-food. Nanoemulsions are generally thermodynamically stable, isotropic, transparent or translucent homogeneous dispersion systems that can be used to carry lipids, thereby improving the absorption rate in the digestive tract and increasing bioavailability. DHA nanoemulsions will break and decompose when placed at room temperature for a long time. Making nanoemulsions into dry emulsions can significantly improve their stability at room temperature. Rehydration may cause droplets to aggregate and particle size to change, which is not conducive to absorption and needs to be improved.
发明内容Contents of the invention
针对现有技术存在的纳米级DHA藻油复水可能会造成液滴聚集,且人体的可接受度差的问题,本发明的目的在于提供一种纳米级DHA藻油冻干速溶片及其制备方法,具有良好风味、口感好、食用方便、易吸收且有较高载油量,复水后能较好保持原乳液粒径,改善吸收率及生物利用度。Aiming at the problem that the rehydration of nano-scale DHA algae oil in the prior art may cause droplets to aggregate, and the acceptability of the human body is poor, the purpose of the present invention is to provide a nano-scale DHA algae oil freeze-dried instant tablet and its preparation The method has the advantages of good flavor, good taste, convenient consumption, easy absorption and high oil loading capacity. After rehydration, the particle size of the original emulsion can be better maintained, and the absorption rate and bioavailability are improved.
为实现上述目的,本发明提供了如下技术方案:一种纳米级DHA藻油冻干速溶片,以重量份数计,其原料包括:DHA藻油10-40份、蛋白5-15份、冻干保护剂40-70份、稳定剂0.1-5份、乳化剂0.1-5份、矫味剂0.05-0.2份、纯化水285-667份。In order to achieve the above object, the present invention provides the following technical scheme: a nano-scale DHA algae oil freeze-dried instant tablet, in parts by weight, its raw materials include: 10-40 parts of DHA algae oil, 5-15 parts of protein, frozen Dry protection agent 40-70 parts, stabilizer 0.1-5 parts, emulsifier 0.1-5 parts, flavoring agent 0.05-0.2 parts, purified water 285-667 parts.
进一步地,还包括填充剂1-10重量份。Further, 1-10 parts by weight of a filler is also included.
进一步地,还包括香精0.1-0.5重量份。Further, 0.1-0.5 parts by weight of essence is also included.
进一步地,所述蛋白选自牛奶蛋白、分离乳清蛋白、浓缩乳清蛋白、大豆蛋白和玉米醇溶蛋白中的至少一种;Further, the protein is selected from at least one of milk protein, whey protein isolate, whey protein concentrate, soybean protein and zein;
所述冻干保护剂选自糖类和/或糖醇类;The lyoprotectant is selected from sugars and/or sugar alcohols;
所述乳化剂选自牛奶磷脂、大豆磷脂、卵磷脂、微晶纤维素、单硬脂酸甘油酯、中链甘油三酯、蔗糖脂肪酸酯、司盘60和酪蛋白酸钠中的至少一种;The emulsifier is selected from at least one of milk lecithin, soybean lecithin, lecithin, microcrystalline cellulose, glycerol monostearate, medium chain triglyceride, sucrose fatty acid ester, Span 60 and sodium caseinate kind;
所述矫味剂选自柠檬酸、苹果酸、三氯蔗糖、甜菊糖苷、阿斯巴甜和甜蜜素中的至少一种;The flavoring agent is selected from at least one of citric acid, malic acid, sucralose, steviol glycosides, aspartame and cyclamate;
所述填充剂选自麦芽糊精、菊粉、马铃薯淀粉、甘薯淀粉、抗性淀粉和抗性糊精中的至少一种。The filler is at least one selected from maltodextrin, inulin, potato starch, sweet potato starch, resistant starch and resistant dextrin.
进一步地,所述糖类选自L-阿拉伯糖、低聚果糖、聚葡萄糖、低聚半乳糖、水苏糖、低聚木糖、乳糖、海藻糖和葡萄糖中的至少一种;Further, the carbohydrate is selected from at least one of L-arabinose, fructooligosaccharide, polydextrose, galactooligosaccharide, stachyose, xylooligosaccharide, lactose, trehalose and glucose;
所述糖醇类选自D-甘露糖醇、异麦芽酮糖醇和木糖醇中的至少一种;The sugar alcohols are selected from at least one of D-mannitol, isomalt and xylitol;
所述糖醇类与糖类的重量比为(1-3):1。The weight ratio of the sugar alcohols to sugars is (1-3):1.
进一步地,所述香精选自甜橙香精和/或百香果香精。Further, the fragrance is selected from sweet orange essence and/or passion fruit essence.
一种纳米级DHA藻油冻干速溶片的制备方法,包括如下步骤:A preparation method of nanoscale DHA algae oil freeze-dried instant tablets, comprising the steps of:
S1:将纯化水分成两份,第一份纯化水和第二分纯化水的质量比为(1-2):1,将DHA藻油、蛋白、乳化剂与第一份纯化水通过高速分散均质机混合均匀;S1: Divide the purified water into two parts, the mass ratio of the first part of purified water to the second part of purified water is (1-2): 1, and the DHA algae oil, protein, emulsifier and the first part of purified water are dispersed at high speed The homogenizer mixes evenly;
S2:将冻干保护剂、稳定剂、矫味剂、填充剂和第二份纯化水混合均匀,并在60-85℃下水浴加热水合10-120min;S2: Mix the lyoprotectant, stabilizer, flavoring agent, filler and the second part of purified water evenly, and heat and hydrate in a water bath at 60-85°C for 10-120min;
S3:将步骤S1制得的混合液和步骤S2制得的混合液与香精通过高速分散均质机混合均匀,得到乳液;然后将乳液转移至高压均质机中均质处理2-3次,得到纳米级乳液;S3: Mix the mixed solution prepared in step S1, the mixed solution prepared in step S2, and the essence through a high-speed dispersing homogenizer to obtain an emulsion; then transfer the emulsion to a high-pressure homogenizer for homogenization treatment 2-3 times, Obtain nano-emulsion;
S4:将步骤S3制得的纳米级乳液转移至模具内,随后送入干燥仓中,在在-40℃预冻3h,真空度为0Pa;保持真空度为0Pa开启加热系统,升华干燥,以每分钟1℃的升温速率进行升温,当温度达到-32℃时,保温2h;当温度达到-25℃时,保温4h;当温度达到-20℃时,保温6h;当温度达到-10℃时,保温4h;当温度达到-0℃时,保温2.5h;当温度达到10℃时,保温1.5h;然后开启真空系统,当温度达到30℃、真空度为20Pa时,保温1.5h,即得冻干速溶片。S4: Transfer the nano-emulsion prepared in step S3 into the mold, then send it into the drying chamber, pre-freeze at -40°C for 3 hours, and the vacuum degree is 0Pa; keep the vacuum degree at 0Pa and turn on the heating system, sublimation and drying, to Heat up at a rate of 1°C per minute. When the temperature reaches -32°C, keep warm for 2 hours; when the temperature reaches -25°C, keep warm for 4 hours; when the temperature reaches -20°C, keep warm for 6 hours; when the temperature reaches -10°C , keep warm for 4h; when the temperature reaches -0°C, keep warm for 2.5h; when the temperature reaches 10°C, keep warm for 1.5h; then turn on the vacuum system, when the temperature reaches 30°C and the vacuum degree is 20Pa, keep warm for 1.5h, that is, Freeze-dried instant tablets.
优选地,第一份纯化水和第二分纯化水的质量比为1.5:1。Preferably, the mass ratio of the first purified water to the second purified water is 1.5:1.
进一步地,在步骤S1中,通过高速分散均质机均质的条件为:转速为8000-15000r/min,均质2-5min。Further, in step S1, the conditions for homogenizing by a high-speed dispersing homogenizer are: the rotation speed is 8000-15000 r/min, and the homogenization takes 2-5 minutes.
进一步地,在步骤S3中,通过高速分散均质机均质的条件为:转速为8000-15000r/min,时间1-2min;Further, in step S3, the conditions for homogenization by a high-speed dispersing homogenizer are: the rotating speed is 8000-15000r/min, and the time is 1-2min;
通过高压均质机均质的条件为:均质压力为500-1200bar。The conditions for homogenization by a high-pressure homogenizer are: the homogenization pressure is 500-1200 bar.
进一步地,在步骤S3中,将步骤S1制得的混合液、步骤S2制得的混合液以及香精通过高速分散均质机混合,得到乳液。Further, in step S3, the mixed liquid prepared in step S1, the mixed liquid prepared in step S2 and the essence are mixed by a high-speed dispersing homogenizer to obtain an emulsion.
综上所述,本发明具有以下有益效果:In summary, the present invention has the following beneficial effects:
1、本申请通过添加蛋白,由于蛋白能在油水界面形成屏障,冻干后包裹DHA藻油,从而改善DHA藻油带来的腥味;通过添加冻干保护剂,使样品在冻干过程中产生大量的微小冰晶体,使得冻干速溶片复水后能较好保持原乳液粒径,改善吸收率及生物利用度;通过合理搭配冻干保护剂所占比例及各组分配比,更易干燥形成疏松多孔结构,速溶口感更佳。1. In this application, by adding protein, since the protein can form a barrier at the oil-water interface, DHA algae oil will be wrapped after freeze-drying, thereby improving the fishy smell brought by DHA algae oil; by adding a freeze-drying protective agent, the sample can be preserved during the freeze-drying process. A large number of tiny ice crystals are produced, so that the freeze-dried instant tablets can better maintain the particle size of the original emulsion after rehydration, and improve the absorption rate and bioavailability; by reasonably matching the proportion of freeze-drying protective agents and the distribution ratio of each component, it is easier to dry A loose and porous structure is formed, and the instant taste is better.
2、本申请的制备方法,通过经过均质处理生产的冻干片,能形成更规则的骨架结构,藻油微粒可达纳米级别且分布均匀,速溶性好,口感好,食用方便,因为是纳米级所以更好吸收;将水溶性成分和脂溶性成分分别溶解后混合,使物料在各自分散体系内充分混合均匀,均质后产品采用真空冷冻干燥技术,最大限度的降低了加工过程中DHA藻油的氧化,从而保留更高的活性,方便保存、携带。2. The preparation method of the present application can form a more regular skeleton structure through the freeze-dried flakes produced by homogeneous treatment, and the algae oil particles can reach the nanometer level and are evenly distributed, with good instant solubility, good taste, and convenient consumption, because it is Nano-scale, so it is better absorbed; the water-soluble components and fat-soluble components are dissolved and mixed separately, so that the materials are fully mixed and evenly mixed in their respective dispersion systems. After homogenization, the product adopts vacuum freeze-drying technology to minimize the DHA in the processing process Algae oil is oxidized to retain higher activity, which is convenient for storage and portability.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作一简单地介绍,显而易见地,下面描述中的附图是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description These are some embodiments of the present invention. For those skilled in the art, other drawings can also be obtained according to these drawings without any creative effort.
图1为本申请实施例1冻干速溶片复水后的粒径分布图;Fig. 1 is the particle size distribution figure after rehydration of the freeze-dried instant tablet of Example 1 of the present application;
图2为本申请对比例3冻干液的粒径分布图;Fig. 2 is the particle size distribution figure of comparative example 3 freeze-dried liquid of the present application;
图3为本申请对比例5冻干速溶片复水后的粒径分布图。Fig. 3 is the particle size distribution diagram of the lyophilized instant tablet of Comparative Example 5 of the present application after rehydration.
具体实施方式Detailed ways
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图1-3,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings 1-3 in the embodiments of the present invention. Obviously, the described The embodiments are some of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.
本申请中所使用的原料均可通过市售获得。All raw materials used in this application can be obtained commercially.
实施例Example
实施例1Example 1
纳米级DHA藻油冻干速溶片的制备方法,包括如下步骤:The preparation method of nanoscale DHA algae oil freeze-dried instant tablet comprises the following steps:
S1:将纯化水分成两份,将DHA藻油20份、蛋白10份、乳化剂6.3份与第一份纯化水300份通过高速分散均质机在转速为10000r/min,混合3min,备用;S1: Divide the purified water into two parts, mix 20 parts of DHA algae oil, 10 parts of protein, 6.3 parts of emulsifier and 300 parts of the first purified water through a high-speed dispersing homogenizer at a speed of 10000r/min, mix for 3 minutes, and set aside;
其中,蛋白为分离乳清蛋白;Wherein, the protein is whey protein isolate;
乳化剂由牛奶磷脂5份、中链甘油三酯0.8份和大豆磷脂0.5份组成;The emulsifier is composed of 5 parts of milk lecithin, 0.8 part of medium chain triglyceride and 0.5 part of soybean lecithin;
S2:向第二份纯化水200份中加入冻干保护剂58.4份、稳定剂0.2份、矫味剂0.1份和填充剂5份,于70℃水浴加热水合60min,直至溶解完全,备用;S2: Add 58.4 parts of lyoprotectant, 0.2 parts of stabilizer, 0.1 part of flavoring agent and 5 parts of filler to the second part of 200 parts of purified water, heat and hydrate in a water bath at 70°C for 60 minutes until completely dissolved, and set aside;
其中,冻干保护剂由D-甘露糖醇38.4份和乳糖20份组成;Among them, the lyoprotectant consists of 38.4 parts of D-mannitol and 20 parts of lactose;
稳定剂为黄原胶;The stabilizer is xanthan gum;
矫味剂为三氯蔗糖;The flavoring agent is sucralose;
填充剂为菊粉;The filler is inulin;
S3:将步骤S1制得的油分散液和步骤S2制得的水分散液通过高速分散均质机混合均匀,转速为10000r/min,时间2min,得到水包油型的乳液;S3: Mix the oil dispersion prepared in step S1 and the water dispersion prepared in step S2 uniformly through a high-speed dispersing homogenizer at a speed of 10000 r/min for 2 minutes to obtain an oil-in-water emulsion;
然后将乳液转移至高压均质机中,均质压力为1000bar,均质3次,得到纳米级乳液;Then the emulsion is transferred to a high-pressure homogenizer, and the homogenization pressure is 1000 bar, and the homogenization is performed 3 times to obtain a nanoscale emulsion;
S4:将步骤S3制得的纳米级乳液转移至模具内,随后送入干燥仓内进行预冻,预冻温度为-40℃,预冻时间为3h,控温时间50min,预冻真空度为0Pa;S4: Transfer the nano-emulsion prepared in step S3 into the mold, and then send it into the drying bin for pre-freezing. The pre-freezing temperature is -40°C, the pre-freezing time is 3h, the temperature control time is 50min, and the pre-freezing vacuum degree is 0 Pa;
预冻结束后,在-40℃下,保温3h后,保持真空度为0Pa,开启加热系统,以每分钟1℃的升温速率,升温至-32℃,随后保温2h;再以每分钟1℃的升温速率,升温至-25℃,随后保温4h,再以每分钟1℃的升温速率,升温至-20℃,随后保温6h,再以每分钟1℃的升温速率,升温至-10℃,随后保温4h,再以每分钟1℃的升温速率,升温至0℃,随后保温2.5h;再以每分钟1℃的升温速率,升温至10℃,随后保温1.5h;After pre-freezing, keep the vacuum at 0 Pa at -40°C for 3 hours, turn on the heating system, raise the temperature to -32°C at a rate of 1°C per minute, and then keep warm for 2 hours; The heating rate is raised to -25°C, and then kept for 4 hours, then raised to -20°C at a heating rate of 1°C per minute, then kept at a temperature of 6 hours, and then raised to -10°C at a heating rate of 1°C per minute, Then keep it warm for 4 hours, then raise the temperature to 0°C at a rate of 1°C per minute, and then keep it for 2.5 hours; then raise the temperature to 10°C at a rate of 1°C per minute, and then keep it for 1.5 hours;
然后开启真空系统,将真空度升高至20Pa再以每分钟1℃的升温速率,升温至30℃,随后保温1.5h结束干燥,制得冻干速溶片。Then turn on the vacuum system, raise the vacuum degree to 20 Pa, then raise the temperature to 30° C. at a rate of 1° C. per minute, and then keep it warm for 1.5 hours to complete the drying to obtain freeze-dried instant tablets.
实施例2Example 2
和实施例1的区别仅在于,DHA藻油的重量份为15份。The only difference with Example 1 is that the weight portion of DHA algae oil is 15 parts.
实施例3Example 3
和实施例1的区别仅在于,DHA藻油的重量份为25份。The only difference with Example 1 is that the weight portion of DHA algae oil is 25 parts.
实施例4Example 4
和实施例1的区别仅在于,DHA藻油的重量份为30份。The only difference with Example 1 is that the weight portion of DHA algae oil is 30 parts.
实施例5Example 5
和实施例1的区别仅在于,第一份纯化水的重量份为240份,第二份纯化水的重量份为160份。The only difference from Example 1 is that the first part of purified water has 240 parts by weight, and the second part of purified water has 160 parts by weight.
实施例6Example 6
和实施例1的区别仅在于,第一份纯化水的重量份为200份,第二份纯化水的重量份为135份。The only difference from Example 1 is that the first part of purified water has 200 parts by weight, and the second part of purified water has 135 parts by weight.
实施例7Example 7
和实施例1的区别仅在于,第一份纯化水的重量份为185份,第二份纯化水的重量份为100份。The only difference from Example 1 is that the first part of purified water has 185 parts by weight, and the second part of purified water has 100 parts by weight.
实施例8Example 8
和实施例1的区别仅在于,S3步骤中均质压力为800bar。The only difference from Example 1 is that the homogeneous pressure in step S3 is 800 bar.
实施例9Example 9
和实施例1的区别仅在于,S3步骤中均质压力为1200bar。The only difference from Example 1 is that the homogeneous pressure in step S3 is 1200 bar.
实施例10Example 10
和实施例1的区别仅在于,冻干保护剂D-甘露糖醇的重量份为43.4份,乳糖的重量份为15份。The only difference from Example 1 is that the weight part of the lyoprotectant D-mannitol is 43.4 parts, and the weight part of lactose is 15 parts.
实施例11Example 11
和实施例1的区别仅在于,冻干保护剂D-甘露糖醇的重量份为30份,乳糖的重量份为28.4份。The only difference from Example 1 is that the weight part of the lyoprotectant D-mannitol is 30 parts, and the weight part of lactose is 28.4 parts.
实施例12Example 12
和实施例1的区别仅在于,将步骤S1制得的油分散液和步骤S2制得的水分散液以及甜橙香精0.1份通过高速分散均质机混合均匀,转速为10000r/min,时间2min,得到水包油型乳液。The difference from Example 1 is that the oil dispersion prepared in step S1, the water dispersion prepared in step S2, and 0.1 part of sweet orange essence are mixed uniformly by a high-speed dispersing homogenizer at a speed of 10,000 r/min for 2 minutes , to obtain an oil-in-water emulsion.
实施例13Example 13
和实施例1的区别仅在于,蛋白为牛奶蛋白10份。The only difference with Example 1 is that the protein is 10 parts of milk protein.
实施例14Example 14
和实施例1的区别仅在于,乳化剂为6.3份,由大豆磷脂5份、蔗糖脂肪酸酯0.8份和微晶纤维素0.5份组成。The only difference from Example 1 is that the emulsifier is 6.3 parts, consisting of 5 parts of soybean lecithin, 0.8 part of sucrose fatty acid ester and 0.5 part of microcrystalline cellulose.
实施例15Example 15
和实施例1的区别仅在于,冻干保护剂为木糖醇38.4份,葡萄糖20份。The only difference from Example 1 is that the lyoprotectant is 38.4 parts of xylitol and 20 parts of glucose.
对比例comparative example
对比例1Comparative example 1
和实施例1的区别仅在于,DHA藻油的重量份为35份。The only difference with Example 1 is that the weight portion of DHA algae oil is 35 parts.
对比例2Comparative example 2
第一份纯化水的重量份为400份,第二份纯化水的重量份为267份。The weight part of the first purified water is 400 parts, and the weight part of the second purified water is 267 parts.
对比例3Comparative example 3
和实施例1的区别仅在于,未进行步骤S4的操作。The only difference from Embodiment 1 is that the operation of step S4 is not performed.
对比例4Comparative example 4
和实施例1的区别仅在于,冻干保护剂D-甘露糖醇的重量份为26.6份,乳糖的重量份为13.4份。The only difference from Example 1 is that the weight part of the lyoprotectant D-mannitol is 26.6 parts, and the weight part of lactose is 13.4 parts.
对比例5Comparative example 5
纳米级DHA藻油冻干速溶片的制备方法,包括如下步骤:The preparation method of nanoscale DHA algae oil freeze-dried instant tablet comprises the following steps:
S1:向纯化水500份中加入冻干保护剂58.4份、稳定剂0.2份、矫味剂0.1份和填充剂5份,于70℃水浴加热水合60min,直至溶解完全;S1: Add 58.4 parts of lyoprotectant, 0.2 parts of stabilizer, 0.1 part of flavoring agent and 5 parts of filler to 500 parts of purified water, heat and hydrate in a water bath at 70°C for 60 minutes until completely dissolved;
其中,冻干保护剂由D-甘露糖醇38.4份和乳糖20份组成;Among them, the lyoprotectant consists of 38.4 parts of D-mannitol and 20 parts of lactose;
稳定剂为黄原胶;The stabilizer is xanthan gum;
矫味剂为三氯蔗糖;The flavoring agent is sucralose;
填充剂为菊粉;The filler is inulin;
S2:向步骤S1制得的混合液中加入DHA藻油20份、蛋白10份、乳化剂6.3份,通过高速分散均质机在转速为10000r/min,混合3min,备用;S2: Add 20 parts of DHA algae oil, 10 parts of protein, and 6.3 parts of emulsifier to the mixed solution prepared in step S1, and mix for 3 minutes through a high-speed dispersing homogenizer at a speed of 10000 r/min, and set aside;
其中,蛋白为分离乳清蛋白;Wherein, the protein is whey protein isolate;
乳化剂由牛奶磷脂5份、中链甘油三酯0.8份和大豆磷脂0.5份组成;The emulsifier is composed of 5 parts of milk lecithin, 0.8 part of medium chain triglyceride and 0.5 part of soybean lecithin;
S3:将步骤S2制得的混合液通过高速分散均质机混合均匀,转速为10000r/min,时间2min,得到乳液;S3: Mix the mixed solution prepared in step S2 uniformly with a high-speed dispersing homogenizer at a speed of 10000r/min for 2min to obtain an emulsion;
然后将乳液转移至高压均质机中,均质压力为1000bar,均质3次,得到纳米级乳液;Then the emulsion is transferred to a high-pressure homogenizer, and the homogenization pressure is 1000 bar, and the homogenization is performed 3 times to obtain a nanoscale emulsion;
S4:同实施例1。S4: Same as Example 1.
对比例6Comparative example 6
和实施例1的区别仅在于,未添加蛋白。The only difference from Example 1 is that no protein is added.
性能检测试验performance test
一、包埋率测定1. Determination of embedding rate
对实施例1-4和对比例1制备的冻干速溶片进行如下测试:The freeze-dried instant tablet prepared by embodiment 1-4 and comparative example 1 is tested as follows:
测试方法:取2g整片冻干速溶片样品于烧杯中,加入20mL正己烷,充分振荡后取出速溶片样品过滤,再用20mL正己烷冲洗烧杯滤液合并后,放入通过万分之一天平称重的烧杯中,通过80℃水浴将正己烷挥发,擦干烧杯水分,之后通过万分之一天平称重记录表面油含量,测试结果见表1。Test method: Take 2g of the whole freeze-dried instant tablet sample in a beaker, add 20mL of n-hexane, take out the instant tablet sample and filter it after fully shaking, then rinse the beaker with 20mL of n-hexane and combine the filtrate, put it into the 1/10,000th balance to weigh In a heavy beaker, volatilize the n-hexane in an 80°C water bath, wipe off the water in the beaker, and then weigh and record the surface oil content with a ten-thousandth balance. The test results are shown in Table 1.
包埋率=1-(冻干速溶片表面DHA含量/冻干速溶片中DHA总量)Embedding rate=1-(DHA content on the surface of the freeze-dried instant tablet/the total amount of DHA in the freeze-dried instant tablet)
表1实施例1-4及对比例1冻干速溶片的包埋率The embedding rate of table 1 embodiment 1-4 and comparative example 1 freeze-dried instant tablet
结合实施例1-4和对比例1并结合表1可以看出,采用本申请方法制备的冻干速溶片包埋率在90%左右,随着DHA藻油添加量的增大包埋率也会增大,但达到一定值,由于壁材达到饱和无法包裹多余的油脂,从而导致包埋率的降低。即冻干速溶片样品中DHA添加量为20-30%,在此添加量范围内,DHA藻油能较好包埋在冻干速溶片中。In conjunction with Examples 1-4 and Comparative Example 1 and in conjunction with Table 1, it can be seen that the embedment rate of the freeze-dried instant tablet prepared by the method of the present application is about 90%, and the embedment rate also increases with the increase of the amount of DHA algae oil added. It will increase, but when it reaches a certain value, the excess oil cannot be wrapped due to the saturation of the wall material, resulting in a decrease in the embedding rate. That is, the amount of DHA added in the sample of the freeze-dried instant tablet is 20-30%, and within the range of the added amount, the DHA algae oil can be better embedded in the freeze-dried instant tablet.
二、模拟口腔溶解实验2. Simulated oral dissolution experiment
对实施例1,5-11、15和对比例2、4制备的冻干速溶片分别进行如下测试:The freeze-dried instant tablet prepared by Example 1, 5-11, 15 and Comparative Example 2, 4 is respectively tested as follows:
测试方法:将一片完整的冻干速溶片放入置于37℃恒温振荡水浴锅的烧杯中振荡频率为50r/min,烧杯中盛有5mL提前预热的模拟口腔消化液(5mg/mL黏蛋白,150U/mL唾液淀粉酶,pH6.8),放入冻干速溶片后开始计时,当冻干片完全溶解后计时结束,检测结果见表3。冻干液浓度为速溶片全部成分重量(g)与水体积(mL)的比值。Test method: Put a complete freeze-dried instant tablet into a beaker placed in a constant temperature oscillating water bath at 37°C with an oscillation frequency of 50r/min. The beaker contains 5mL preheated simulated oral digestive juice (5mg/mL mucin , 150U/mL salivary amylase, pH6.8), put into the freeze-dried instant tablet and start timing, when the freeze-dried tablet is completely dissolved, the timing ends, and the test results are shown in Table 3. The concentration of the lyophilized liquid is the ratio of the weight (g) of all ingredients of the instant tablet to the volume of water (mL).
表2实施例1,5-7及对比例2冻干速溶片溶解时间Table 2 embodiment 1,5-7 and comparative example 2 freeze-dried instant tablet dissolving time
结合实施例1、5-7和对比例2并结合表2可以看出,在模拟口腔实验中,所有实施例冻干速溶片都可以快速溶解,且冻干液浓度越低溶解速度越快,实际在口腔中的速度可能更快,这是由于浓度更低的冻干液干燥后依然能保持原有骨架结构,与水接触后由于毛细管力更快的吸收水分,从而快速溶解,但浓度为15g/100mL的溶解时间与20g/100mL接近,可能速溶片在同一体积下水分扩散速率已经达到饱和,继续降低浓度不会明显加快溶解速度。即冻干液浓度设置在20-30g/100mL较为合适。利用快速溶解这一优势,通过冻干速溶片的形式补充DHA藻油更加方便快捷。In combination with Examples 1, 5-7 and Comparative Example 2 and in combination with Table 2, it can be seen that in the simulated oral cavity experiment, all the freeze-dried instant tablets of the examples can be dissolved quickly, and the lower the concentration of the lyophilized solution, the faster the dissolution rate. The actual speed in the oral cavity may be faster. This is because the lyophilized liquid with lower concentration can still maintain the original skeleton structure after drying. After contacting with water, the capillary force absorbs water faster and dissolves quickly. The dissolution time of 15g/100mL is close to that of 20g/100mL. It is possible that the water diffusion rate of the instant tablet has reached saturation under the same volume, and further reduction of the concentration will not significantly increase the dissolution rate. That is, it is more appropriate to set the concentration of the lyophilized liquid at 20-30g/100mL. Taking advantage of the advantage of rapid dissolution, it is more convenient and quicker to supplement DHA algae oil in the form of freeze-dried instant tablets.
结合实施例1、8和9并结合表2,可以看出压力改变对速溶性影响不大。Combining Examples 1, 8 and 9 and Table 2, it can be seen that pressure changes have little effect on instant solubility.
结合实施例1、10、11和15及对比例4并结合表2,可以看出当乳糖比例增加时,溶解时间短,但实际生产中乳糖含量过高会导致成品塌陷,冻干骨架不坚实,应适当提高提供骨架支撑作用的冻干保护剂的含量。而改变冻干保护剂种类后,由于添加木糖醇和葡萄糖的速溶片有轻微塌陷,产品表明形成致密的糖层,致使溶解速度明显减慢。当添加冻干保护剂比例不足时,溶解时间很长,由于蛋白的相对比例增大,导致成品绵软,缺少硬质骨架,影响速溶性。Combining Examples 1, 10, 11 and 15 and Comparative Example 4 with Table 2, it can be seen that when the proportion of lactose increases, the dissolution time is short, but the high content of lactose in actual production will cause the finished product to collapse, and the freeze-dried skeleton is not solid , the content of the lyoprotectant that provides the skeleton support should be appropriately increased. After changing the type of lyoprotectant, because the instant tablet added with xylitol and glucose has a slight collapse, the product shows that a dense sugar layer is formed, resulting in a significantly slower dissolution rate. When the proportion of lyoprotectant is insufficient, the dissolution time is very long, and the relative proportion of protein increases, resulting in soft finished product, lack of hard skeleton, and affecting instant solubility.
三、粒径测试3. Particle size test
对实施例1,8-11和对比例3-5制备的冻干速溶片进行如下测试:The freeze-dried instant tablet prepared by embodiment 1, 8-11 and comparative example 3-5 is tested as follows:
测试方法:取冻干速溶片1g于20mL纯化水中复水,充分混合均匀后,使用ZetasizerNanoZS90(Malvern,UK)测定样品的粒径和多分散系数,25℃平衡120s后,用连续15个读数测量样品。每个样品进行三次平行,取平均值,测试结果见表3,表4,图1,图2,图3。Test method: Take 1 g of freeze-dried instant tablet and rehydrate it in 20 mL of purified water. After mixing thoroughly, use Zetasizer Nano ZS90 (Malvern, UK) to measure the particle size and polydispersity coefficient of the sample. sample. Each sample was carried out in parallel three times, and the average value was taken. The test results are shown in Table 3, Table 4, Fig. 1, Fig. 2, Fig. 3.
表3实施例1、8和9冻干速溶片粒径与压力Table 3 Embodiment 1, 8 and 9 freeze-dried instant tablet particle size and pressure
结合实施例1、8和9并结合表3可以看出,冻干液处理的压力越大,冻干速溶片粒径越小,高压均质属于高能乳化过程,通过剪切碰撞使较粗的内相原始颗粒破碎成纳米液滴。再结合表2可以判断复水后粒径大小与溶解速度并不直接关联。In conjunction with Examples 1, 8 and 9 and in conjunction with Table 3, it can be seen that the greater the pressure of the freeze-dried solution, the smaller the particle size of the freeze-dried instant tablet, and the high-pressure homogenization belongs to the high-energy emulsification process. The primary particles in the internal phase are broken into nano-droplets. Combined with Table 2, it can be judged that the particle size after rehydration is not directly related to the dissolution rate.
表4实施例1、10、11和15及对比例3-5冻干速溶片粒径和多分散系数Table 4 embodiment 1,10,11 and 15 and comparative example 3-5 lyophilized instant tablet particle diameter and polydispersity coefficient
图1为实施例1冻干速溶片复水后的粒径分布图;Fig. 1 is the particle size distribution figure after the rehydration of the freeze-dried instant tablet of embodiment 1;
图2为对比例3冻干液的粒径分布图。Figure 2 is a particle size distribution diagram of the freeze-dried liquid of Comparative Example 3.
图3为对比例5冻干速溶片复水后的粒径分布图。Figure 3 is a particle size distribution diagram of the freeze-dried instant tablet of Comparative Example 5 after rehydration.
结合实施例1、10、11和15并结合表4可以看出,冻干速溶片复水后粒径在250nm左右,改变冻干保护剂的浓度对复水粒径影响不大,多分散系数(PDI)接近,而改变冻干保护剂的种类直接影响复水粒径,PDI增大,说明D-甘露糖醇和乳糖的组合优于木糖醇和葡萄糖的组合,由于前者在冻干过程中更好保持冻干液的骨架结构,防止塌陷,保证液滴不会聚集导致粒径增大。In combination with Examples 1, 10, 11 and 15 and in conjunction with Table 4, it can be seen that the particle size of the freeze-dried instant tablet is about 250nm after rehydration, and changing the concentration of the freeze-drying protective agent has little effect on the rehydration particle size, and the polydispersity coefficient (PDI) is close, and changing the type of lyoprotectant directly affects the rehydration particle size, and the PDI increases, indicating that the combination of D-mannitol and lactose is better than the combination of xylitol and glucose, because the former is more effective in the freeze-drying process. It is best to maintain the skeleton structure of the lyophilized liquid to prevent collapse and ensure that the droplets will not aggregate and cause particle size to increase.
结合实施例1和对比例3、4以及图1-2并结合表4可以看出,添加冻干保护剂后,冻干速溶片复水能较好保持原始冻干液的粒径大小,冻干后乳液粒径会稍稍增大,当添加冻干保护剂浓度过低时,复水后粒径明显增大。In conjunction with Example 1 and Comparative Examples 3 and 4 and Figures 1-2 and in conjunction with Table 4, it can be seen that after adding the lyoprotectant, the rehydration of the lyophilized instant tablet can better maintain the particle size of the original lyophilized liquid, The particle size of the emulsion will increase slightly after drying, and when the concentration of the added lyoprotectant is too low, the particle size will increase significantly after rehydration.
结合实施例1和对比例5以及图3并结合表4可以看出,冻干液处理过程中未均匀分散各体系,直接导致冻干复水粒径增大,乳液多分散系数为0.424,表明混合体系分子量分布宽,乳液不均匀。In combination with Example 1 and Comparative Example 5 and Fig. 3 and in combination with Table 4, it can be seen that each system is not uniformly dispersed during the treatment of the lyophilized liquid, which directly leads to an increase in the particle size of the lyophilized rehydration, and the polydispersity coefficient of the emulsion is 0.424, indicating that The molecular weight distribution of the mixed system is wide, and the emulsion is not uniform.
四、感官评价4. Sensory evaluation
对实施例1,12-15和对比例6制备的冻干速溶片进行如下测试:The freeze-dried instant tablet prepared by embodiment 1, 12-15 and comparative example 6 is tested as follows:
腥味测试方法:由经过一定培训的15人组成感官评价小组进行感官评价。测试的质量属性为腥味。所有的样品都放在贴有标签和加盖的玻璃容器中同时呈现给每个小组成员。按照腥味严重程度采用9分制评分法进行评分,分数为1-9之间的整数,其中1=非常不喜欢(腥味严重),9=非常喜欢(腥味较轻或无腥味感),感官打分结果见表5。Fishy smell test method: A sensory evaluation team composed of 15 people who have undergone certain training conducts sensory evaluation. The quality attribute tested was fishy odour. All samples were presented to each panelist simultaneously in labeled and covered glass containers. Use 9-point scoring method to score according to the severity of fishy smell, and the score is an integer between 1-9, wherein 1=dislikes very much (severe fishy smell), 9=likes very much (light fishy smell or no fishy smell) ), the sensory scoring results are shown in Table 5.
表5实施例1,12-15和对比例6冻干速溶片感官评价Table 5 Example 1, 12-15 and comparative example 6 freeze-dried instant tablet sensory evaluation
结合实施例1,12-15及对比例6并结合表5,可以看出不添加蛋白会明显导致腥味评分降低,而改变蛋白的种类也会影响对腥味的评分,可能是由于不同蛋白可能带有不同的风味,从而对腥味有不同的包裹掩盖效果。此外改变冻干保护剂、乳化剂的种类对腥味影响不大。添加香精后也能改善DHA藻油带来的腥味,提高入口可接受程度。Combining Example 1, 12-15 and Comparative Example 6 with Table 5, it can be seen that not adding protein will significantly reduce the score of fishy smell, and changing the type of protein will also affect the score of fishy smell, which may be due to different protein It may have different flavors, so it has different wrapping and masking effects on fishy smell. In addition, changing the types of lyoprotectant and emulsifier had little effect on fishy smell. Adding essence can also improve the fishy smell brought by DHA algae oil and improve the acceptable level of entrance.
结合实施例1,5-7及对比例2并结合表2和表5,可以看出,冻干液浓度越低感官评分越高,速溶性越好。Combining Examples 1, 5-7 and Comparative Example 2 with Table 2 and Table 5, it can be seen that the lower the concentration of the lyophilized solution, the higher the sensory score and the better the instant solubility.
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present invention, rather than limiting them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: It is still possible to modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the various embodiments of the present invention. scope.
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