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CN108703340A - A kind of eucommia ulmoides seed oil powder electuary and preparation method thereof - Google Patents

A kind of eucommia ulmoides seed oil powder electuary and preparation method thereof Download PDF

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CN108703340A
CN108703340A CN201810282404.2A CN201810282404A CN108703340A CN 108703340 A CN108703340 A CN 108703340A CN 201810282404 A CN201810282404 A CN 201810282404A CN 108703340 A CN108703340 A CN 108703340A
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eucommia
powder
seed oil
seed
oil
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李加兴
严友兵
朱式业
黄诚
杨建军
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XIANGXI LAODIE BIOLOGICAL CO Ltd
Jishou University
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XIANGXI LAODIE BIOLOGICAL CO Ltd
Jishou 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
    • A23L25/00Food consisting mainly of nutmeat or seeds; Preparation or treatment thereof
    • A23L25/30Mashed or comminuted products, e.g. pulp, pastes, meal, powders; Products made therefrom, e.g. blocks, flakes, snacks; Liquid or semi-liquid products
    • AHUMAN NECESSITIES
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    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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    • A23L33/115Fatty acids or derivatives thereof; Fats or oils
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    • 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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    • A23L33/40Complete food formulations for specific consumer groups or specific purposes, e.g. infant formula
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    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
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    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • A23P10/35Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
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    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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Abstract

The invention discloses a kind of eucommia ulmoides seed oil powder electuary and preparation method thereof, preparation method includes pretreatment of raw material, vacuum microwave humid heat treatment, supercritical extract carries oil, mechanical ball mill activates, super-high-pressure homogenization processing, is concentrated and dried, allotment drying.The method of the present invention first extracts eucommia ulmoides seed oil using Eucommia as raw material from Eucommia;Then it is raw material rationally to utilize the waste seed of bark of eucommia dregs of rice after carrying oil, using technologies such as mechanical ball mill activation, super-high-pressure homogenization processing, spray drying, it prepares rich in small molecular protein, starch and contains a small amount of gutta-percha, while there is the seed dregs of rice activity powder of preferably embedding effect and emulsifiability;Further, it is that wall material passes through micronization processing, vacuum spray drying using eucommia ulmoides seed oil as core material, seed dregs of rice activity powder, can prepare mobility, favorable dispersibility powdered oil, and has reducing blood lipid, blood pressure lowering, promote the development of nervous system, brain and retina, prevents senile dementia and allergy and other effects.

Description

一种杜仲籽油粉末冲剂及其制备方法A kind of eucommia seed oil powder granule and preparation method thereof

技术领域technical field

本发明属于粉末油脂加工技术领域,具体涉及一种杜仲籽油粉末冲剂及其制备方法。The invention belongs to the technical field of powder oil processing, and in particular relates to an eucommia seed oil powder granule and a preparation method thereof.

背景技术Background technique

杜仲(EucommiaulmoidesOliv.)又名木棉、思仙、思仲、思锦树,为单科单属落叶乔木,被誉为“活化石植物”,是我国特有的珍贵树种。我国杜仲森林资源丰富,总量占全世界95%,其野生分布中心在中国的中部地区,并广泛种植于湖南、湖北、河南、山西、四川、贵州、云南等省,种植面积已达400万亩。杜仲在我国有2000多年的药用历史。《神农本草经》和《本草纲目》均将杜仲列为上品,并记载“杜仲色紫,味甘而辛,其性湿平,甘温能补,微辛能润,故能入肝而补肾;主治腰膝痛,补中益精气,坚筋骨,强志,除阴下痒湿,小便余沥;久服,轻身耐劳”。现代研究表明,杜仲含木脂素类、环烯醚萜类、黄酮类、苯丙素类、甾醇类及三萜类、多糖类、抗真菌蛋白和矿物元素等多种活性物质,其中多数具有保健功效和药理活性,如降血压、降血脂、降血糖、抗肿瘤、抑菌抗病毒、抗炎、抗氧化等。杜仲的根、茎、叶、花、果实和种子中还含有天然高分子资源-杜仲胶。杜仲胶具有高抗撕、低生热、中高温度的高阻尼性等性能,可作为高端绿色轮胎、医疗器械、减震消音器件等的生产材料,是杜仲产业研究和开发的重点和热点,杜仲胶有望作为我国第二天然橡胶资源。Eucommia ulmoides Oliv., also known as Kapok, Sixian, Sizhong, and Sijinshu, is a deciduous tree of a single family and a single genus. It is known as a "living fossil plant" and is a unique and precious tree species in my country. my country's Eucommia ulmoides is rich in forest resources, accounting for 95% of the world's total. Its wild distribution center is in the central region of China, and it is widely planted in Hunan, Hubei, Henan, Shanxi, Sichuan, Guizhou, Yunnan and other provinces. The planting area has reached 4 million mu. Eucommia has a medicinal history of more than 2,000 years in my country. Both "Shen Nong's Materia Medica" and "Compendium of Materia Medica" listed Eucommia as the top grade, and recorded that "Eucommia ulmoides is purple in color, sweet and pungent in taste, and its nature is damp and flat. ; Cure mainly waist and knee pain, invigorate the vital energy, strengthen the muscles and bones, strengthen the will, remove itching and dampness under the yin, and urinate more than a little; take it for a long time, lighten the body and stand hard work." Modern research shows that Eucommia contains various active substances such as lignans, iridoids, flavonoids, phenylpropanoids, sterols and triterpenes, polysaccharides, antifungal proteins and mineral elements, most of which are It has health benefits and pharmacological activities, such as lowering blood pressure, lowering blood fat, lowering blood sugar, anti-tumor, antibacterial, anti-viral, anti-inflammatory, anti-oxidation, etc. The roots, stems, leaves, flowers, fruits and seeds of Eucommia also contain natural polymer resources - Eucommia gum. Eucommia gum has properties such as high tear resistance, low heat generation, and high damping at medium and high temperatures. It can be used as a production material for high-end green tires, medical equipment, shock-absorbing and sound-absorbing devices, etc. It is the focus and hotspot of Eucommia industry research and development. Eucommia Rubber is expected to be the second natural rubber resource in my country.

基于杜仲的药用保健作用和杜仲胶的发现,杜仲这一独特的“活化石”越来越受重视,人们对杜仲的研究也不断深入。其中,杜仲籽油因其富含а-亚麻酸是近些年来杜仲的又一开发热点。杜仲籽油主要存在于杜仲的翅果中,其富含亚麻酸、亚油酸等多不饱和脂肪酸,尤其是а-亚麻酸含量高达60%以上,是一种优质的亚麻酸植物资源。α-亚麻酸和亚油酸是人体必需脂肪酸,其中α-亚麻酸是体内各组织生物膜的结构材料,也是合成人体一系列前列腺素的前体。正常人从食物中摄取α-亚麻酸后,经△6-脱氢酶、碳链延长酶等的作用,生成一系列代谢产物,其中最重要的是EPA和DHA。EPA是体内三烯前列腺素(如PGI3,TXA3)前体,DHA是大脑、视网膜等神经系统磷脂的主要成份。正是基于α-亚麻酸、亚油酸的作用,使杜仲籽油具有降血脂,降血压,促进神经系统、脑和视网膜的发育,预防老年痴呆症和过敏症等功效。粉末油脂是一种用水溶性壁材将芯材包裹后获得的粉末颗粒,具有较好的流动性、乳化稳定性和分散性,可方便油脂的使用、运输和储存。因此,可以以杜仲翅果或杜仲籽油为原料,开发杜仲籽油粉末油脂或固体饮料产品,以充分发挥杜仲籽油的保健功效价值、拓宽杜仲籽油的用途和提高其附加值。Based on the medicinal health effects of Eucommia ulmoides and the discovery of eucommia ulmoides gum, more and more attention has been paid to this unique "living fossil" of eucommia ulmoides, and people's research on eucommia ulmoides is also deepening. Among them, Eucommia ulmoides seed oil is another development focus of Eucommia ulmoides in recent years because it is rich in а-linolenic acid. Eucommia ulmoides seed oil mainly exists in the samara of Eucommia ulmoides, which is rich in linolenic acid, linoleic acid and other polyunsaturated fatty acids, especially the α-linolenic acid content is as high as 60%, and it is a high-quality linolenic acid plant resource. α-linolenic acid and linoleic acid are essential fatty acids for the human body, among which α-linolenic acid is the structural material of the biofilm of various tissues in the body, and is also the precursor for the synthesis of a series of prostaglandins in the human body. After normal people ingest α-linolenic acid from food, a series of metabolites are produced through the action of △6-dehydrogenase and carbon chain elongation enzyme, the most important of which are EPA and DHA. EPA is the precursor of triene prostaglandins (such as PGI3, TXA3) in the body, and DHA is the main component of phospholipids in the nervous system such as the brain and retina. It is based on the effect of α-linolenic acid and linoleic acid that Eucommia ulmoides seed oil has the effects of lowering blood fat and blood pressure, promoting the development of the nervous system, brain and retina, and preventing Alzheimer's disease and allergies. Powdered oil is a kind of powder particles obtained by wrapping the core material with water-soluble wall material. It has good fluidity, emulsification stability and dispersibility, and can facilitate the use, transportation and storage of oil. Therefore, eucommia samara or eucommia seed oil can be used as raw materials to develop eucommia eucommia seed oil powder oil or solid beverage products, so as to fully exert the health care value of eucommia ulmoides seed oil, broaden the use of eucommia ulmoides seed oil and increase its added value.

通常,粉末油脂一般采用环糊精、明胶、阿拉伯胶等作为壁材,通过喷雾干燥技术进行制备。如,麻成金等(杜仲翅果籽油微胶囊化及抗氧化性能研究,食品科学,2005,26(9):261~264)公开了杜仲翅果籽油的微胶囊化方法,其以杜仲籽油为芯材、β-环糊精为壁材,先加热使环糊精溶解冷却后加入杜仲翅果籽油,在磁力搅拌器上搅拌一定时间,置于冰箱冷藏室中约48h,然后抽滤再真空干燥。又如,麻成金等(喷雾干燥法制备微胶囊化杜仲籽油的研究,中国粮油学报,2008,23(6):141~144)公开了喷雾干燥法制备微胶囊化杜仲籽油的工艺,其以杜仲籽油为芯材,壁材选用了明胶:麦芽糊精为3:2、A型纯胶:麦芽糊精为l:l、阿拉伯胶:麦芽糊精1:1.5三种复合壁材,将乳化剂、水和壁材混合溶解后,加入杜仲籽油,在30MPa压力下均质处理,在进风温度190℃、出风温度80~90℃条件下进行喷雾干燥。虽然上述两个技术方案均可制备出杜仲籽油粉末油脂产品,但是考虑到更加充分、合理的利用杜仲籽翅果,上述技术方案仍然有改进的空间。Generally, powdered oils and fats are generally prepared by spray drying technology using cyclodextrin, gelatin, gum arabic, etc. as wall materials. For example, Ma Chengjin et al. (Research on microencapsulation and antioxidant properties of eucommia samara seed oil, Food Science, 2005, 26(9): 261-264) disclosed a microencapsulation method for eucommia samara seed oil. Seed oil is the core material, and β-cyclodextrin is the wall material. First, heat to dissolve the cyclodextrin and cool it down, then add Eucommia samara seed oil, stir on a magnetic stirrer for a certain period of time, put it in the refrigerator for about 48 hours, and then Suction filtration and vacuum drying. As another example, Ma Chengjin et al. (Research on Microencapsulated Eucommia Seed Oil Prepared by Spray Drying Method, Chinese Journal of Cereals and Oils, 2008, 23 (6): 141-144) disclosed the process of preparing microencapsulated Eucommia ulmoides seed oil by spray drying method, It uses Eucommia ulmoides seed oil as the core material, and the wall material has selected three kinds of composite wall materials: gelatin: maltodextrin 3:2, A-type pure gum: maltodextrin 1:1, gum arabic: maltodextrin 1:1.5 , after mixing and dissolving the emulsifier, water and wall material, adding eucommia seed oil, homogenizing treatment under 30MPa pressure, and spray drying under the conditions of 190°C inlet air temperature and 80-90°C outlet air temperature. Although the above two technical solutions can prepare Eucommia ulmoides seed oil powder oil products, considering the more sufficient and reasonable utilization of eucommia samara, the above technical solutions still have room for improvement.

油脂包埋时使用的壁材主要有蛋白类、碳水化合物和亲水胶体等,如大豆蛋白、乳清蛋白、变性淀粉、阿拉伯胶等。申请人发现,杜仲翅果提取牡丹籽油剩余的籽粕中富含蛋白质、淀粉,并且会残余部分杜仲胶,因此可以利用籽粕为原料,进一步加工处理制备成可包埋牡丹籽油的壁材,这样实现了提油后的剩余物籽粕的回收利用,使杜仲籽翅果中的油脂、蛋白质、淀粉、胶质等被充分、合理利用。而且,现有技术中已经披露了通过水酶法工艺制备的大豆油和大豆蛋白作为制取粉末油脂的芯材和壁材的方案,具体的张雷等(响应面优化水酶法制备大豆粉末油脂,中国油脂,2017,42(3):12-17)公开了大豆粉末油脂的制备工艺,其利用新鲜的大豆进行清理后粉碎,加入碱性蛋白酶,进行酶解、灭酶、离心后,取离心后富含大豆油和大豆蛋白的液相,进一步添加复合乳化剂和麦芽糊精、酪蛋白酸钠,将液相经过恒温高速搅拌、高压均质、喷雾干燥,获得大豆粉末油脂。虽然该工艺实现了同时利用大豆中的大豆油、大豆蛋白分别作为芯材、壁材制备粉末油脂,但是却无法精确控制芯材大豆油、壁材大豆蛋白的比例,最终制备的产品质量并不稳定。The wall materials used for oil embedding mainly include proteins, carbohydrates, and hydrocolloids, such as soybean protein, whey protein, modified starch, and gum arabic. The applicant found that the remaining seed meal of extracting peony seed oil from Eucommia ulmoides samara is rich in protein and starch, and there will be a part of eucommia gum. Therefore, the seed meal can be used as a raw material for further processing to prepare a wall that can embed peony seed oil. In this way, the recycling of the residue seed meal after oil extraction is realized, so that the oil, protein, starch, gum, etc. in the eucommia samara are fully and rationally utilized. Moreover, soybean oil and soybean protein prepared by an aqueous enzymatic process have been disclosed in the prior art as a scheme for producing core materials and wall materials for powdered oils. Specifically, Zhang Lei et al. Grease, China Oils and Fats, 2017, 42(3):12-17) discloses the preparation process of soybean powder oil, which utilizes fresh soybeans to clean and pulverize, add alkaline protease, perform enzymolysis, deenzyme, and centrifugation, After centrifugation, the liquid phase rich in soybean oil and soybean protein is taken, and compound emulsifier, maltodextrin, and sodium caseinate are further added, and the liquid phase is subjected to constant temperature and high-speed stirring, high-pressure homogenization, and spray drying to obtain soybean powder oil. Although this process realizes the simultaneous use of soybean oil and soybean protein in soybeans as core material and wall material to prepare powdered oil, it cannot precisely control the ratio of core material soybean oil and wall material soybean protein, and the quality of the final product is not good. Stablize.

发明内容Contents of the invention

针对上述问题,本发明提供了一种杜仲籽油粉末冲剂及其制备方法,其以杜仲翅果为原料,先从杜仲翅果中提取杜仲籽油;然后合理利用提油后的废弃物杜仲籽粕为原料,采用机械球磨活化、超高压均质处理、喷雾干燥等技术,制备出富含小分子蛋白、淀粉及含有少量杜仲胶,同时具有较好包埋效果和乳化性能的籽粕活性粉;进一步,以杜仲籽油为芯材、籽粕活性粉为壁材通过超微细化处理、真空喷雾干燥,可制备出流动性、分散性良好的粉末油脂,且具备降血脂,降血压,促进神经系统、脑和视网膜的发育,预防老年痴呆症和过敏症等功效。In view of the above problems, the present invention provides a powder granule of Eucommia ulmoides seed oil and a preparation method thereof, which uses eucommia samara as raw material, first extracts eucommia ulmoides seed oil from eucommia samara; then rationally utilizes the waste Eucommia ulmoides seeds after oil extraction Dried meal is used as raw material, and activated by mechanical ball milling, ultra-high pressure homogeneous treatment, spray drying and other technologies to prepare seed meal active powder rich in small molecular protein, starch and a small amount of eucommia gum, which has good embedding effect and emulsifying performance ; Further, taking Eucommia ulmoides seed oil as the core material and seed dregs active powder as the wall material through ultrafine treatment and vacuum spray drying, powder oil with good fluidity and dispersibility can be prepared, and it has the functions of lowering blood fat, lowering blood pressure, promoting The development of the nervous system, brain and retina, the prevention of Alzheimer's disease and allergies, etc.

一种杜仲籽油粉末冲剂的制备方法,其特征在于包括如下步骤:A preparation method of Eucommia ulmoides seed oil powder granule, is characterized in that comprising the steps:

1)原料预处理:将杜仲翅果干燥至含水量低于12%,剥去杜仲翅果的果壳之后粉碎至粒度为10~20目,获得杜仲翅果粉;1) Raw material pretreatment: drying the eucommia samara until the water content is lower than 12%, peeling off the husk of the eucommia samara and crushing to a particle size of 10-20 mesh to obtain eucommia samara powder;

2)真空微波湿热处理:于步骤(1)获得的杜仲翅果粉的表面喷施清水,同时不断搅拌均匀,直至杜仲翅果粉最终的含水量为25~35%,之后转移至微波炉腔体内,进行真空微波处理,控制杜仲翅果粉的水分含量为9%~12%;现有技术中,采用超临界萃取提取油脂只需要将原料干燥并粉碎,控制好原料粒度和水分含量(通常粒度太小,夹带剂的通透性变差;粒度太大,原料内的脂肪不易脱离;水分含量太高,成品油水分含量高;水分含量过低,干燥的难度和成本增加);一般超临界萃取后饼粕的残油率为2%~4%,为了进一步降低饼粕残油率只能调整萃取工艺,但是使用更加严苛的萃取工艺,如延长萃取时间、增加萃取压力等,会使成本大幅增加或较难实现;而通过本发明上述步骤,可以使杜仲翅果粉在真空微波湿热处理过程中,先吸水溶胀(表面喷施清水),然后通过真空微波作用,使水份在快速蒸发的同时形成分子通道,并将油脂夹带出来,可以提高后续超临界萃取的得率和降低饼粕的残油率。实施例2中具体给出了真空微波湿热处理后超临界萃取的残油率数据。2) Vacuum microwave heat treatment: Spray water on the surface of the eucommia samara powder obtained in step (1), while stirring continuously until the final moisture content of the eucommia samara powder is 25-35%, then transfer it to the cavity of a microwave oven, and carry out Vacuum microwave treatment controls the moisture content of eucommia samara powder to be 9% to 12%; in the prior art, adopting supercritical extraction to extract oil only needs to dry and pulverize the raw materials, and control the particle size and moisture content of the raw materials (usually the particle size is too small, The permeability of the entrainer becomes poor; the particle size is too large, and the fat in the raw material is not easy to detach; the moisture content is too high, and the moisture content of the finished oil is high; the moisture content is too low, the difficulty and cost of drying increase); general supercritical extraction The residual oil rate of the meal is 2% to 4%. In order to further reduce the residual oil rate of the meal, the extraction process can only be adjusted, but the use of a more stringent extraction process, such as prolonging the extraction time and increasing the extraction pressure, will greatly increase the cost Or difficult to realize; And by above-mentioned steps of the present invention, can make ulmoides ulmoides samara powder, in the vacuum microwave wet-heat treatment process, absorb water and swell earlier (clear water is sprayed on the surface), then by vacuum microwave action, make moisture content form while rapid evaporation Molecular channels and entrainment of oil can improve the yield of subsequent supercritical extraction and reduce the residual oil rate of cake. In Example 2, the residual oil rate data of supercritical extraction after vacuum microwave heat treatment are given in detail.

3)超临界萃取提油:以步骤(2)获得的杜仲翅果粉为原料,采用超临界萃取提油,获得杜仲籽油和杜仲籽粕;3) Oil extraction by supercritical extraction: using the Eucommia samara powder obtained in step (2) as a raw material, adopting supercritical extraction to extract oil to obtain Eucommia ulmoides seed oil and Eucommia ulmoides seed meal;

4)机械球磨活化:取步骤(3)获得的杜仲籽粕与清水按质量比1:3~7混合均匀,之后利用胶体磨反复匀浆,使浆液以重量计95%以上可以通过100目筛,获得籽粕浆液;将籽粕浆液过100目筛,收集筛下物加入球磨机内,进行机械球磨,之后离心,得上层活化籽粕浆液和下层沉淀;通过该步骤,可以使籽粕浆液的中的蛋白质、淀粉等在机械球磨的摩擦、碰撞、冲击等机械力作用下,使晶体结构及物化性能发生改变,如蛋白质分解成小分子蛋白、破坏淀粉晶格结构使其变性,以形成具有较好包埋、乳化效果的活性物;4) Mechanical ball milling activation: take the Eucommia ulmoides seed meal obtained in step (3) and clear water and mix evenly in a mass ratio of 1:3 to 7, and then use a colloid mill to repeatedly homogenize, so that more than 95% of the slurry can pass through a 100-mesh sieve by weight , to obtain seed meal slurry; pass the seed meal slurry through a 100-mesh sieve, collect the under-screened material and add it to a ball mill, perform mechanical ball milling, and then centrifuge to obtain the upper layer of activated seed meal slurry and the lower layer of precipitation; through this step, the seed meal slurry can be made Under the action of mechanical forces such as friction, collision, and impact of mechanical ball milling, the protein and starch in the powder will change the crystal structure and physical and chemical properties, such as decomposing protein into small molecular proteins, destroying the starch lattice structure and denaturing it to form Active substances with better embedding and emulsifying effects;

5)超高压均质处理:将步骤(4)得到的活化籽粕浆液过200目筛,取筛下物于120~150Mpa的条件下进行超高压均质处理,使活化籽粕浆液的粒度小于200nm;进一步通过该步骤,在超高压的作用下,可以使活化籽粕浆液的粒度达纳米级,进一步形成具有较好包埋、乳化效果的活性物;5) Ultra-high pressure homogenization treatment: pass the activated seed meal slurry obtained in step (4) through a 200-mesh sieve, and take the under-sieve to carry out ultra-high pressure homogenization treatment under the condition of 120-150Mpa, so that the particle size of the activated seed meal slurry is less than 200nm; further through this step, under the action of ultra-high pressure, the particle size of the activated seed meal slurry can reach the nanometer level, and further form active substances with better embedding and emulsifying effects;

6)浓缩干燥:将经步骤(5)处理后的活化籽粕浆液浓缩至固形物含量为15%~25%,之后喷雾干燥制粉,获得籽粕活性粉;6) Concentrating and drying: Concentrating the activated seed meal slurry treated in step (5) to a solid content of 15% to 25%, and then spray drying to make powder to obtain active seed meal powder;

7)调配干燥:取步骤(3)获得的杜仲籽油、步骤(6)获得的籽粕活性粉、清水混合后进行高速搅拌,之后于150~180Mpa的条件下进行超微细化处理,使乳液的粒度小于120nm,然后真空低温喷雾干燥制粉,即可;该步骤中,通过超微细化处理可完成籽粕活性粉对杜仲籽油的包埋,并使杜仲籽油、籽粕活性粉、清水形成纳米级的均匀乳液,使干燥后的产品具备优良的分散性、流动性和溶解性;进一步,该步骤中采用真空低温喷雾干燥,可避免杜仲籽油中亚麻酸被氧化破坏;真空低温喷雾干燥的条件优选为:真空度0.80~0.98MPa,进风温度80~95℃;7) Preparation and drying: take the Eucommia ulmoides seed oil obtained in step (3), the seed meal active powder obtained in step (6), and clear water and mix them with high-speed stirring. The particle size is less than 120nm, and then vacuum low-temperature spray drying to make powder; in this step, the embedding of Eucommia ulmoides seed oil by seed meal active powder can be completed through ultra-fine treatment, and Eucommia ulmoides seed oil, seed meal active powder, Clear water forms a nano-scale uniform emulsion, so that the dried product has excellent dispersibility, fluidity and solubility; further, vacuum low-temperature spray drying is used in this step to avoid oxidative damage to linolenic acid in Eucommia seed oil; vacuum low-temperature The preferred conditions for spray drying are: vacuum degree 0.80-0.98MPa, air inlet temperature 80-95°C;

对于通过上述步骤:原料预处理、真空微波湿热处理、超临界萃取提油、机械球磨活化、超高压均质处理、浓缩干燥、调配干燥制备的杜仲籽油粉末冲剂,实施例3中给出了杜仲籽油粉末冲剂的包埋率、溶解性、过氧化值、含水率等的数据;For the eucommia seed oil powder granules prepared by the above steps: raw material pretreatment, vacuum microwave wet heat treatment, supercritical extraction oil extraction, mechanical ball milling activation, ultra-high pressure homogenization treatment, concentrated drying, and preparation and drying, given in Example 3 The data of entrapment rate, solubility, peroxide value, moisture content, etc. of Eucommia ulmoides seed oil powder granules;

上述步骤中,步骤(5)中活化籽粕浆液、步骤(7)中乳液的粒度采用GB/T19627-2005“粒度分析—光子相关光谱法”(PCS法)进行检测,粒度均用中位粒径(D50)表示;水分含量、固定物含量的检测采用常压105℃烘干法。In the above steps, the particle size of the activated seed meal slurry in step (5) and the emulsion in step (7) are detected by GB/T19627-2005 "Particle Size Analysis-Photon Correlation Spectroscopy" (PCS method), and the particle size is measured by median particle size. Diameter (D50) means; the detection of moisture content and fixed matter content adopts the normal pressure 105 ℃ drying method.

作为具体技术方案,所述步骤(2)中,真空微波处理的条件为:真空度0.90~0.98MPa、微波剂量为0.25~5kw/kg。As a specific technical solution, in the step (2), the vacuum microwave treatment conditions are: vacuum degree 0.90-0.98 MPa, microwave dose 0.25-5 kw/kg.

作为具体技术方案,所述步骤(3)中,超临界萃取的条件为:萃取压力30~45MPa,萃取时间1~3h,萃取温度42~55℃,分离温度28~32℃,CO2流量25~30kg/h。As a specific technical scheme, in the step (3), the conditions for supercritical extraction are: extraction pressure 30-45MPa, extraction time 1-3h, extraction temperature 42-55°C, separation temperature 28-32°C, CO Flow rate 25 ~30kg/h.

作为具体技术方案,所述步骤(4)中,球磨的工艺条件为:球磨机转速80~500r/min、球磨介质填充率8%~30%、球磨时间1~4h。As a specific technical solution, in the step (4), the technical conditions of the ball milling are: ball mill speed 80-500r/min, ball milling medium filling rate 8%-30%, ball milling time 1-4h.

作为优选技术方案,所述步骤(4)中,球磨的工艺条件为:球磨机转速220~300r/min、球磨介质填充率10%~12%、球磨时间2~3h。As a preferred technical solution, in the step (4), the technical conditions of the ball milling are: the speed of the ball mill is 220-300 r/min, the filling rate of the ball milling medium is 10%-12%, and the ball milling time is 2-3 hours.

作为具体技术方案,所述步骤(7)中,杜仲籽油、籽粕活性粉、清水以质量计的比例为2~5:5~10:40~50。As a specific technical solution, in the step (7), the ratio by mass of Eucommia ulmoides seed oil, seed meal active powder, and clear water is 2-5:5-10:40-50.

作为具体技术方案,所述步骤(7)中,还包括加入功能成分与杜仲籽油、籽粕活性粉、清水混合;所述功能成分含有:As a specific technical solution, in the step (7), it also includes adding functional ingredients and mixing with Eucommia ulmoides seed oil, seed meal active powder, and clear water; the functional ingredients contain:

1)葛根提取物、山楂提取物、大豆提取物、红茶提取物中的一种或多种;1) One or more of kudzu root extract, hawthorn extract, soybean extract, and black tea extract;

2)维生素E、迷迭香提取物、茶多酚中的一种或多种;通过上述配伍,在杜仲籽油的基础上,可添加具有降血脂作用的葛根提取物、山楂提取物、大豆提取物、红茶提取物,可以进一步增强产品的降血脂的功效,以生产具有辅助降血脂作用的保健品;另外,加入具有抗氧化作用的维生素E、迷迭香提取物、茶多酚,可以防止高亚麻酸含量的杜仲籽油的氧化,以延长产品的货架期,维持产品的功效稳定。2) One or more of vitamin E, rosemary extract, and tea polyphenols; through the above compatibility, on the basis of eucommia seed oil, kudzu root extract, hawthorn extract, soybean Extract and black tea extract can further enhance the blood lipid-lowering effect of the product, so as to produce health care products with auxiliary blood lipid-lowering effect; in addition, adding vitamin E, rosemary extract, and tea polyphenols with antioxidant effects can Prevent the oxidation of eucommia seed oil with high linolenic acid content to prolong the shelf life of the product and maintain the stability of the product's efficacy.

作为具体技术方案,所述步骤(7)中,还包括加入营养强化剂与杜仲籽油、籽粕活性粉、清水混合;所述营养强化剂至少含有:蛋白质、碳水化合物、α-乳清蛋白、二十二碳六烯酸、益生菌、核苷酸、卵磷脂、乳清钙、花生四烯酸;杜仲籽油富含亚麻酸,可以为人体提供丰富的亚麻酸,另外蛋白质、碳水化合物、α-乳清蛋白、二十二碳六烯酸、益生菌、核苷酸、卵磷脂、乳清钙、花生四烯酸等是婴幼儿生长所需的营养活性物质;因此通过上述配伍,使本产品可作为婴幼儿食品使用。As a specific technical solution, in the step (7), it also includes adding a nutritional fortifier and mixing it with Eucommia ulmoides seed oil, seed meal active powder, and clear water; the nutritional fortifier contains at least: protein, carbohydrates, α-lactalbumin , docosahexaenoic acid, probiotics, nucleotides, lecithin, whey calcium, arachidonic acid; Eucommia seed oil is rich in linolenic acid, which can provide rich linolenic acid for the human body, and protein, carbohydrates , α-lactalbumin, docosahexaenoic acid, probiotics, nucleotides, lecithin, whey calcium, arachidonic acid, etc. are nutritionally active substances required for the growth of infants; therefore, through the above compatibility, This product can be used as food for infants and young children.

作为具体技术方案,所述步骤(7)中,还包括加入微胶囊壁材、乳化剂与杜仲籽油、籽粕活性粉、清水混合;所述微胶囊壁材为环状糊精、阿拉伯胶、壳聚糖中的一种或几种;所述乳化剂为单硬脂酸甘油酯、蔗糖脂肪酸酯;当产品配方中添加其它性能不同、种类不同的功能成分、营养强化剂后,为了进一步改善和稳定最终产品的质量,可以使用常规的微胶囊壁材、乳化剂等。As a specific technical solution, in the step (7), it also includes adding microcapsule wall material, emulsifier and Eucommia ulmoides seed oil, seed meal active powder, clear water and mixing; the microcapsule wall material is cyclodextrin, gum arabic , one or more of chitosan; the emulsifier is glyceryl monostearate and sucrose fatty acid ester; To further improve and stabilize the quality of the final product, conventional microcapsule wall materials, emulsifiers, etc. can be used.

采用上述任一所述方法制备的杜仲籽油粉末冲剂。Eucommia ulmoides seed oil powder granules prepared by any of the methods described above.

具体实施方式Detailed ways

下面结合具体实施方式对本发明做进一步的说明,需要指出的是以下实施方式仅是以例举的形式对本发明所做的解释性说明,但本发明的保护范围并不仅限于此,所有本领域的技术人员以本发明的精神对本发明所做的等效的替换均落入本发明的保护范围。The present invention will be further described below in conjunction with specific embodiments. It should be pointed out that the following embodiments are only explanatory descriptions of the present invention in the form of examples, but the protection scope of the present invention is not limited thereto. Equivalent replacements made by the skilled person to the present invention based on the spirit of the present invention all fall within the protection scope of the present invention.

实施例1Example 1

一种杜仲籽油粉末冲剂的制备方法,包括如下步骤:A preparation method of eucommia seed oil powder granules, comprising the steps of:

1)原料预处理:将杜仲翅果用电热鼓风干燥箱干燥至含水量低于12%,剥去杜仲翅果的果壳之后使用微型植物粉碎机粉碎至粒度为10~20目,获得杜仲翅果粉;1) Raw material pretreatment: Dry the eucommia samara with an electric blast drying oven until the water content is lower than 12%, peel off the husk of the eucommia samara, and use a micro-plant pulverizer to crush it to a particle size of 10-20 meshes to obtain the eucommia ulmoides Samara powder;

2)真空微波湿热处理:于步骤(1)获得的杜仲翅果粉的表面喷施清水,同时不断搅拌均匀,直至杜仲翅果粉最终的含水量为25~35%,之后转移至微波炉腔体内,于真空度0.90~0.98MPa、微波剂量为1.5kw/kg条件下进行真空微波处理,控制杜仲翅果粉的水分含量为9%~12%;2) Vacuum microwave heat treatment: Spray water on the surface of the eucommia samara powder obtained in step (1), while stirring continuously until the final water content of the eucommia samara powder is 25-35%, then transfer it to the cavity of the microwave oven, and Vacuum microwave treatment is carried out under the condition of vacuum degree of 0.90-0.98MPa and microwave dose of 1.5kw/kg, and the moisture content of Eucommia samara powder is controlled at 9%-12%;

3)超临界萃取提油:以步骤(2)获得的杜仲翅果粉为原料,采用超临界萃取设备于萃取压力42MPa,萃取时间2h,萃取温度45℃,分离温度30℃,CO2流量25~30kg/h的条件下提油,获得杜仲籽油和杜仲籽粕;经检测,得到的杜仲籽油过氧化值为1.23mmol/kg,酸价为0.18mg/g;杜仲籽粕中含蛋白质36.53%,含淀粉18.32%;3) Oil extraction by supercritical extraction: using the eucommia samara powder obtained in step (2) as raw material, using supercritical extraction equipment at an extraction pressure of 42 MPa, an extraction time of 2 hours, an extraction temperature of 45°C, a separation temperature of 30°C, and a CO flow rate of 25 to The oil was extracted under the condition of 30kg/h to obtain eucommia seed oil and eucommia seed meal; after testing, the peroxidation value of the obtained eucommia seed oil was 1.23mmol/kg, and the acid value was 0.18mg/g; the protein content in eucommia ulmoides seed meal was 36.53 %, containing 18.32% starch;

4)机械球磨活化:取步骤(3)获得的杜仲籽粕与清水按质量比1:3~7混合均匀,之后利用胶体磨反复匀浆,使浆液以重量计95%以上可以通过100目筛,获得籽粕浆液;将籽粕浆液过100目筛,收集筛下物加入球磨机内,于球磨机转速220~300r/min、球磨介质填充率10%~12%、球磨时间2~3h下进行机械球磨,之后离心,得上层活化籽粕浆液和下层沉淀;4) Mechanical ball milling activation: take the Eucommia ulmoides seed meal obtained in step (3) and clear water and mix evenly in a mass ratio of 1:3 to 7, and then use a colloid mill to repeatedly homogenize, so that more than 95% of the slurry can pass through a 100-mesh sieve by weight , to obtain the seed meal slurry; pass the seed meal slurry through a 100-mesh sieve, collect the undersieve and put it into the ball mill, and perform mechanical grinding at a ball mill speed of 220-300r/min, a ball milling medium filling rate of 10%-12%, and a ball milling time of 2-3h. Ball milling, followed by centrifugation, to obtain the upper activated seed meal slurry and the lower sediment;

5)超高压均质处理:将步骤(4)得到的活化籽粕浆液过200目筛,取筛下物于120~150Mpa的条件下利用纳米对撞机进行超高压均质处理,使活化籽粕浆液的粒度小于200nm;5) Ultra-high pressure homogenization treatment: pass the activated seed meal slurry obtained in step (4) through a 200-mesh sieve, take the under-sieve and use a nano collider to perform ultra-high pressure homogenization treatment under the condition of 120-150Mpa, so that the activated seed meal The particle size of the meal slurry is less than 200nm;

6)浓缩干燥:将经步骤(5)处理后的活化籽粕浆液浓缩至固形物含量为15%~25%、之后于进风温度160~185℃的条件下进行喷雾干燥制粉,获得籽粕活性粉;6) Concentration and drying: Concentrate the activated seed meal slurry treated in step (5) to a solid content of 15% to 25%, and then spray dry and make powder under the condition of an inlet air temperature of 160 to 185°C to obtain seed Meal active powder;

7)调配干燥:取步骤(3)获得的杜仲籽油、步骤(6)获得的籽粕活性粉、清水混合后进行高速搅拌,之后于150~180Mpa的条件下利用纳米对撞机进行超微细化90℃的条件下进行真空低温喷雾干燥制粉,即可;7) Deployment and drying: take the eucommia seed oil obtained in step (3), the seed meal active powder obtained in step (6), and clear water and mix them with high-speed stirring, and then use a nano collider to carry out ultrafine Under the condition of 90℃, carry out vacuum low-temperature spray drying to make powder;

上述步骤中,主要原料杜仲翅果由湘西老爹生物有限公司提供;主要仪器设备:微型植物粉碎机,FZ102型,天津市泰斯特仪器有限公司;电热鼓风干燥箱,101-2AB型,天津市泰斯特仪器有限公司;超临界萃取设备,型号HA420-40-96,南通市华安超临界萃取有限公司;纳米对撞机,20/150D型,廊坊通用机械制造有限公司;喷雾干燥机,SD-04型,长沙海凌生物科技有限公司;In the above steps, the main raw material Eucommia ulmoides Samara was provided by Xiangxi Laodi Biological Co., Ltd.; the main equipment: miniature plant pulverizer, FZ102 type, Tianjin Test Instrument Co., Ltd.; electric blast drying oven, 101-2AB type, Tianjin Test Instrument Co., Ltd.; supercritical extraction equipment, model HA420-40-96, Nantong Huaan Supercritical Extraction Co., Ltd.; nano collider, 20/150D type, Langfang General Machinery Manufacturing Co., Ltd.; spray dryer , SD-04 type, Changsha Hailing Biotechnology Co., Ltd.;

上述步骤中,步骤(5)中活化籽粕浆液、步骤(7)中乳液的粒度采用GB/T19627-2005“粒度分析—光子相关光谱法”(PCS法)进行检测,粒度均用中位粒径(D50)表示;水分含量、固定物含量的检测采用常压105℃烘干法;过氧化值的测定采用GB/T 5538的方法;酸价的测定采用GB/T 5530的方法;蛋白质含量的测定采用微量凯氏定氮法;淀粉含量的测定采用GB/T 5009.9的方法。In the above steps, the particle size of the activated seed meal slurry in step (5) and the emulsion in step (7) are detected by GB/T19627-2005 "Particle Size Analysis-Photon Correlation Spectroscopy" (PCS method), and the particle size is measured by median particle size. The diameter (D50) is indicated; the detection of moisture content and fixed substance content adopts the drying method at 105 °C under normal pressure; the determination of peroxide value adopts the method of GB/T 5538; the determination of acid value adopts the method of GB/T 5530; protein content Determination of micro-Kjeldahl method; determination of starch content using the method of GB/T 5009.9.

实施例2Example 2

真空微波湿热处理对超临界萃取的残油率影响测定。Determination of the effect of vacuum microwave heat treatment on the residual oil rate of supercritical extraction.

1、杜仲籽粕的制备1. Preparation of eucommia seed meal

真空微波湿热处理组:采用实施例1的方法,取超临界萃取提油后得到的杜仲籽粕测定残油率;Vacuum microwave wet heat treatment group: adopt the method of Example 1, take the Eucommia ulmoides seed meal obtained after supercritical extraction and oil extraction, and measure the residual oil rate;

常规方法对照组:采用实施例1的方法,但不进行真空微波湿热处理,取超临界萃取提油后得到的杜仲籽粕测定残油率。Conventional method control group: adopt the method of Example 1, but without vacuum microwave heat treatment, take the Eucommia ulmoides seed meal obtained after supercritical extraction to measure the residual oil rate.

2、残油率的测定2. Determination of residual oil rate

每组取3份样品检测,残油率的测定采用索氏抽提法。Three samples were taken from each group for testing, and the residual oil rate was determined by Soxhlet extraction method.

3、结果分析3. Analysis of results

表1真空微波湿热处理对超临界萃取的残油率影响Table 1 Effect of vacuum microwave heat treatment on the residual oil rate of supercritical extraction

由表1可知,采用本发明方法,先对杜仲翅果粉进行真空微波湿热处理后,超临界萃取的剩余物杜仲籽粕残油率更低。It can be known from Table 1 that, by adopting the method of the present invention, after the eucommia samara powder is first subjected to vacuum microwave heat treatment, the residue of eucommia ulmoides seed meal after supercritical extraction has a lower residual oil rate.

实施例3Example 3

本发明杜仲籽油粉末冲剂的包埋率、流动性、溶解性、过氧化值、含水率等指标的测定。Determination of indicators such as embedding rate, fluidity, solubility, peroxide value, moisture content and the like of the eucommia seed oil powder granule of the present invention.

1、包埋率的测定1. Determination of embedding rate

包埋率=(1-表面油含量/总含量油)×100%Embedding rate=(1-surface oil content/total oil content)×100%

杜仲籽油粉末冲剂表面油含量测定:以石油醚为溶剂,准确称取5.0g杜仲籽油粉末冲剂样品,将120mL石油醚分三次加入,每次均充分振荡,过滤、合并滤液,滤液经减压浓缩后,所得油脂质量即为杜仲籽油粉末冲剂表面油含量。Determination of surface oil content of eucommia seed oil powder granules: using petroleum ether as a solvent, accurately weigh 5.0g eucommia eucommia seed oil powder granules, add 120mL petroleum ether in three times, shake fully each time, filter and combine the filtrates, and the filtrates are reduced After pressing and concentrating, the quality of the obtained oil is the surface oil content of the eucommia seed oil powder granule.

杜仲籽油粉末冲剂总含油量测定:用无水乙醚作溶剂,准确称量5.0g杜仲籽油粉末冲剂样品,加入150~180mL无水乙醚,索氏提取4~6h,收集无水乙醚减压蒸馏,所得油脂质量即为杜仲籽油粉末冲剂总含油量测定。Determination of the total oil content of eucommia seed oil powder granules: use anhydrous ether as a solvent, accurately weigh 5.0 g of eucommia eucommia seed oil powder granules, add 150-180 mL of anhydrous ether, extract by Soxhlet for 4-6 hours, collect anhydrous ether under reduced pressure Distillation, the quality of the obtained oil is the total oil content of the eucommia seed oil powder granule.

2、溶解性2. Solubility

取1g杜仲籽油粉末冲剂(m1)于50mL烧杯中,加入10mL蒸馏水(25℃),用秒表开始计时保持60s,立即取复水后的杜仲籽油粉末冲剂1mL于恒重的铝盒中,放入105±2℃的烘箱中干燥4h,称重(m2),然后按下式计算其溶解性,同时用市售奶粉作对比。Take 1g of eucommia seed oil powder granule (m 1 ) in a 50mL beaker, add 10mL of distilled water (25°C), start timing with a stopwatch for 60s, immediately take 1mL of eucommia ulmoides seed oil powder granule in an aluminum box with constant weight , dried in an oven at 105±2°C for 4 hours, weighed (m 2 ), and then calculated its solubility according to the following formula, while using commercially available milk powder for comparison.

式中:In the formula:

m1,杜仲籽油粉末冲剂质量,g;m 1 , mass of eucommia seed oil powder granule, g;

m2,复水干燥后的杜仲籽油粉末冲剂质量,g。m 2 , mass of eucommia seed oil powder granule after rehydration and drying, g.

3、流动性的测定3. Determination of fluidity

将漏斗固定保持铅直,漏斗口离桌面高约8cm,桌面放置白纸,将50g杜仲籽油粉末冲剂从漏斗加入,测定自由下落在白纸上所形成锥形的底部直径,用直径的大小来判别其流动性的大小。同时用市售奶粉作对比,直径越大表示流动性越好。Fix the funnel and keep it vertical. The height of the funnel mouth is about 8cm from the tabletop. Place a white paper on the tabletop. Add 50g Eucommia ulmoides seed oil powder granule from the funnel. Measure the diameter of the bottom of the cone formed by free falling on the white paper. To determine the size of its mobility. At the same time, compared with commercially available milk powder, the larger the diameter, the better the fluidity.

4、过氧化值、含水量的测定4. Determination of peroxide value and water content

杜仲籽油粉末冲剂的过氧化值按照GB/T 5538的方法测定;含水量采用105℃常压干燥法。The peroxide value of Eucommia ulmoides seed oil powder granule was determined according to the method of GB/T 5538; the water content was dried under normal pressure at 105°C.

5、测定结果5. Measurement results

表2本发明杜仲籽油粉末冲剂的包埋率、流动性、溶解性、过氧化值、含水率Table 2 Embedding rate, fluidity, solubility, peroxide value, water content of Eucommia ulmoides seed oil powder granule of the present invention

项目project 市售奶粉commercial milk powder 本发明杜仲籽油粉末冲剂Eucommia ulmoides seed oil powder granule of the present invention 包埋率/%Embedding rate/% -- 86.486.4 溶解性/%Solubility/% 86.886.8 78.978.9 流动性/cmLiquidity/cm 9.869.86 9.729.72 过氧化值/(mmol/kg)Peroxide value/(mmol/kg) -- 1.381.38 含水量/%Moisture content/% -- 6.756.75

由表2可知,本发明杜仲籽油粉末冲剂的包埋率为86.4%,处于较高水平,说明通过机械球磨活化、超高压均质处理后的籽粕活性粉具有较好的包埋效果;本发明杜仲籽油粉末冲剂的流动性为9.72cm,与市售奶粉差异不大,而溶解度为78.8%,稍低于市售奶粉;另外,本发明杜仲籽油粉末冲剂的过氧化值较低,为1.38mmol/kg,说明通过籽粕活性粉对杜仲籽油的包埋和真空低温喷雾干燥,可以有效抑制杜仲籽油的氧化劣变。As can be seen from Table 2, the embedding rate of Eucommia ulmoides seed oil powder granule of the present invention is 86.4%, which is at a relatively high level, indicating that the active powder of seed meal activated by mechanical ball milling and ultra-high pressure homogenization has a better embedding effect; The fluidity of the eucommia seed oil powder granule of the present invention is 9.72 cm, which is not much different from the commercially available milk powder, while the solubility is 78.8%, which is slightly lower than the commercially available milk powder; in addition, the peroxide value of the eucommia ulmoides seed oil powder granule of the present invention is relatively low , was 1.38mmol/kg, indicating that the oxidative deterioration of eucommia seed oil can be effectively inhibited by embedding eucommia ulmoides seed oil in seed meal active powder and vacuum low-temperature spray drying.

Claims (10)

1.一种杜仲籽油粉末冲剂的制备方法,其特征在于包括如下步骤:1. a preparation method of eucommia seed oil powder granule, is characterized in that comprising the steps: 1)原料预处理:将杜仲翅果干燥至含水量低于12%,剥去杜仲翅果的果壳之后粉碎至粒度为10~20目,获得杜仲翅果粉;1) Raw material pretreatment: drying the eucommia samara until the water content is lower than 12%, peeling off the husk of the eucommia samara and crushing to a particle size of 10-20 mesh to obtain eucommia samara powder; 2)真空微波湿热处理:于步骤(1)获得的杜仲翅果粉的表面喷施清水,同时不断搅拌均匀,直至杜仲翅果粉最终的含水量为25~35%,之后转移至微波炉腔体内,进行真空微波处理,控制杜仲翅果粉的水分含量为9%~12%;2) Vacuum microwave heat treatment: Spray water on the surface of the eucommia samara powder obtained in step (1), while stirring continuously until the final moisture content of the eucommia samara powder is 25-35%, then transfer it to the cavity of a microwave oven, and carry out Vacuum microwave treatment to control the moisture content of eucommia samara powder to 9% to 12%; 3)超临界萃取提油:以步骤(2)获得的杜仲翅果粉为原料,采用超临界萃取提油,获得杜仲籽油和杜仲籽粕;3) Oil extraction by supercritical extraction: using the Eucommia samara powder obtained in step (2) as a raw material, adopting supercritical extraction to extract oil to obtain Eucommia ulmoides seed oil and Eucommia ulmoides seed meal; 4)机械球磨活化:取步骤(3)获得的杜仲籽粕与清水按质量比1:3~7混合均匀,之后利用胶体磨反复匀浆,使浆液以重量计95%以上可以通过100目筛,获得籽粕浆液;将籽粕浆液过100目筛,收集筛下物加入球磨机内,进行机械球磨,之后离心,得上层活化籽粕浆液和下层沉淀;4) Mechanical ball milling activation: take the Eucommia ulmoides seed meal obtained in step (3) and clear water and mix evenly in a mass ratio of 1:3 to 7, and then use a colloid mill to repeatedly homogenize, so that more than 95% of the slurry can pass through a 100-mesh sieve by weight , to obtain a seed meal slurry; pass the seed meal slurry through a 100-mesh sieve, collect the under-sieve material and add it to a ball mill, perform mechanical ball milling, and then centrifuge to obtain the activated seed meal slurry in the upper layer and the sediment in the lower layer; 5)超高压均质处理:将步骤(4)得到的活化籽粕浆液过200目筛,取筛下物于120~150Mpa的条件下进行超高压均质处理,使活化籽粕浆液的粒度小于200nm;5) Ultra-high pressure homogenization treatment: pass the activated seed meal slurry obtained in step (4) through a 200-mesh sieve, and take the under-sieve to carry out ultra-high pressure homogenization treatment under the condition of 120-150Mpa, so that the particle size of the activated seed meal slurry is less than 200nm; 6)浓缩干燥:将经步骤(5)处理后的活化籽粕浆液浓缩至固形物含量为15%~25%,之后喷雾干燥制粉,获得籽粕活性粉;6) Concentrating and drying: Concentrating the activated seed meal slurry treated in step (5) to a solid content of 15% to 25%, and then spray drying to make powder to obtain active seed meal powder; 7)调配干燥:取步骤(3)获得的杜仲籽油、步骤(6)获得的籽粕活性粉、清水混合后进行高速搅拌,之后于150~180Mpa的条件下进行超微细化处理,使乳液的粒度小于120nm,然后真空低温喷雾干燥制粉,即可。7) Preparation and drying: take the Eucommia ulmoides seed oil obtained in step (3), the seed meal active powder obtained in step (6), and clear water and mix them with high-speed stirring. The particle size is less than 120nm, and then vacuum low-temperature spray drying to make powder. 2.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(2)中,真空微波处理的条件为:真空度为0.90~0.98MPa、微波剂量为0.25~5kw/kg。2. a kind of Eucommia ulmoides seed oil powder granule as claimed in claim 1, is characterized in that in described step (2), the condition of vacuum microwave treatment is: vacuum degree is 0.90~0.98MPa, microwave dosage is 0.25~5kw/ kg. 3.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(3)中,超临界萃取的条件为:萃取压力30~45MPa,萃取时间1~3h,萃取温度42~55℃,分离温度28~32℃,CO2流量25~30kg/h。3. a kind of eucommia seed oil powder granule as claimed in claim 1, it is characterized in that in described step (3), the condition of supercritical extraction is: extraction pressure 30~45MPa, extraction time 1~3h, extraction temperature 42 ~55℃, separation temperature 28~32℃, CO 2 flow rate 25~30kg/h. 4.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(4)中,球磨的工艺条件为:球磨机转速80~500r/min、球磨介质填充率8%~30%、球磨时间1~4h。4. a kind of Eucommia ulmoides seed oil powder granule as claimed in claim 1, is characterized in that in described step (4), the process condition of ball mill is: ball mill rotating speed 80~500r/min, ball mill medium filling rate 8%~30 %, ball milling time 1 ~ 4h. 5.如权利要求4所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(4)中,球磨的工艺条件为:球磨机转速220~300r/min、球磨介质填充率10%~12%、球磨时间2~3h。5. A kind of Eucommia ulmoides seed oil powder granule as claimed in claim 4, is characterized in that in described step (4), the process condition of ball mill is: ball mill rotating speed 220~300r/min, ball mill medium filling rate 10%~12 %, ball milling time 2 ~ 3h. 6.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(7)中,杜仲籽油、籽粕活性粉、清水以质量计的比例为2~5:5~10:40~50。6. a kind of eucommia seed oil powder granule as claimed in claim 1, is characterized in that in described step (7), the ratio by mass of eucommia seed oil, seed meal active powder, clear water is 2~5:5~ 10:40-50. 7.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(7)中,还包括加入功能成分与杜仲籽油、籽粕活性粉、清水混合;所述功能成分含有:7. a kind of eucommia seed oil powder granule as claimed in claim 1, is characterized in that in described step (7), also comprises adding functional ingredient and mixes with eucommia seed oil, seed dregs active powder, clear water; Said functional ingredient contain: 1)葛根提取物、山楂提取物、大豆提取物、红茶提取物中的一种或多种;1) One or more of kudzu root extract, hawthorn extract, soybean extract, and black tea extract; 2)维生素E、迷迭香提取物、茶多酚中的一种或多种。2) One or more of vitamin E, rosemary extract, and tea polyphenols. 8.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(7)中,还包括加入营养强化剂与杜仲籽油、籽粕活性粉、清水混合;所述营养强化剂至少含有:蛋白质、碳水化合物、α-乳清蛋白、二十二碳六烯酸、益生菌、核苷酸、卵磷脂、乳清钙、花生四烯酸。8. a kind of eucommia seed oil powder granule as claimed in claim 1, is characterized in that in described step (7), also comprises adding nutrition enhancer and mixes with eucommia seed oil, seed dregs active powder, clear water; The fortifier contains at least: protein, carbohydrates, α-lactalbumin, docosahexaenoic acid, probiotics, nucleotides, lecithin, whey calcium, and arachidonic acid. 9.如权利要求1所述的一种杜仲籽油粉末冲剂,其特征在于所述步骤(7)中,还包括加入微胶囊壁材、乳化剂与杜仲籽油、籽粕活性粉、清水混合;所述微胶囊壁材为环状糊精、阿拉伯胶、壳聚糖中的一种或几种;所述乳化剂为单硬脂酸甘油酯、蔗糖脂肪酸酯。9. a kind of eucommia ulmoides seed oil powder granule as claimed in claim 1, is characterized in that in described step (7), also comprises adding microcapsule wall material, emulsifier and eucommia ulmoides seed oil, seed dregs active powder, clear water mix ; The microcapsule wall material is one or more of cyclodextrin, gum arabic, and chitosan; the emulsifier is glycerol monostearate, sucrose fatty acid ester. 10.采用权利要求1~9任一所述方法制备的杜仲籽油粉末冲剂。10. The Eucommia ulmoides seed oil powder granule prepared by any one of claims 1-9.
CN201810282404.2A 2018-04-02 2018-04-02 A kind of eucommia ulmoides seed oil powder electuary and preparation method thereof Pending CN108703340A (en)

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