CN104905321A - Wall-breaking Haematoccoccus Pluvialis powder microcapsules and preparation process thereof - Google Patents
Wall-breaking Haematoccoccus Pluvialis powder microcapsules and preparation process thereof Download PDFInfo
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Abstract
本发明公开了一种破壁雨生红球藻粉微胶囊的制备工艺,包括:步骤一、对雨生红球藻粉进行破壁处理;步骤二、取糖和蛋白质溶于水中,水与糖和蛋白质的总量的比例为1∶0.2~0.4,之后调节糖和蛋白质的水溶液pH为6-9,再于温度95-135℃下反应0.5-6h,使糖和蛋白质发生美拉德反应;其中,糖为葡萄糖、乳糖或麦芽糖中的任意一种,蛋白质为酪蛋白或大豆分离蛋白;以及,步骤三、以步骤二中得到的美拉德反应产物作为壁材、步骤一中得到的破壁雨生红球藻粉作为芯材制备得到破壁雨生红球藻粉微胶囊。本发明还公开了一种破壁雨生红球藻粉微胶囊。该微胶囊虾青素含量高。具有良好的稳定性和水溶性,增加其在液体食品中的应用范围。
The invention discloses a process for preparing microcapsules of Haematococcus pluvialis powder, which comprises: step 1, breaking the wall of Haematococcus pluvialls powder; step 2, dissolving sugar and protein in water, and mixing the water with the The ratio of the total amount of sugar and protein is 1:0.2~0.4, then adjust the pH of the aqueous solution of sugar and protein to 6-9, and then react at a temperature of 95-135°C for 0.5-6h to cause Maillard reaction of sugar and protein ; wherein, the sugar is any one of glucose, lactose or maltose, and the protein is casein or soybean protein isolate; and, step 3, using the Maillard reaction product obtained in step 2 as the wall material, the Broken Haematococcus pluvialis powder was used as the core material to prepare microcapsules of broken Haematococcus pluvialls powder. The invention also discloses a broken wall Haematococcus pluvialis powder microcapsule. The microcapsules are high in astaxanthin. It has good stability and water solubility, increasing its application range in liquid food.
Description
技术领域technical field
本发明涉及微胶囊技术领域,具体涉及一种破壁雨生红球藻粉微胶囊的制备工艺,同时也涉及一种破壁雨生红球藻粉微胶囊。The invention relates to the technical field of microcapsules, in particular to a preparation process of broken-wall Haematococcus pluvialis powder microcapsules, and also to a broken-wall Haematococcus pluvialls powder microcapsule.
背景技术Background technique
雨生红球藻(Haematoccoccus pluvialis)是一种分布广泛的单细胞绿藻,在逆境条件下能形成厚壁孢子并大量积累多种具有生理功能的类胡萝卜素,主要包括虾青素、虾青素单酯、虾青素双酯、黄体素、β-胡萝卜素、海胆酮、角黄质等,其中80%为虾青素及其酯类。雨生红球藻是目前已知自然界中存在的虾青素含量最高的生物,可达1.5-4%干重。Haematoccoccus pluvialis is a widely distributed single-celled green algae, which can form thick-walled spores and accumulate a large number of carotenoids with physiological functions under adverse conditions, mainly including astaxanthin, astaxanthin, and astaxanthin. Astaxanthin monoester, astaxanthin diester, lutein, β-carotene, echinenone, canthaxanthin, etc., 80% of which are astaxanthin and its esters. Haematococcus pluvialis is currently known to exist in nature with the highest content of astaxanthin, up to 1.5-4% dry weight.
虾青素由于其末端环上的羰基和羟基使得它有最高的抗氧化活性,其抗氧化能力是β-胡萝卜素的10倍,原花青素的60倍,维生素E的550倍(MikiW.,Biological functions and activities of animal carotenoids.Pure Appl.Chem.,1991,Vol.63,No.1,pp.141-146)。另外,虾青素具有很强的抑制肿瘤生成、增强免疫功能、抵御紫外线伤害等多种生理功效(Pashkow FJ,Watumull DG,Campbell CL.Astaxanthin:a novel potential treatment for oxidative stress andinflammation in cardiovascular disease.Am J Cardiol.2008May22;101(10A):58D-68D.),因而广泛应用于食品、医药、化妆品、保健品、水产养殖等领域。在美国已经获得了FDA的批准,允许作为新的膳食成分进入保健品市场。超强的抗氧化能力和多种的生物活性,以及艳丽的红色赋予了虾青素广泛的应用前景和市场潜力,它已广泛应用于水产、家禽养殖业、食品、保健品、化妆品和医药业等领域。Astaxanthin has the highest antioxidant activity due to the carbonyl and hydroxyl groups on its terminal ring, and its antioxidant capacity is 10 times that of β-carotene, 60 times that of proanthocyanidins, and 550 times that of vitamin E (MikiW., Biological functions and activities of animal carotenoids. Pure Appl. Chem., 1991, Vol.63, No.1, pp.141-146). In addition, astaxanthin has a variety of physiological effects such as inhibiting tumor formation, enhancing immune function, and resisting ultraviolet rays (Pashkow FJ, Watumull DG, Campbell CL. Astaxanthin: a novel potential treatment for oxidative stress and inflammation in cardiovascular disease.Am J Cardiol.2008May22; 101 (10A): 58D-68D.), thus widely used in food, medicine, cosmetics, health products, aquaculture and other fields. In the United States, it has been approved by the FDA, allowing it to enter the health care product market as a new dietary ingredient. Super strong antioxidant capacity, various biological activities, and bright red color endow astaxanthin with broad application prospects and market potential. It has been widely used in aquatic products, poultry farming, food, health care products, cosmetics and pharmaceutical industries and other fields.
对于雨生红球藻的破壁、或雨生红球藻中的虾青素提取方法、或者虾青素油的微胶囊化包埋处理,目前都有文献单独报道,将虾青素油进行微胶囊化包埋需要进行虾青素的提取,过程复杂且产量及效果上均会有损失,不能完全发挥雨生红球藻的功效。目前没有雨生红球藻破壁后直接进行微胶囊化处理的报道。主要是由于存在以下问题:破壁雨生红球藻的细胞壁碎片增加了微胶囊化处理难度;常规的变性淀粉、阿拉伯胶等壁材包埋效果差,导致产品稳定性差,而直接对破壁雨生红球藻液喷雾又会造成虾青素油的氧化损失。For the breaking of the wall of Haematococcus pluvialis, or the extraction method of astaxanthin in Haematococcus pluvialls, or the microencapsulation and embedding treatment of astaxanthin oil, there are separate reports in the literature at present, and astaxanthin oil is microencapsulated Chemical embedding requires the extraction of astaxanthin, the process is complicated and the yield and effect will be lost, and the efficacy of Haematococcus pluvialis cannot be fully exerted. At present, there is no report of direct microencapsulation of Haematococcus pluvialis after breaking the wall. Mainly due to the following problems: the cell wall fragments of broken Haematococcus pluvialis increase the difficulty of microencapsulation; conventional modified starch, gum arabic and other wall materials have poor embedding effects, resulting in poor product stability, and directly for the broken wall The spraying of Haematococcus pluvialis liquid will cause the oxidation loss of astaxanthin oil.
发明内容Contents of the invention
本发明的一个目的是解决至少上述问题和/或缺陷,并提供至少后面将说明的优点。An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages as will be described hereinafter.
本发明还有一个目的是提供一种破壁雨生红球藻粉微胶囊的制备工艺,本发明通过将美拉德反应产物作为壁材,并结合使用喷雾方法,有效克服了破壁雨生红球藻的细胞壁碎片难以微胶囊化的问题,直接对破壁藻粉进行微胶囊化,将微胶囊化虾青素与藻粉干燥相结合,生产出含有藻粉的微胶囊化虾青素产品,减少了产品提取工艺,采用美拉德反应产物作为壁材避免了虾青素的含量降低,也避免了虾青素油的氧化损失。Another object of the present invention is to provide a preparation process of broken-walled Haematococcus pluvialis powder microcapsules. The present invention effectively overcomes the problem of broken-walled Pluvialls by using the Maillard reaction product as a wall material and using a spray method in combination with the spraying method. To solve the problem that the cell wall fragments of Haematococcus are difficult to microencapsulate, directly microencapsulate the broken algal powder, combine the microencapsulated astaxanthin with the drying of the algal powder, and produce the microencapsulated astaxanthin containing the algal powder product, the product extraction process is reduced, and the Maillard reaction product is used as the wall material to avoid the reduction of astaxanthin content and the oxidation loss of astaxanthin oil.
本发明的再一目的是提供一种破壁雨生红球藻粉微胶囊,本发明的破壁雨生红球藻粉微胶囊有效降低了微胶囊的表面虾青素含量,掩盖了虾青素油的腥味,具有良好的稳定性和水溶性,虾青素含量达到0.5-1%,产品质量高。Another object of the present invention is to provide a microcapsule of broken-walled Haematococcus pluvialls powder. The broken-walled Haematococcus pluvialls powder microcapsule of the present invention effectively reduces the surface astaxanthin content of the microcapsules and covers the astaxanthin The fishy smell of vegetable oil has good stability and water solubility, the content of astaxanthin reaches 0.5-1%, and the product quality is high.
为此,本发明提供的技术方案为:For this reason, the technical scheme provided by the invention is:
一种破壁雨生红球藻粉微胶囊的制备工艺,包括如下步骤:A preparation process of broken-wall Haematococcus pluvialis powder microcapsules, comprising the steps of:
步骤一、对待处理的雨生红球藻粉进行破壁处理;Step 1, the Haematococcus pluvialis powder to be treated is subjected to wall-breaking treatment;
步骤二、以重量比例1∶0.5~3取糖和蛋白质溶于水中,其中水与所述糖和蛋白质的总量的比例为1∶0.2~0.4,之后调节糖和蛋白质的水溶液至pH为6-9,再于温度95-135℃下反应0.5-6h,使糖和蛋白质发生美拉德反应;Step 2, dissolving sugar and protein in water at a weight ratio of 1: 0.5 to 3, wherein the ratio of water to the total amount of sugar and protein is 1: 0.2 to 0.4, and then adjusting the aqueous solution of sugar and protein to a pH of 6 -9, and then react at a temperature of 95-135°C for 0.5-6h to cause Maillard reaction of sugar and protein;
其中,所述糖为葡萄糖、乳糖、或麦芽糖中的任意一种,所述蛋白质为酪蛋白或大豆分离蛋白;以及,Wherein, the sugar is any one of glucose, lactose, or maltose, and the protein is casein or soybean protein isolate; and,
步骤三、以步骤二中得到的美拉德反应产物作为壁材、步骤一中得到的破壁雨生红球藻粉作为芯材制备得到破壁雨生红球藻粉微胶囊。Step 3, using the Maillard reaction product obtained in step 2 as the wall material and the broken-wall Haematococcus pluvialis powder obtained in step 1 as the core material to prepare microcapsules of broken-wall Haematococcus pluvialls powder.
优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤二中,发生所述美拉德反应的具体条件为:所述糖和蛋白质的重量比例为1∶1,调节糖和蛋白质的水溶液溶液至pH为8.5,然后于反应温度105℃下反应2.5h。Preferably, in the preparation process of the broken-walled Haematococcus pluvialis powder microcapsules, in the second step, the specific conditions for the Maillard reaction to occur are: the weight ratio of the sugar to the protein is 1 : 1, adjust the aqueous solution of sugar and protein to pH 8.5, and then react at a reaction temperature of 105°C for 2.5h.
优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤三中,利用喷雾干燥方法将所述芯材和壁材制备成破壁雨生红球藻粉微胶囊,其中,喷雾干燥时进风温度为150-200℃,出风温度为60-100℃。Preferably, in the preparation process of the broken-walled Haematococcus pluvialis powder microcapsules, in the third step, the core material and the wall material are prepared into broken-walled Haematococcus pluvialls powder by using a spray drying method The microcapsules, wherein the air inlet temperature is 150-200°C and the air outlet temperature is 60-100°C during spray drying.
优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤三中,利用喷雾干燥方法将所述芯材和壁材制备成破壁雨生红球藻粉微胶囊之前,还包括如下步骤:Preferably, in the preparation process of the broken-walled Haematococcus pluvialis powder microcapsules, in the third step, the core material and the wall material are prepared into broken-walled Haematococcus pluvialls powder by using a spray drying method Before the microcapsules, the following steps are also included:
(3.1)芯材壁材混匀:按重量比例为1∶2.5~4取步骤一中得到的芯材和步骤二中得到的壁材并混匀;以及,(3.1) Mixing of core material and wall material: take the core material obtained in step 1 and the wall material obtained in step 2 in a weight ratio of 1: 2.5-4 and mix them uniformly; and,
(3.2)均质:于高压均质压力30-50MP下,对步骤(3.1)中得到的芯材和壁材的混合溶液进行均质2~3次。(3.2) Homogenization: Under the high-pressure homogenization pressure of 30-50MP, the mixed solution of the core material and the wall material obtained in the step (3.1) is homogenized for 2-3 times.
优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤一中,采用以下方法中的任意一种方法对待处理的雨生红球藻粉进行破壁处理:Preferably, in the preparation process of the described broken-walled Haematococcus pluvialls powder microcapsules, in the step 1, any one of the following methods is adopted to carry out the wall-breaking treatment of the Haematococcus pluvialls powder to be treated :
(1)高压均质机机械破壁:于温度4℃,压力40-150MP下进行均质;(1) Mechanical wall breaking of high-pressure homogenizer: homogenize at a temperature of 4°C and a pressure of 40-150MP;
(2)球磨机机械破壁:于转速400-600rpm下处理1-2h;或,(2) Mechanical wall breaking of ball mill: treatment at 400-600rpm for 1-2h; or,
(3)首先采用酶法于温度30~60℃预处理下雨生红球藻粉1h,采用的酶为总量占所述雨生红球藻粉重量0.5~2‰的果胶酶、纤维素酶和蛋白酶,之后再加入HCl或柠檬酸进行加热处理30-60min,或者进行球磨处理60-120min。(3) First, pretreat Haematococcus pluvialis powder at a temperature of 30-60° C. by enzymatic method for 1 hour, and the enzymes used are pectinase and fiber whose total amount accounts for 0.5-2‰ of the weight of said Haematococcus pluvialls powder Sulfase and protease, then add HCl or citric acid for heat treatment for 30-60min, or ball mill for 60-120min.
较优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤一中,所述方法(3)中,所述HCl的体积百分比为1%~5%,所述柠檬酸的质量百分比为1%~5%。More preferably, in the preparation process of the broken-walled Haematococcus pluvialis powder microcapsules, in the step 1, in the method (3), the volume percentage of the HCl is 1% to 5%, The mass percentage of the citric acid is 1%-5%.
较优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤一中,进行破壁处理之前向雨生红球藻粉中添加占所述雨生红球藻粉重量0.1-2%的抗氧化剂,其中所述抗氧化剂选自VC、VE或BHT中的一种或几种。More preferably, in the preparation process of the described broken-walled Haematococcus pluvialls powder microcapsules, in the step 1, before performing the wall-breaking treatment, add the described hematococcus pluvialls to the Haematococcus pluvialls powder 0.1-2% of the weight of algae powder is an antioxidant, wherein the antioxidant is selected from one or more of VC, VE or BHT.
较优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述喷雾干燥时的进风温度为180℃,出风温度为80℃。More preferably, in the preparation process of the broken-walled Haematococcus pluvialis powder microcapsules, the air inlet temperature during the spray drying is 180°C, and the air outlet temperature is 80°C.
较优选的是,所述的破壁雨生红球藻粉微胶囊的制备工艺中,所述步骤(3.1)中,所述芯材和壁材的重量比例为1∶2.5;所述步骤(3.2)中,所述高压均质的压力为40MP下,均质的次数为2次。More preferably, in the preparation process of the described broken-walled Haematococcus pluvialis powder microcapsules, in the step (3.1), the weight ratio of the core material and the wall material is 1: 2.5; the step ( In 3.2), the pressure of the high-pressure homogenization is 40MP, and the number of homogenization is 2 times.
一种破壁雨生红球藻粉微胶囊,所述破壁雨生红球藻粉微胶囊由任一所述的方法制得。A broken-wall Haematococcus pluvialis powder microcapsule, which is prepared by any one of the methods described.
本发明至少包括以下有益效果:The present invention at least includes the following beneficial effects:
本发明利用美拉德反应物为主要壁材制备破壁雨生红球藻微胶囊,制得的破壁雨生红球藻微胶囊为红色粉末,按照本发明优化的喷雾干燥工艺,微胶囊包埋率和产化率均达到90%以上,虾青素含量达到0.5-1%,具有良好的稳定性和水溶性,增加其在液体食品中的应用范围。The present invention utilizes the Maillard reactant as the main wall material to prepare broken-wall Haematococcus pluvialls microcapsules, and the prepared broken-walled Haematococcus pluvialls microcapsules are red powder. According to the optimized spray drying process of the present invention, the microcapsules Both the embedding rate and yield rate reach over 90%, the astaxanthin content reaches 0.5-1%, has good stability and water solubility, and increases its application range in liquid food.
本发明在破壁工艺中添加了抗氧化剂,结合美拉德反应物抗氧化壁材使用,对虾青素起到了双层防护作用。In the present invention, an antioxidant is added in the wall-breaking process, and the anti-oxidation wall material of the Maillard reactant is used in conjunction with a double-layer protection effect on the astaxanthin.
采用本发明的壁材和优化的工艺参数,如混合、均质等,有效降低了微胶囊的表面虾青素含量,掩盖了虾青素油的腥味,提高产品质量。Adopting the wall material of the present invention and optimized process parameters, such as mixing and homogenization, can effectively reduce the astaxanthin content on the surface of the microcapsules, cover up the fishy smell of astaxanthin oil, and improve product quality.
本发明工艺简单,产品收率高,生产成本低。The invention has the advantages of simple process, high product yield and low production cost.
本发明的其它优点、目标和特征将部分通过下面的说明体现,部分还将通过对本发明的研究和实践而为本领域的技术人员所理解。Other advantages, objectives and features of the present invention will partly be embodied through the following descriptions, and partly will be understood by those skilled in the art through the study and practice of the present invention.
附图说明Description of drawings
图1为本发明其中一个实施例中电子显微镜观察到的未破壁雨生红球藻细胞的电镜图;Fig. 1 is the electron micrograph of the unbroken Haematococcus pluvialis cell observed by electron microscope in one of the embodiments of the present invention;
图2为本发明其中一个实施例中电子显微镜观察到的破壁后的雨生红球藻细胞的电镜图;Fig. 2 is the electron micrograph of the Haematococcus pluvialis cell after the wall breaking observed by the electron microscope in one of the embodiments of the present invention;
图3为本发明其中一个实施例中微胶囊化包埋的破壁雨生红球藻粉的电镜扫描图。Fig. 3 is a scanning electron micrograph of microencapsulated embedded Haematococcus pluvialis powder in one embodiment of the present invention.
具体实施方式Detailed ways
下面结合附图对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。The present invention will be further described in detail below in conjunction with the accompanying drawings, so that those skilled in the art can implement it with reference to the description.
应当理解,本文所使用的诸如“具有”、“包含”以及“包括”术语并不配出一个或多个其它元件或其组合的存在或添加。It should be understood that terms such as "having", "comprising" and "including" as used herein do not entail the presence or addition of one or more other elements or combinations thereof.
本发明提供一种破壁雨生红球藻粉微胶囊的制备工艺,包括如下步骤:The invention provides a preparation process of broken-wall Haematococcus pluvialis powder microcapsules, comprising the following steps:
步骤一、对待处理的雨生红球藻粉进行破壁处理;Step 1, the Haematococcus pluvialis powder to be treated is subjected to wall-breaking treatment;
步骤二、以重量比例1∶0.5~3取糖和蛋白质溶于水中,其中水与所述糖和蛋白质的总量的比例为1∶0.2~0.4,之后调节糖和蛋白质的水溶液至pH为6-9,再于温度95-135℃下反应0.5-6h,使糖和蛋白质发生美拉德反应;Step 2, dissolving sugar and protein in water at a weight ratio of 1: 0.5 to 3, wherein the ratio of water to the total amount of sugar and protein is 1: 0.2 to 0.4, and then adjusting the aqueous solution of sugar and protein to a pH of 6 -9, and then react at a temperature of 95-135°C for 0.5-6h to cause Maillard reaction of sugar and protein;
其中,所述糖为葡萄糖、乳糖、或麦芽糖中的任意一种,所述蛋白质为酪蛋白或大豆分离蛋白;以及,Wherein, the sugar is any one of glucose, lactose, or maltose, and the protein is casein or soybean protein isolate; and,
步骤三、以步骤二中得到的美拉德反应产物作为壁材、步骤一中得到的破壁雨生红球藻粉作为芯材制备得到破壁雨生红球藻粉微胶囊。Step 3, using the Maillard reaction product obtained in step 2 as the wall material and the broken-wall Haematococcus pluvialis powder obtained in step 1 as the core material to prepare microcapsules of broken-wall Haematococcus pluvialls powder.
美拉德反应产物(Maillard Reaction Product,MRPs)具有一定的抗氧化性能,其中某些物质的抗氧化强度可以和食品中常用的抗氧化剂相媲美;不同底物的反应可以形成不同特色的风味物质,赋予产品新的风味特色。同时,美拉德反应物作为壁材具有优良的乳化和成膜性能。微胶囊化可以有效地减少虾青素受光、氧、水的影响,减少氧化;防止贮存过程中芯材的挥发;保护和控制芯材的释放;改变芯材的颜色、形状、密度、分散性能等理化性质;降低或掩盖虾青素油剂中的特殊腥气味;提高与其它物料的混合性及其流动性等。因此用水溶性美拉德反应产物作为壁材对虾青素进行微胶囊化包埋,可有效地提高稳定性,扩大其应用范围。本发明制备的破壁雨生红球藻微胶囊为红色粉末。按照本发明的方法,该微胶囊具有良好的稳定性和水溶性,增加了其在液体食品中的应用范围。本发明工艺简单,产品收率高,生产成本低。Maillard reaction products (Maillard Reaction Products, MRPs) have certain antioxidant properties, and the antioxidant strength of some of them can be compared with the antioxidants commonly used in food; the reaction of different substrates can form different flavor substances , giving the product new flavor characteristics. At the same time, the Maillard reactant has excellent emulsifying and film-forming properties as a wall material. Microencapsulation can effectively reduce the influence of astaxanthin by light, oxygen, and water, and reduce oxidation; prevent volatilization of the core material during storage; protect and control the release of the core material; change the color, shape, density, and dispersion properties of the core material and other physical and chemical properties; reduce or cover up the special fishy smell in astaxanthin oil; improve the mixing and fluidity with other materials, etc. Therefore, the water-soluble Maillard reaction product is used as the wall material to microencapsulate astaxanthin, which can effectively improve the stability and expand its application range. The broken Haematococcus pluvialis microcapsules prepared by the invention are red powder. According to the method of the invention, the microcapsule has good stability and water solubility, which increases its application range in liquid food. The invention has the advantages of simple process, high product yield and low production cost.
作为优选,所述步骤二中,发生所述美拉德反应的具体条件为:所述糖和蛋白质的重量比例为1∶1,调节糖和蛋白质的水溶液溶液至pH为8.5,然后于反应温度105℃下反应2.5h。As a preference, in the step 2, the specific conditions for the Maillard reaction to occur are: the weight ratio of the sugar and protein is 1:1, the aqueous solution of sugar and protein is adjusted to pH 8.5, and then the reaction temperature Reaction at 105°C for 2.5h.
作为优选,所述步骤三中,利用喷雾干燥方法将所述芯材和壁材制备成破壁雨生红球藻粉微胶囊,其中,喷雾干燥时进风温度为150-200℃,出风温度为60-100℃。喷雾干燥法制备微胶囊主要由芯材和壁材形成的乳状液在干燥塔内雾化干燥。在喷雾过程中,虽然热空气的温度很高,但由于水从壁材中快速蒸发,从而保证了芯材温度低于100℃,因此特别适用于热敏性较强物料的干燥。本发明将美拉德反应产物作为壁材和喷雾干燥方法联用,使得依照本发明制备的微胶囊包埋率和产化率均达到90%以上,虾青素含量达到0.5-1%,取本发明制得的破壁雨生红球藻粉微胶囊1g置于10~20mL水中,搅拌2~5min,其能很快溶解均匀,得到破壁雨生红球藻粉微胶囊溶液。即该破壁雨生红球藻粉微胶囊具有良好的稳定性和水溶性,增加了其在液体食品中的应用范围。As a preference, in the third step, the core material and the wall material are prepared into microcapsules of Haematococcus pluvialis powder by spray drying, wherein the temperature of the air inlet during spray drying is 150-200°C, and the temperature of the air outlet is The temperature is 60-100°C. The preparation of microcapsules by spray drying method is mainly to spray and dry the emulsion formed by the core material and the wall material in the drying tower. During the spraying process, although the temperature of the hot air is high, the temperature of the core material is guaranteed to be lower than 100°C due to the rapid evaporation of water from the wall material, so it is especially suitable for drying materials with strong heat sensitivity. In the present invention, the Maillard reaction product is used as the wall material in combination with the spray drying method, so that the embedding rate and yield of the microcapsules prepared according to the present invention can reach more than 90%, and the content of astaxanthin can reach 0.5-1%. 1 g of the broken-wall Haematococcus pluvialis powder microcapsule prepared by the invention is placed in 10-20 mL of water, stirred for 2-5 minutes, and can be quickly dissolved uniformly to obtain a broken-wall Haematococcus pluvialls powder microcapsule solution. That is, the broken-wall Haematococcus pluvialis powder microcapsule has good stability and water solubility, which increases its application range in liquid food.
作为优选,所述喷雾干燥时的进风温度为180℃,出风温度为80℃。Preferably, the air inlet temperature during the spray drying is 180°C, and the outlet air temperature is 80°C.
作为优选,所述步骤三中,利用喷雾干燥方法将所述芯材和壁材制备成破壁雨生红球藻粉微胶囊之前,还包括如下步骤:As a preference, in the step three, before the core material and the wall material are prepared into broken-wall Haematococcus pluvialis powder microcapsules by spray drying method, the following steps are also included:
(3.1)芯材壁材混匀:按重量比例为1∶2.5~4取步骤一中得到的芯材和步骤二中得到的壁材,总固形物浓度为15-25%,充分混合搅拌5-30min,使之混匀;该总固形物包括混合好的蛋白、多糖及其反应物、和雨生红球藻等。以及,(3.2)均质:于高压均质压力30-50MP下,对步骤(3.1)中得到的芯材和壁材的混合溶液进行均质2~3次。之后再进入喷雾干燥步骤。经过以上步骤,能够有效降低微胶囊的表面虾青素含量,掩盖了虾青素油的腥味,提高产品质量。(3.1) Mixing of core material and wall material: take the core material obtained in step 1 and the wall material obtained in step 2 in a weight ratio of 1: 2.5 to 4, the total solids concentration is 15-25%, and fully mix and stir for 5 -30min, make it mix; the total solids include mixed protein, polysaccharide and its reactants, and Haematococcus pluvialis, etc. And, (3.2) homogenization: under the high-pressure homogenization pressure of 30-50MP, the mixed solution of the core material and the wall material obtained in the step (3.1) is homogenized for 2-3 times. Then enter the spray drying step. Through the above steps, the astaxanthin content on the surface of the microcapsules can be effectively reduced, the fishy smell of the astaxanthin oil is covered, and the product quality is improved.
作为优选,所述步骤(3.1)中,所述芯材和壁材的重量比例为1∶2.5,总固形物浓度20%,充分搅拌10min使之混匀;所述步骤(3.2)中,所述高压均质的压力为40MP下,均质的次数为2次。As a preference, in the step (3.1), the weight ratio of the core material and the wall material is 1:2.5, the total solids concentration is 20%, fully stirred for 10 minutes to make it evenly mixed; in the step (3.2), the The pressure of the high-pressure homogenization is 40MP, and the number of homogenization is 2 times.
作为优选,所述步骤一中,采用以下方法中的任意一种方法对待处理的雨生红球藻粉进行破壁处理:As preferably, in said step 1, any one of the following methods is adopted to carry out wall-breaking treatment of Haematococcus pluvialis powder to be treated:
(1)高压均质机机械破壁:于温度4℃,压力40-150MP下进行均质;(1) Mechanical wall breaking of high-pressure homogenizer: homogenize at a temperature of 4°C and a pressure of 40-150MP;
(2)球磨机机械破壁:于转速400-600rpm下处理1-2h;或,(2) Mechanical wall breaking of ball mill: treatment at 400-600rpm for 1-2h; or,
(3)首先采用酶法于温度30~60℃预处理下雨生红球藻粉1h,采用的酶为总量占所述雨生红球藻粉重量0.5~2‰的果胶酶、纤维素酶和蛋白酶,之后再加入HCl或柠檬酸进行加热处理30-60min,或者进行球磨处理60-120min。如图1、图2和图3所示,经以上的方法破壁后,雨生红球藻粉的破壁率能达到90%以上,一般来说,只要破壁率要达到80-100%即可用于制作微胶囊。破壁率的评价:采用浮游生物计数板显微镜下计数,(3) First, pretreat Haematococcus pluvialis powder at a temperature of 30-60° C. by enzymatic method for 1 hour, and the enzymes used are pectinase and fiber whose total amount accounts for 0.5-2‰ of the weight of said Haematococcus pluvialls powder Sulfase and protease, then add HCl or citric acid for heat treatment for 30-60min, or ball mill for 60-120min. As shown in Figure 1, Figure 2 and Figure 3, after the above method of breaking the wall, the breaking rate of Haematococcus pluvialis powder can reach more than 90%. Generally speaking, as long as the breaking rate reaches 80-100% It can be used to make microcapsules. Evaluation of wall breaking rate: counting under a plankton counting plate under a microscope,
作为优选,所述步骤一中,所述方法(3)中,所述HCl的体积百分比为1%~5%,所述柠檬酸的质量百分比为1%~5%。Preferably, in the step 1, in the method (3), the volume percentage of the HCl is 1%-5%, and the mass percentage of the citric acid is 1%-5%.
作为优选,所述步骤一中,进行破壁处理之前向雨生红球藻粉中添加占所述雨生红球藻粉重量0.1-2%的抗氧化剂,其中所述抗氧化剂选自VC、VE或BHT中的一种或几种。在破壁工艺中添加抗氧化剂,和美拉德反应物抗氧化壁材联合使用,对虾青素起到了双层防护作用。As a preference, in the step 1, before the wall breaking treatment, 0.1-2% of the weight of the Haematococcus pluvialis powder is added to the Haematococcus pluvialis powder, wherein the antioxidant is selected from VC, One or more of VE or BHT. Adding antioxidants in the wall-breaking process, combined with Maillard reactant antioxidant wall materials, has a double-layer protection effect on astaxanthin.
一种破壁雨生红球藻粉微胶囊,所述破壁雨生红球藻粉微胶囊由任一所述的方法制得。A broken-wall Haematococcus pluvialis powder microcapsule, which is prepared by any one of the methods described.
实施例1Example 1
破壁雨生红球藻粉微胶囊制备工艺:Preparation process of broken-wall Haematococcus pluvialis powder microcapsules:
配制8%雨生红球藻粉水溶液,添加藻粉干重0.1%的抗氧化剂如维生素C-钠,采用高压均质机机械破壁法,制得破壁率在90%以上的破壁藻粉溶液作为芯材;Prepare an 8% aqueous solution of Haematococcus pluvialis powder, add 0.1% of the dry weight of the algae powder as an antioxidant such as vitamin C-sodium, and use a high-pressure homogenizer to mechanically break the wall to obtain a wall-breaking algae with a breaking rate of more than 90%. powder solution as core material;
制备美拉德反应产物壁材,糖和蛋白质比例为1∶1,pH8.5,反应温度110℃,反应时间为2.5h;Prepare the wall material of the Maillard reaction product, the ratio of sugar and protein is 1:1, the pH is 8.5, the reaction temperature is 110°C, and the reaction time is 2.5h;
将芯材壁材混匀充分混合搅拌5-10min;高压均质,均质压力30-50MP,均质2次;最后进行喷雾干燥。Mix the core material and wall material thoroughly for 5-10 minutes; high pressure homogenization, homogenization pressure 30-50MP, homogenization 2 times; finally spray drying.
所述壁材与芯材混合前,过100目筛绢;所述芯材和壁材的质量配比为1∶3,总固形物浓度为20%;所述喷雾干燥进风温度为180℃,出风温度为80℃。Before the wall material is mixed with the core material, pass through a 100-mesh sieve; the mass ratio of the core material and the wall material is 1:3, and the total solids concentration is 20%; the air inlet temperature of the spray drying is 180°C , the outlet air temperature is 80°C.
实施例2Example 2
破壁雨生红球藻粉微胶囊制备工艺:Preparation process of broken-wall Haematococcus pluvialis powder microcapsules:
配制10%雨生红球藻粉水溶液,添加藻粉干重的抗氧化剂如维生素E,采用球磨机机械破壁法,制得破壁率在90%以上的破壁藻粉溶液;制备美拉德反应产物壁材,糖和蛋白质比例为1∶0.8,pH8.0,反应温度110℃,反应时间为3.5h;将芯材壁材混匀充分混合搅拌5-10min;高压均质,均质压力30-50MP,均质2次;最后进行喷雾干燥。Prepare a 10% aqueous solution of Haematococcus pluvialis powder, add an antioxidant such as vitamin E of the dry weight of the algal powder, and adopt a ball mill mechanical wall breaking method to obtain a broken wall algae powder solution with a wall breaking rate of more than 90%; prepare Maillard The wall material of the reaction product, the ratio of sugar and protein is 1:0.8, pH8.0, the reaction temperature is 110°C, and the reaction time is 3.5h; the core material and wall material are mixed and stirred thoroughly for 5-10min; high pressure homogenization, homogenization pressure 30-50MP, homogenize twice; finally spray dry.
所述壁材与芯材混合前,过100目筛绢;所述芯材和壁材的质量配比为1∶4,总固形物浓度为18%;所述喷雾干燥进风温度为180℃,出风温度为80℃。Before the wall material is mixed with the core material, pass through a 100-mesh sieve; the mass ratio of the core material and the wall material is 1:4, and the total solids concentration is 18%; the air inlet temperature of the spray drying is 180°C , the outlet air temperature is 80°C.
实施例3Example 3
破壁雨生红球藻粉微胶囊制备工艺,包括如下步骤:The preparation process of broken-wall Haematococcus pluvialis powder microcapsules comprises the following steps:
步骤一、将雨生红球藻粉溶于水形成水溶液,之后向其中添加占所述雨生红球藻粉重量0.1%的抗氧化剂VC和VE。之后利用高压均质机于温度4℃,压力40MP下进行均质,以机械破壁,得到破壁雨生红球藻粉作为芯材。Step 1: dissolving Haematococcus pluvialis powder in water to form an aqueous solution, and then adding 0.1% of the weight of the Haematococcus pluvialls powder to antioxidants VC and VE. Then use a high-pressure homogenizer to homogenize at a temperature of 4°C and a pressure of 40MP, and mechanically break the wall to obtain broken-wall Haematococcus pluvialis powder as a core material.
步骤二、以重量比例1∶0.5取糖和蛋白质溶于水中,其中水与所述糖和蛋白质的总量的比例为1∶0.2,之后调节糖和蛋白质的水溶液至pH为6,再于温度95℃下反应6h,使糖和蛋白质发生美拉德反应,并将反应产物作为壁材;Step 2, dissolve sugar and protein in water at a weight ratio of 1:0.5, wherein the ratio of water to the total amount of sugar and protein is 1:0.2, then adjust the aqueous solution of sugar and protein to a pH of 6, and then React at 95°C for 6 hours to cause Maillard reaction between sugar and protein, and use the reaction product as wall material;
其中,所述糖为葡萄糖,所述蛋白质为酪蛋白;以及,Wherein, the sugar is glucose, and the protein is casein; and,
步骤三、以步骤二中得到的美拉德反应产物作为壁材、步骤一中得到的破壁雨生红球藻粉作为芯材,按照如下步骤制备得到破壁雨生红球藻粉微胶囊:Step 3, using the Maillard reaction product obtained in step 2 as the wall material, and the broken-wall Haematococcus pluvialis powder obtained in step 1 as the core material, and prepare broken-wall Haematococcus pluvialls powder microcapsules according to the following steps :
(3.1)芯材壁材混匀:按重量比例为1∶3取步骤一中得到的芯材和步骤二中得到的壁材并混匀;以及,(3.1) Mixing of core material and wall material: take the core material obtained in step 1 and the wall material obtained in step 2 in a weight ratio of 1:3 and mix them; and,
(3.2)均质:于高压均质压力30MP下,对步骤(3.1)中得到的芯材和壁材的混合溶液进行均质3次。(3.2) Homogenization: Under the high-pressure homogenization pressure of 30 MP, the mixed solution of the core material and the wall material obtained in the step (3.1) was homogenized for 3 times.
(3.3)利用喷雾干燥方法将均质过的所述芯材和壁材的混合溶液制备成破壁雨生红球藻粉微胶囊,其中,喷雾干燥时进风温度为150℃,出风温度为60℃。(3.3) Prepare the mixed solution of the homogenized core material and wall material into broken-wall Haematococcus pluvialis powder microcapsules by spray drying method, wherein the air inlet temperature is 150°C during spray drying, and the air outlet temperature is 150°C. is 60°C.
实施例4Example 4
破壁雨生红球藻粉微胶囊制备工艺,包括如下步骤:The preparation process of broken-wall Haematococcus pluvialis powder microcapsules comprises the following steps:
步骤一、将雨生红球藻粉溶于水形成水溶液,之后向其中添加占所述雨生红球藻粉重量1%的抗氧化剂VC。之后首先采用酶法于温度30~60℃预处理下雨生红球藻粉1h,采用的酶为总量占所述雨生红球藻粉重量0.5~2‰的果胶酶、纤维素酶和蛋白酶,之后再加入HCl或柠檬酸进行加热处理30-60min,或者进行球磨处理60-120min。所述HCl的体积百分比为1%~5%,所述柠檬酸的质量百分比为1%~5%。以破壁,得到破壁雨生红球藻粉作为芯材。Step 1: dissolving Haematococcus pluvialis powder in water to form an aqueous solution, and then adding VC, an antioxidant accounting for 1% by weight of the Haematococcus pluvialls powder, thereinto. After that, firstly, the enzyme method is used to pretreat the Haematococcus pluvialis powder at a temperature of 30-60°C for 1 hour. and protease, and then add HCl or citric acid for heat treatment for 30-60min, or perform ball milling treatment for 60-120min. The volume percentage of the HCl is 1%-5%, and the mass percentage of the citric acid is 1%-5%. The broken wall is used to obtain the broken Haematococcus pluvialis powder as the core material.
步骤二、以重量比例1∶1取糖和蛋白质溶于水中,其中水与所述糖和蛋白质的总量的比例为1∶0.3,之后调节糖和蛋白质的水溶液至pH为8.5,再于温度105℃下反应2.5h,使糖和蛋白质发生美拉德反应,并将反应产物作为壁材;Step 2, dissolve sugar and protein in water at a weight ratio of 1:1, wherein the ratio of water to the total amount of sugar and protein is 1:0.3, then adjust the aqueous solution of sugar and protein to pH 8.5, and then React at 105°C for 2.5 hours to cause Maillard reaction between sugar and protein, and use the reaction product as wall material;
其中,所述糖为麦芽糖,所述蛋白质为酪蛋白;以及,Wherein, the sugar is maltose, and the protein is casein; and,
步骤三、以步骤二中得到的美拉德反应产物作为壁材、步骤一中得到的破壁雨生红球藻粉作为芯材,按照如下步骤制备得到破壁雨生红球藻粉微胶囊:Step 3, using the Maillard reaction product obtained in step 2 as the wall material, and the broken-wall Haematococcus pluvialis powder obtained in step 1 as the core material, and prepare broken-wall Haematococcus pluvialls powder microcapsules according to the following steps :
(3.1)芯材壁材混匀:按重量比例为1∶2.5取步骤一中得到的芯材和步骤二中得到的壁材并混匀;以及,(3.1) Mixing of core material and wall material: take the core material obtained in step 1 and the wall material obtained in step 2 in a weight ratio of 1:2.5 and mix them; and,
(3.2)均质:于高压均质压力40MP下,对步骤(3.1)中得到的芯材和壁材的混合溶液进行均质2次。(3.2) Homogenization: Under the high-pressure homogenization pressure of 40MP, the mixed solution of the core material and the wall material obtained in step (3.1) was homogenized twice.
(3.3)利用喷雾干燥方法将均质过的所述芯材和壁材的混合溶液制备成破壁雨生红球藻粉微胶囊,其中,喷雾干燥时进风温度为180℃,出风温度为80℃。(3.3) Prepare the mixed solution of the homogenized core material and wall material into broken-wall Haematococcus pluvialis powder microcapsules by spray drying method, wherein the air inlet temperature is 180°C during spray drying, and the air outlet temperature is 180°C. is 80°C.
实施例5Example 5
破壁雨生红球藻粉微胶囊制备工艺,包括如下步骤:The preparation process of broken-wall Haematococcus pluvialis powder microcapsules comprises the following steps:
步骤一、将雨生红球藻粉溶于水形成水溶液,之后向其中添加占所述雨生红球藻粉重量2%的抗氧化剂BHT,其中所述抗氧化剂选自VC、VE或BHT中的一种或几种。之后利用球磨机机械破壁:于转速400-600rpm下处理1-2h以机械破壁,得到破壁雨生红球藻粉作为芯材。Step 1, dissolving the Haematococcus pluvialis powder in water to form an aqueous solution, and then adding 2% of the weight of the Haematococcus pluvialls powder to the antioxidant BHT, wherein the antioxidant is selected from VC, VE or BHT one or more of. After that, use a ball mill to mechanically break the wall: process at a rotational speed of 400-600rpm for 1-2 hours to mechanically break the wall, and obtain the broken Haematococcus pluvialis powder as the core material.
步骤二、以重量比例1∶3取糖和蛋白质溶于水中,其中水与所述糖和蛋白质的总量的比例为1∶0.4,之后调节糖和蛋白质的水溶液至pH为9,再于温度135℃下反应0.5h,使糖和蛋白质发生美拉德反应,并将反应产物作为壁材;Step 2, dissolving sugar and protein in water with a weight ratio of 1: 3, wherein the ratio of water to the total amount of sugar and protein is 1: 0.4, then adjusting the aqueous solution of sugar and protein to pH to be 9, and then React at 135°C for 0.5h to cause Maillard reaction between sugar and protein, and use the reaction product as wall material;
其中,所述糖为乳糖,所述蛋白质为大豆分离蛋白;以及,Wherein, the sugar is lactose, and the protein is soybean protein isolate; and,
步骤三、以步骤二中得到的美拉德反应产物作为壁材、步骤一中得到的破壁雨生红球藻粉作为芯材,按照如下步骤制备得到破壁雨生红球藻粉微胶囊:Step 3, using the Maillard reaction product obtained in step 2 as the wall material, and the broken-wall Haematococcus pluvialis powder obtained in step 1 as the core material, and prepare broken-wall Haematococcus pluvialls powder microcapsules according to the following steps :
(3.1)芯材壁材混匀:按重量比例为1∶4取步骤一中得到的芯材和步骤二中得到的壁材并混匀;以及,(3.1) Mixing of core material and wall material: take the core material obtained in step 1 and the wall material obtained in step 2 in a weight ratio of 1:4 and mix them; and,
(3.2)均质:于高压均质压力50MP下,对步骤(3.1)中得到的芯材和壁材的混合溶液进行均质2次。(3.2) Homogenization: Under the high-pressure homogenization pressure of 50MP, the mixed solution of the core material and the wall material obtained in the step (3.1) was homogenized twice.
(3.3)利用喷雾干燥方法将均质过的所述芯材和壁材的混合溶液制备成破壁雨生红球藻粉微胶囊,其中,喷雾干燥时进风温度为200℃,出风温度为100℃。(3.3) Prepare the mixed solution of the homogenized core material and wall material into broken-wall Haematococcus pluvialis powder microcapsules by spray drying method, wherein the air inlet temperature is 200°C during spray drying, and the air outlet temperature is 200°C. is 100°C.
本发明通过将美拉德反应产物作为壁材,并结合使用喷雾方法,有效克服了破壁雨生红球藻的细胞壁碎片难以微胶囊化的问题,直接对破壁藻粉进行微胶囊化,将微胶囊化虾青素与藻粉干燥相结合,生产出含有藻粉的微胶囊化虾青素产品,减少了产品提取工艺,采用美拉德反应产物作为壁材避免了虾青素的含量降低,也避免了虾青素油的氧化损失。该工艺集合了微胶囊化的封闭作用和美拉德反应产物本身的抗氧化作用,具有较强的保护虾青素的效果。使得依照本发明制备的微胶囊包埋率和产化率均达到90%以上,虾青素含量达到0.5-1%,具有良好的稳定性和水溶性,增加了其在液体食品中的应用范围。The present invention effectively overcomes the problem that the cell wall fragments of broken Haematococcus pluvialis are difficult to microencapsulate by using the Maillard reaction product as the wall material in combination with the spraying method, and directly microencapsulates the broken wall algae powder, Combine microencapsulated astaxanthin with algal powder drying to produce microencapsulated astaxanthin products containing algal powder, which reduces the extraction process of the product, and uses Maillard reaction products as wall materials to avoid the content of astaxanthin Reduce and avoid the oxidation loss of astaxanthin oil. This process combines the sealing effect of microencapsulation and the antioxidant effect of the Maillard reaction product itself, and has a strong effect of protecting astaxanthin. The microcapsules prepared according to the present invention have an embedding rate and yield of more than 90%, an astaxanthin content of 0.5-1%, good stability and water solubility, and increase its application range in liquid food .
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节和这里示出与描述的图例。Although the embodiment of the present invention has been disclosed as above, it is not limited to the use listed in the specification and implementation, it can be applied to various fields suitable for the present invention, and it can be easily understood by those skilled in the art Therefore, the invention is not limited to the specific details and examples shown and described herein without departing from the general concept defined by the claims and their equivalents.
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