CN113208111A - 一种复合壁材的甜菜红素微胶囊的制备方法 - Google Patents

一种复合壁材的甜菜红素微胶囊的制备方法 Download PDF

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CN113208111A
CN113208111A CN202110616032.4A CN202110616032A CN113208111A CN 113208111 A CN113208111 A CN 113208111A CN 202110616032 A CN202110616032 A CN 202110616032A CN 113208111 A CN113208111 A CN 113208111A
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betacyanin
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polysaccharide
rice protein
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程大友
楚朝霞
代翠红
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Harbin Institute of Technology
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Abstract

一种复合壁材的甜菜红素微胶囊的制备方法，它涉及食品领域，本发明提供一种以“麦芽糊精‑大米蛋白‑菊芋多糖”为壁材的、能长期稳定存在且具有良好生物活性的“甜菜红素微胶囊”。本发明以麦芽糊精‑大米蛋白‑菊芋多糖为壁材原料，包覆甜菜红素。本发明所采用的一切原料均为对身体有益的食品级材料。芯材甜菜红素是安全性极高的天然色素和抗氧化剂；复合型壁材麦芽糊精‑大米蛋白‑菊芋多糖是对甜菜红素起最大稳定性的组合，其成本较低，能提升甜菜色素胶囊产品外观，且能为甜菜红素微胶囊提供附加营养价值。本发明应用于甜菜红素领域。

Description

一种复合壁材的甜菜红素微胶囊的制备方法
技术领域
本发明属于生物活性物质纳米胶囊化技术领域，具体涉一种复合壁材的甜菜红素微胶囊的制备方法。
背景技术
甜菜色素(Betalains)是一种以六碳结构为骨架的水溶性化合物，由含氮的色素核心结构-甜菜醛氨酸衍生而来。其90％以上的成分是红紫色的甜菜红素(betacyanin)。甜菜红素具有较强的自由基清除能力，极高的抗菌、抗炎、抗癌、抗氧化活性以及优良的紫红色着色功能。诸多优良特性使甜菜红素在医药、化妆品和食品工业中具有极高的应用价值和发展潜力。
然而，甜菜红素在加工储存过程中稳定性较差，容易受到光、热、空气、水和金属离子等理化因素的影响，这使其应用有限，目前仅作为食品添加剂存在于市场且市售甜菜色素粉土腥味严重。为了提高甜菜红素的稳定性增加其商业应用，可采用多种方法减缓其降解，其中最优的方法是将其微胶囊化(Encapsulation)。
麦芽糊精是由酸或酶水解淀粉形成的多糖，味道平淡易于干燥，其分子结构对甜菜红素具有色素稳定性。麦芽糊精包封效果优良且成本低但其乳化能力较差，其性质与其葡萄糖当量(DE)有关，DE越大，溶氧性、褐变反应越大，而组织性、黏度、色素稳定性和抗结晶性越差，包封甜菜红素时10-15DE的麦芽糊精效果最佳。菊芋多糖是植物中储备性多糖，种类丰富来源广泛，对血糖控制、体重控制和肠道健康起良好作用。果胶酶法(SEI法)提取的菊芋多糖中蔗果五糖、蔗果六糖及其以上聚合度菊芋多糖含量较高，抗氧化活性较强，包封甜菜红素时能与甜菜红素协同作用有效提升甜菜红素抗氧化活性和稳定性，但作为单一包封剂时有多糖的劣势。
蛋白质和多肽具有良好的溶解性、乳化性和成膜性，且能为人体提供必需氨基酸。其中，大米蛋白氨基酸配比合理，符合WHO/FAO推荐的理想模式，相较其他蛋白，大米蛋白是唯一可免于过敏试验的蛋白，且大米蛋白有一定抗糖抗癌作用，可与甜菜红素协同作用提升其生物活性。α-淀粉酶提取的大米蛋白(RPE法)乳化能力较强，且对人体肠道起良好促进作用。但大米蛋白做壁材时包封率较低。而麦芽糊精、菊芋多糖、大米蛋白联合使用包封活性物质，不仅能综合它们的的优点提高胶囊包封率和抗氧化性能，而且能为产物提供附加营养价值。然而以麦芽糊精(10-15DE)-大米蛋白(RPE)-菊芋多糖(果胶酶SEI法提取)的复合物为壁材包封甜菜红素的研究未见报道。
发明内容
本发明的首要目的是提供一种以“麦芽糊精(10-15DE)-大米蛋白(RPE)”为壁材的、能长期稳定存在且具有良好生物活性的“甜菜红素微胶囊”。
本发明的另一目的是提供这种具有控释功能和优良抗氧化性能的甜菜红素微胶囊的制备方法和技术。
本发明的一种复合壁材的甜菜红素微胶囊的制备方法，它是按照以下步骤进行的：
步骤一、称取多糖，以水为溶剂配制质量百分含量为10％～30％多糖溶液，振荡使麦芽糊精充分溶胀形成透明溶液，溶胀时间20min～180min，振荡频率为 120rpm～500rpm，温度为25～40℃；
其中，多糖为麦芽糊精、菊芋多糖中的一种或者两种按照等质量比混合而成；所述的麦芽糊精中葡萄糖当量为10～15DE；
步骤二、将大米蛋白加入多糖溶液，磁力搅拌均匀制得复合液，在复合液中加入占壁材总重0％～1％的胶类，得多糖-大米蛋白混合液；
其中，大米蛋白与多糖的质量比为(1～15)：(85～99)；所述的大米蛋白为酶法提取的大米蛋白，所述的磁力搅拌频率为2000～10000rpm，所述的磁力搅拌时间 2～10min；
步骤三、以甜菜红素溶液为芯材，麦芽糊精-大米蛋白混合液为壁材，将甜菜红素溶液倒入步骤二中的麦芽糊精-大米蛋白混合液，调节pH至5.5～6.5；搅拌混合液使反应生成微胶囊，搅拌频率为2000～10000rpm，反应时间为0.5～3h，反应温度为25～40℃；
其中，芯材中甜菜红素溶液中固体物质总重与壁材的质量比为1:3～15；微胶囊体系中固液比为1g:(5～15)mL；
步骤四、将步骤三反应后的反应液通过冷冻干燥法干燥，冷冻干燥真空度 2～100pa，制冷室温度为-40～-60℃，干燥时间为24～48h，之后把干燥产物磨成胶囊粉末，即得所述的复合壁材的甜菜红素微胶囊。
进一步地，所述的甜菜红素溶液为红甜菜水提液、甜菜汁或甜菜水提液干燥后的产物。
进一步地，向甜菜红素溶液中添加柠檬酸或抗坏血酸至甜菜红素溶液pH＝5.5～6.5。
进一步地，所述的酶法提取的大米蛋白是通过α-淀粉酶提取得到的，具体为以米粉为原料，用α-淀粉酶在80～100℃处理米粉2～4h，离心过滤除去杂质，即得大米蛋白。
进一步地，所述的菊芋多糖为果胶酶法提取的多糖，具体为破碎菊芋原料，加水，在30～50℃以果胶酶处理30～120min，过滤除去杂质，得菊芋多糖酶法提取物。
进一步地，所述的胶类为卡拉胶、果胶、瓜尔豆胶、阿拉伯胶中的一种或多种。
进一步地，步骤三中pH是通过食用酸调节的，所述的食用酸为柠檬酸、柠檬酸钠、抗坏血酸或其混合物。
进一步地，所述的大米蛋白与麦芽糊精的质量比为(5～10)：(85～99)。
进一步地，步骤三中所述的反应时间为0.5～3h，反应温度为25～40℃。
进一步地，所述的冷冻干燥真空度10～50pa，干燥时间为30～48h。
本发明初步纯化甜菜红素提取液，以10-15DE麦芽糊精和大米蛋白(RPE)的复合材料为包覆剂，采用冷冻干燥法制备甜菜红素微胶囊。以麦芽糊精-蛋白质联合使用包封活性物质，不仅能综合多糖和蛋白质的优点提高胶囊包封率和稳定性，而且能为产物提供附加营养价值。然而以麦芽糊精和蛋白质的复合物为壁材包封甜菜红素的研究未见报道。
本发明的有益效果：
(1)本发明所采用的一切原料均为对身体有益的食品级材料。芯材甜菜红素是安全性极高的天然色素和抗氧化剂；复合型壁材大米蛋白-麦芽糊精是对甜菜红素起最大稳定性的组合，其成本较低，能提升甜菜色素胶囊产品外观，且能为甜菜红素微胶囊提供附加营养价值。
(2)本发明采用的冷冻干燥法是最能保护甜菜红素颜色和抗氧化活性的干燥技术，10-15DE麦芽糊精-大米蛋白复合壁材适合冷冻干燥工艺，可防止冷冻过程中产品中粗大冰晶生成，减少甜菜红素微胶囊褐变反应，其与冷冻干燥工艺以及本发明中制备过程的结合能最大限度的保护红素色泽、稳定性和抗氧化活性。
(3)本发明所制甜菜红素微胶囊无市售甜菜粉的土腥味，颜色鲜艳，口感良好，具有良好的生物活性和稳定性。不仅可作为安全的添加剂增加食物，药品,化妆品的天然颜色和抗氧化性能，而且可应用于医药领域治疗和预防疾病。
(4)本发明操作方法简单，原料价廉易得，成本合适，需求广泛，市场化潜力大。
附图说明
图1为实施例1、2、3、4的微胶囊扫描电镜照片；其中，a、b：实施例1；c、 d：实施例2；e、f：实施例3；g、h：实施例4。
图2为实施例1、2、3的微胶囊实物图；其中a为实施例1壁材中大米蛋白占 1％的实物图，b为实施例2壁材中大米蛋白占5％的实物图，c为实施例3壁材中大米蛋白占10％的实物图；
图3为实施例1、2、3的加速储存稳定性曲线图；其中，A为实施例3的曲线， B为实施例2的曲线，C为实施例1的曲线；
具体实施方式
本领域的普通技术人员可以理解，上述各实施方式是实现本发明的具体实施例，而在实际应用中，可以在形式上和细节上对其作各种改变，而不偏离本发明的精神和范围。
为使本发明实施例的目的、技术方案和优点更加清楚明白，下面将详细叙述清楚说明本发明所揭示内容的精神，任何所属技术领域技术人员在了解本发明内容的实施例后，当可由本发明内容所教示的技术，加以改变及修饰，其并不脱离本发明内容的精神与范围。
本发明的示意性实施例及其说明用于解释本发明，但并不作为对本发明的限定。
实施例1：
本实施例的一种复合壁材的甜菜红素微胶囊的制备方法，是按照以下步骤进行的：
以大米蛋白(RPE):麦芽糊精-菊芋多糖＝1:99为壁材的微胶囊的制备
(1)利用大孔树脂纯化一批甜菜红素溶液，经冷冻干燥冻干，置于棕色瓶备用。
(2)称取20g麦芽糊精(10-15DE)，20g菊芋多糖(SEI法制备)于500ml 烧杯中，加入160ml蒸馏水，配制20％的多糖溶液，以保鲜膜封口，在室温条件下(28℃)，置溶液于200r/min的摇床上，溶胀2h。
(3)取10ml(约10.5g)20％“麦芽糊精-菊芋多糖”溶液于三角瓶中，其中含麦芽糊精1.05g，菊芋糖1.05g。在溶液中加入0.021g大米蛋白，以2000rpm磁力搅拌均匀，配制成多糖：大米蛋白＝1:99的复合溶液。
(4)取甜菜红素干粉0.212g于量杯，溶于5.4ml蒸馏水中，于磁力搅拌条件下，倒入步骤(3)所制溶液，再取6ml蒸馏水洗涤量杯两次，将洗涤液注入反应液，加入柠檬酸调节pH至5.5～6。控制胶囊溶液固液比为1:10，微胶囊壁芯比为1:10。
(5)胶囊溶液在室温条件下搅拌反应30min，后放入-20℃冰箱冷冻2h，然后放入冷冻干燥机，冷冻干燥48h，得到甜菜红素微胶囊，研磨成粉末，储存在棕色瓶中，置于冰箱中。
实施例2：
本实施例的一种复合壁材的甜菜红素微胶囊的制备方法，是按照以下步骤进行的：
以大米蛋白(RPE):麦芽糊精-菊芋多糖＝5:95为壁材的微胶囊的制备
(1)取10ml(约10.5g)实例1中所制麦芽糊精-菊芋多糖溶液于三角瓶中，其中含麦芽糊精1.05g，菊芋糖1.05g。在溶液中加入0.111g大米蛋白(RPE)，以2000rpm磁力搅拌均匀，配制多糖：大米蛋白＝5:95的复合溶液。
(2)取实例1中所制甜菜红素干粉0.221g于量杯，溶于6.3ml蒸馏水中，于磁力搅拌条件下，倒入多糖-大米蛋白溶液，再取8ml蒸馏水洗涤量杯两次，将洗涤液注入反应液，加入柠檬酸调节pH至5.5～6。控制胶囊溶液固液比为1:10，微胶囊壁芯比为1:10。
(3)胶囊溶液在室温条件下搅拌反应30min，后放入-20℃冰箱冷冻2h，然后放入冷冻干燥机，冷冻干燥48h，得到甜菜红素微胶囊，研磨成粉末，储存在棕色瓶中，置于冰箱中。
实施例3：
本实施例的一种复合壁材的甜菜红素微胶囊的制备方法，是按照以下步骤进行的：
以大米蛋白(RPE):麦芽糊精-菊芋多糖＝1:9为壁材的甜菜红素微胶囊的制备
(1)取10ml(约10.5g)实例1中所制20％多糖溶液于三角瓶中，其中含麦芽糊精1.05g，菊芋糖1.05g。将0.233g大米蛋白加入多糖溶液，以2000rpm磁力搅拌均匀，配制成大米蛋白:麦芽糊精-菊芋多糖＝1:9的复合溶液。
(2)取实例1中所制甜菜红素干粉0.233g于量杯，溶于5.7ml蒸馏水中，于磁力搅拌条件下，倒入多糖-大米蛋白溶液，再取10ml蒸馏水洗涤量杯两次，将洗涤液注入三角瓶，加入柠檬酸调节pH至5.5～6。控制胶囊溶液固液比为1:10，微胶囊壁芯比为1:10。
(3)胶囊溶液在室温条件下搅拌反应30min，后放入-20℃冰箱冷冻2h，然后放入冷冻干燥机，冷冻干燥48h，得到甜菜红素微胶囊，研磨成粉末，储存在棕色瓶中，置于冰箱中。
实施例4：
本实施例的一种复合壁材的甜菜红素微胶囊的制备方法，是按照以下步骤进行的：
以大米蛋白(RPE):麦芽糊精-菊芋多糖＝2:8为壁材的甜菜红素微胶囊的制备
(1)取10ml(约10.5g)实例1中所制20％多糖溶液于三角瓶中，其中含麦芽糊精1.05g，菊芋糖1.05g。将0.42g大米蛋白加入多糖溶液，以2000rpm磁力搅拌均匀，配制成大米蛋白:麦芽糊精-菊芋多糖＝2:8的复合溶液。
(2)取实例1中所制甜菜红素干粉0.252g于量杯，溶于7.7ml蒸馏水中，于磁力搅拌条件下，倒入多糖-大米蛋白溶液，再取20ml蒸馏水洗涤量杯两次，将洗涤液注入反应液，加入柠檬酸调节pH至5.5～6。控制胶囊溶液固液比为1:10，微胶囊壁芯比为1:10。
针对上述实施例进行如下性能测试：
测试1：甜菜红素微胶囊粉末微观形态
用扫描电镜观察微胶囊粉末形貌和尺寸，结果如图1。将胶囊粉末样品通过导电胶粘在铜片上，使用离子溅射仪对样品进行喷金处理，之后利用扫描电镜观察所制胶囊形态和粒径。
由图1可知，实施例1、实施例2、实施例3、实施例4均成功制备出纳米胶囊。由扫描电镜观察可知微胶囊粒径平均尺寸随壁材中蛋白质含量增加而逐渐增大，胶囊品质随蛋白质含量增多先上升后下降。临界点为蛋白质含量15％。由图可知，实施例1、2、3所制胶囊粒径均在5～20μm之间，所成胶囊形状接近圆球，实施例3胶囊表面凹陷较少。实施例4胶囊平均尺寸大于20μm，所成胶囊表面粗糙，质量较差。
因此得出结论，壁材中大米蛋白占比1～15％区间内，随着蛋白质含量的增加，包封率增大，完全成型的胶囊数量增多。这是由于蛋白质起乳化作用，增加了成膜性。但蛋白质含量超过15％，壁材对甜菜红素的包封率降低，胶囊质量急剧下降，因此壁材中蛋白质含量不宜过高。
测试2：甜菜红素微胶囊粉末外观观察
图2为实施例1、2、3所制胶囊，其胶囊质量较高。由于成分只有蛋白质上的少量差距，胶囊在肉眼观察中成色相近无明显差别(由于光线原因图片中有细微差别)。
测试3：甜菜红素微胶囊加速储存稳定性测试
甜菜红素是对热极敏感的色素，在65℃对甜菜红素进行加速储存稳定性测试。将微胶囊通过加速法储存在65℃环境下。监测甜菜红素降解情况28天，每7天分析一次甜菜红素含量，直至研究结束。结果如图3。
由图3可知，以“麦芽糊精(10-15DE)-大米蛋白(RPE)-菊芋多糖(果胶酶SEI 法提取)”为壁材的甜菜红素微胶囊热稳定性优良，在测试中，65℃高温环境下，实施例1(壁材中大米蛋白含量1％)、实施例2(壁材中大米蛋白含量5％)仅分解20％左右，而实施例3(壁材中大米蛋白含量10％)仅降解8.75％，展现了优良的储存稳定性。通过对比实施例1、2、3可知，随着壁材中蛋白质含量的增加甜菜红素微胶囊的储存稳定性增加，热稳定性增强，甜菜红素降解率减少。这是由于在有限范围内随着壁材中蛋白质含量增加，壁材溶液溶液乳化能力增强，更有利于成膜，有效的提高了微胶囊包封率。但由图1可知，蛋白质含量过高，包封效果变差，胶囊中色素稳定性会降低。

Claims (10)

1.一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于它是按照以下步骤进行的：
步骤一、称取多糖，以水为溶剂配制质量百分含量为10％～30％多糖溶液，振荡使麦芽糊精充分溶胀形成透明溶液，溶胀时间20min～180min，振荡频率为120rpm～500rpm，温度为25～40℃；
其中，多糖为麦芽糊精、菊芋多糖中的一种或者两种按照等质量比混合而成；所述的麦芽糊精中葡萄糖当量为10～15DE；
步骤二、将大米蛋白加入多糖溶液，磁力搅拌均匀制得复合液，在复合液中加入占壁材总重0％～1％的胶类，得多糖-大米蛋白混合液；
其中，大米蛋白与多糖的质量比为(1～15)：(85～99)；所述的大米蛋白为酶法提取的大米蛋白，所述的磁力搅拌频率为2000～10000rpm，所述的磁力搅拌时间2～10min；
步骤三、以甜菜红素溶液为芯材，麦芽糊精-大米蛋白混合液为壁材，将甜菜红素溶液倒入步骤二中的麦芽糊精-大米蛋白混合液，调节pH至5.5～6.5；搅拌混合液使反应生成微胶囊，搅拌频率为2000～10000rpm，反应时间为0.5～3h，反应温度为25～40℃；
其中，芯材中甜菜红素溶液中固体物质总重与壁材的质量比为1:(3～15)；微胶囊体系中固液比为1g:(5～15)mL；
步骤四、将步骤三反应后的反应液通过冷冻干燥法干燥，冷冻干燥真空度2～100pa，制冷室温度为-40～-60℃，干燥时间为24～48h，之后把干燥产物磨成胶囊粉末，即得所述的复合壁材的甜菜红素微胶囊。
2.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于所述的甜菜红素溶液为红甜菜水提液、甜菜汁或甜菜水提液干燥后的产物。
3.根据权利要求1或2所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于向甜菜红素溶液中添加柠檬酸或抗坏血酸至甜菜红素溶液pH＝5.5～6.5。
4.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于所述的酶法提取的大米蛋白是通过α-淀粉酶提取得到的，具体为以米粉为原料，用α-淀粉酶在80～100℃处理大米粉2～4h，离心过滤除去杂质，即得大米蛋白。
5.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于所述的菊芋多糖为果胶酶法提取的多糖，具体为破碎菊芋原料，加水，在30～50℃以果胶酶处理30～120min，过滤除去杂质，得菊芋多糖酶法提取物。
6.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于所述的胶类为卡拉胶、果胶、瓜尔豆胶、阿拉伯胶中的一种或多种。
7.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于步骤三中pH是通过食用酸调节的，所述的食用酸为柠檬酸、柠檬酸钠、抗坏血酸或其混合物。
8.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于所述的大米蛋白与麦芽糊精的质量比为(1～15)：(85～99)。
9.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于步骤三中所述的反应时间为0.5～3h，反应温度为25～40℃。
10.根据权利要求1所述的一种复合壁材的甜菜红素微胶囊的制备方法，其特征在于所述的冷冻干燥真空度10～50pa，干燥时间为24～48h。
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