CN113304697A - 一种南极磷虾油微粒及其制备方法 - Google Patents
一种南极磷虾油微粒及其制备方法 Download PDFInfo
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Abstract
本发明涉及磷虾油技术领域，具体涉及一种南极磷虾油微粒及其制备方法，南极磷虾油微粒按如下方法制得：(1)蛋白‑多糖复合溶液制备：将蛋白质与多糖混合得到混合粉末，将混合粉末溶于乙醇水溶液，于40‑85℃保温0.2‑6h后过滤得到蛋白质‑多糖复合溶液；(2)蛋白‑多糖‑南极磷虾油乳液制备：蛋白‑多糖复合溶液和南极磷虾油分别预热到40‑85℃，将预热好的南极磷虾油加入到蛋白‑多糖复合溶液中，乳化后得到蛋白‑多糖‑南极磷虾油乳液；(3)南极磷虾油微粒制备：将蛋白‑多糖‑南极磷虾油乳液加入到抗氧化剂水溶液中，将水相干燥后得到南极磷虾油微粒。由该方法制得的南极磷虾油微粒水分散性好、稳定性好、腥味较轻。
Description
技术领域
本发明涉及磷虾油制备技术领域，具体涉及一种南极磷虾油微粒及其制备方法。
背景技术
南极磷虾油生物储量巨大，各国纷纷将其列为重要的战略资源，属于极重要的三大待开发海洋资源之一。以南极磷虾为原料所开发的诸多产品中，属南极磷虾油最具有代表性。近年来，磷虾油因其独特的成分组成与功能特性备受关注。尤其是较高的多不饱和脂肪酸此处(DHA、EPA等)，虾青素/酯、磷脂、脂溶性维生素、甾醇类等多种功能伴随物，使其表现出多种临床功效，极具开发价值。但是南极磷虾油在开发和应用过程中存在突出挑战：(1)南极磷虾油为油状液体，水溶性差，剂型单一；(2)南极磷虾油中富含的多不饱和的脂肪酸和虾青素等物质，性质不稳定，极易受环境影响而发生氧化降解失活，同时氧化过程中产生浓重的异味，影响最终产品的商品价值。
因此，如何改善南极磷虾油的水分散性、稳定性和异味，已成为南极磷虾油应用推广过程中的关键技术问题。
发明内容
针对现有技术南极磷虾油的水分散性差、稳定性差和异味的问题，本发明提供一种南极磷虾油微粒及其制备方法，丰富了南极磷虾油的剂型，水分散性好、稳定性好、腥味较轻。
本发明提供一种南极磷虾油微粒的制备方法，所述制备方法包括如下步骤：
(1)蛋白-多糖复合溶液制备
将蛋白质与多糖按质量比为1-20:1混合得到混合粉末，将混合粉末按照质量体积比0.2-10g/mL溶于乙醇水溶液中，于40-85℃保温0.2-6h，保温结束后过滤除去不溶物，得到蛋白质-多糖复合溶液；
(2)蛋白-多糖-南极磷虾油乳液制备
将步骤(1)制得的蛋白-多糖复合溶液和南极磷虾油分别预热到40-85℃，然后将预热好的南极磷虾油加入到蛋白-多糖复合溶液中，乳化后得到蛋白-多糖-南极磷虾油乳液；所述南极磷虾油与蛋白-多糖复合溶液的体积比为1:1-20；
(3)南极磷虾油微粒制备
将步骤(2)制得的蛋白-多糖-南极磷虾油乳液，加入到抗氧化剂水溶液中，静置0.2-4h，除去水面浮油，将水相干燥后得到南极磷虾油微粒。
进一步地，步骤(1)所述蛋白质为大豆蛋白、酪蛋白、酪蛋白酸钠、乳清蛋白或溶菌酶中的一种或多种；所述多糖为藻酸丙二醇酯、透明质酸、半乳甘露聚糖、果胶、羧甲基纤维素、壳聚糖、海藻酸钠、***胶、葡聚糖中的一种或多种。
进一步地，步骤(1)乙醇水溶液的体积分数为50-80％。
进一步地，步骤(2)还包括南极磷虾油中添加油溶性抗氧化剂；更进一步地，步骤(2)还包括南极磷虾油中添加乳化剂和/或助乳化剂。
进一步地，步骤(3)加入时搅拌速度为400-2000r/min。
进一步地，步骤(3)抗氧化剂水溶液的质量体积分数为0.0001-5g/mL，抗氧化剂为抗坏血酸或其钠盐、乙二胺四乙酸或其钠盐或茶多酚中的一种或多种。
本发明还提供一种采用上述制备方法获得的南极磷虾油微粒。
本发明的有益效果在于，
(1)本发明提供一种南极磷虾油微粒的制备方法，条件温和、绿色环保、成本低，对南极磷虾油有很好的保护、分散作用，改变了南极磷虾油的凝聚状态，使其从液态转变为固态，有效拓宽了南极磷虾油的应用领域；
(2)通过本发明提供的制备方法所得的南极磷虾油微粒，粉末干爽，具有良好的流动性；南极磷虾油的包埋率可达90％以上，虾青素保留率可到97％以上，平均粒径分布无显著变化，表现出水分散性，显著改善了南极磷虾油的贮藏稳定性；改善了腥味；
(3)本发明制备的南极磷虾油在应用过程中，可以简单方便地按需要量添加到预混料食品、保健食品、日化用品和药品等体系当中，尤其是固体基质产品领域，市场前景广阔。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，对于本领域普通技术人员而言，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本发明提供的南极磷虾油微粒的制备方法流程图。
具体实施方式
为了使本技术领域的人员更好地理解本发明中的技术方案，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。
实施例1
如图1所示，一种南极磷虾油微粒，该微粒采用如下制备方法获得：
(1)蛋白-多糖复合溶液制备
将溶菌酶与藻酸丙二醇酯按质量比为10:1混合得到混合粉末，将混合粉末按照质量体积比2g/mL溶于75％乙醇水溶液中，于40℃保温6h，保温结束后过滤除去不溶物，得到蛋白质-多糖的复合溶液；
(2)蛋白-多糖-南极磷虾油乳液制备
将步骤(1)制得的蛋白-多糖复合溶液和南极磷虾油分别预热到60℃，然后将预热好的南极磷虾油边搅拌边加入到蛋白-多糖复合溶液中，乳化后得到蛋白-多糖-南极磷虾油乳液；所述南极磷虾油与蛋白-多糖复合溶液的体积比为1:1，搅拌速度为400r/min；
(3)南极磷虾油微粒制备
将步骤(2)制得的蛋白-多糖-南极磷虾油乳液，加入到质量体积分数为2g/mL的茶多酚抗氧化剂水溶液中，静置2h，除去水面浮油，将水相干燥后得到南极磷虾油微粒，蛋白-多糖-南极磷虾油乳液与抗氧化剂水溶液的体积比为1:1。
实施例2
一种南极磷虾油微粒，该微粒采用如下制备方法获得：
(1)蛋白-多糖复合溶液制备
将蛋白质(溶菌酶和大豆蛋白按质量比1:1混合)与多糖(透明质酸与***胶按质量比1:1混合)按质量比为20:1混合得到混合粉末，将混合粉末按照质量体积比10g/mL溶于80％乙醇水溶液中，于75℃保温0.5h，保温结束后过滤除去不溶物，得到蛋白质-多糖的复合溶液；
(2)蛋白-多糖-南极磷虾油乳液制备
将步骤(1)制得的蛋白-多糖复合溶液和南极磷虾油分别预热到85℃，然后将预热好的南极磷虾油边搅拌边加入到蛋白-多糖复合溶液中，乳化后得到蛋白-多糖-南极磷虾油乳液；所述南极磷虾油与蛋白-多糖复合溶液的体积比为1:10，搅拌速度为1000r/min；
(3)南极磷虾油微粒制备
将步骤(2)制得的蛋白-多糖-南极磷虾油乳液，加入到质量体积分数为5g/mL茶多酚抗氧化剂水溶液中，静置4h，除去水面浮油，将水相干燥后得到南极磷虾油微粒，蛋白-多糖-南极磷虾油乳液与抗氧化剂水溶液的体积比为10:1。
实施例3
一种南极磷虾油微粒，该微粒采用如下制备方法获得：
(1)蛋白-多糖复合溶液制备
将乳清蛋白与果胶按质量比为20:1混合得到混合粉末，将混合粉末按照质量体积比5g/mL溶于50％乙醇水溶液中，于45℃保温4h，保温结束后过滤除去不溶物，得到蛋白质-多糖的复合溶液；
(2)蛋白-多糖-南极磷虾油乳液制备
将步骤(1)制得的蛋白-多糖复合溶液和南极磷虾油分别预热到60℃，然后将预热好的南极磷虾油边搅拌边加入到蛋白-多糖复合溶液中，乳化后得到蛋白-多糖-南极磷虾油乳液；所述南极磷虾油与蛋白-多糖复合溶液的体积比为1:1，搅拌速度为450r/min；
(3)南极磷虾油微粒制备
将步骤(2)制得的蛋白-多糖-南极磷虾油乳液，加入到质量体积分数为0.05g/mL茶多酚抗氧化剂水溶液中，静置0.2h，除去水面浮油，将水相干燥后得到南极磷虾油微粒，蛋白-多糖-南极磷虾油乳液与抗氧化剂水溶液的体积比为20:1。
测试例1过氧化值稳定性测试
参照申请号为CN201611202858.1的中国专利申请所提供的的检测南极磷虾油的过氧化值的方法，具体为：
取定量南极磷虾油m溶解于有机溶剂中，再加入过量碘化钾溶液反应，之后向溶液中不断滴入浓度为C的硫代硫酸钠溶液并检测溶液的电位值，直至溶液的电位值稳定，在滴定过程中离散型地记录滴定体积V及此时溶液的电位值E；
采用二阶微商法绘制所述滴定体积V与所述电位值E之间的关系曲线，找出电位突跃点处的滴定体积Vx，并按照下述公式计算出过氧化值：
其中，V0为按照上述方法对空白样品测定出的所述电位突跃点处的滴定体积；
所述有机溶剂为乙醇：异烷烃＝1-3:2的体积比组成；
所述取定量南极磷虾油m溶解于有机溶剂直至南极磷虾油浓度为40-100mg/mL。
分别测试实施例南极磷虾油微粒初始样品和经20天贮藏后样品过氧化值升高率，过氧化值升高率计算公式如下：
测试结果见表1。
测试例2粒径测试
将实施例1南极磷虾油微粒初始样品和经20天贮藏后样品分别溶解到去离子水中，其比例为1：20，通过马尔文激光粒度仪进行检测。测试结果见表1。
测试例3贮藏稳定性测试
以贮藏过程中虾青素的保留率来评价其贮藏稳定性。
将实施例1样品封装于铝塑瓶中，于40℃恒温箱下放置贮藏，20天后取样，观察样品外观，并测定样品中虾青素的含量，按照如下公式计算贮藏过程中虾青素的保留率，以评价其稳定性。
虾青素的保留率(％)＝Cn/C0×100
其中，Cn为贮藏20天后样品中虾青素含量，C0为起始样品中虾青素含量。
测试结果见表1。
表1实施例1与对照组测试结果
由表1可知，南极磷虾油微粒在虾青素保留率、过氧化值和气味方面的稳定性均显著优于普通磷虾油，通过稀释后测得该发明制备的南极磷虾油微粒在水体系中的平均粒径分布约为24.2μm，贮藏20天后粒径分布无显著变化，且体系均匀，表现出水分散性；本发明制备的南极磷虾油微粒为流动性良好的粉状固体，加工应用性能优良。表明本发明制备的南极磷虾油微粒稳定性优良。
本发明制备的南极磷虾油微粒在应用过程中，可以简单方便的按需要量添加到预混料食品、保健食品、日化用品和药品等体系当中。
尽管通过参考附图并结合优选实施例的方式对本发明进行了详细描述，但本发明并不限于此。在不脱离本发明的精神和实质的前提下，本领域普通技术人员可以对本发明的实施例进行各种等效的修改或替换，而这些修改或替换都应在本发明的涵盖范围内/任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以权利要求所述的保护范围为准。
Claims (8)
1.一种南极磷虾油微粒的制备方法，其特征在于，所述制备方法包括如下步骤：
(1)蛋白-多糖复合溶液制备
将蛋白质与多糖按质量比为1-20:1混合得到混合粉末，将混合粉末按照质量体积比0.2-10g/mL溶于乙醇水溶液中，于40-85℃保温0.2-6h，保温结束后过滤除去不溶物，得到蛋白质-多糖复合溶液；
(2)蛋白-多糖-南极磷虾油乳液制备
将步骤(1)制得的蛋白-多糖复合溶液和南极磷虾油分别预热到40-85℃，然后将预热好的南极磷虾油加入到蛋白-多糖复合溶液中，乳化后得到蛋白-多糖-南极磷虾油乳液；所述南极磷虾油与蛋白-多糖复合溶液的体积比为1:1-20；
(3)南极磷虾油微粒制备
将步骤(2)制得的蛋白-多糖-南极磷虾油乳液，加入到抗氧化剂水溶液中，静置0.2-4h，除去水面浮油，将水相干燥后得到南极磷虾油微粒。
2.如权利要求1所述的制备方法，其特征在于，步骤(1)所述蛋白质为大豆蛋白、酪蛋白、酪蛋白酸钠、乳清蛋白或溶菌酶中的一种或多种。
3.如权利要求1所述的制备方法，其特征在于，步骤(1)所述多糖为藻酸丙二醇酯、透明质酸、半乳甘露聚糖、果胶、羧甲基纤维素、壳聚糖、海藻酸钠、***胶或葡聚糖中的一种或多种。
4.如权利要求1所述的制备方法，其特征在于，步骤(1)乙醇水溶液的体积分数为50-80％。
5.如权利要求1所述的制备方法，其特征在于，步骤(3)加入时搅拌速度为400-2000r/min。
6.如权利要求1所述的制备方法，其特征在于，步骤(3)抗氧化剂水溶液的质量体积分数为0.0001-5g/mL。
7.如权利要求6所述的制备方法，其特征在于，步骤(3)抗氧化剂为抗坏血酸或其钠盐、乙二胺四乙酸或其钠盐或茶多酚中的一种或多种。
8.一种如权利要求1-7任一项所述的制备方法获得的南极磷虾油微粒。
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| US20090061067A1 (en) * | 2007-08-29 | 2009-03-05 | Aker Biomarine Asa | Method for making krill meal |
| CN102860506A (zh) * | 2012-08-08 | 2013-01-09 | 辽宁省大连海洋渔业集团公司 | 磷虾油微囊粉及其制备方法 |
| CN104799278A (zh) * | 2015-03-31 | 2015-07-29 | 武汉天天好生物制品有限公司 | 一种增强降血脂作用的磷虾油微胶囊及其制备方法 |
| CN107232636A (zh) * | 2017-07-28 | 2017-10-10 | 美泰科技（青岛）股份有限公司 | 一种水溶性南极磷虾油微胶囊粉的制备方法 |
| CN107874257A (zh) * | 2017-11-09 | 2018-04-06 | 大连工业大学 | 高包埋率小粒径南极磷虾油纳米粒的制备方法 |
| CN112402404A (zh) * | 2020-12-17 | 2021-02-26 | 日照职业技术学院 | 一种虾青素酯纳米复合物颗粒的制备方法 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115025230A (zh) * | 2022-05-10 | 2022-09-09 | 仙乐健康科技股份有限公司 | 一种乳化剂组合物及其在乳液中的应用 |
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