CN111248433A - 一种有良好稳定性的虾青素纳米乳液及其制备方法 - Google Patents
一种有良好稳定性的虾青素纳米乳液及其制备方法 Download PDFInfo
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- CN111248433A CN111248433A CN202010135638.1A CN202010135638A CN111248433A CN 111248433 A CN111248433 A CN 111248433A CN 202010135638 A CN202010135638 A CN 202010135638A CN 111248433 A CN111248433 A CN 111248433A
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- astaxanthin
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- nanoemulsion
- emulsion
- emulsifier
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
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- A—HUMAN NECESSITIES
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- A—HUMAN NECESSITIES
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Abstract
本发明公开一种有良好稳定性的虾青素纳米乳液,由以下组分按质量份数计:10‑15份虾青素;10‑30份包埋性壁材;8‑25份填充材料;0.1‑3份主乳化剂;0.01‑0.2份助乳化剂;45‑55份稀释介质;0‑5份抗氧化剂,0‑0.5份抑菌剂所生产的纳米级乳液产品,其通过经剪切均化等特殊工艺制备而成,具体以微囊化技术克服了脂溶性虾青素原料在应用中所固有的缺陷,解决了生物利用度低,水溶性差,工艺复杂,工业化困难,应用特性不明朗等问题;壁材及填充材料和乳化剂的组合使用,大大提高了虾青素乳液的稳定性。基于此,本发明所述虾青素乳液可作为一种原料,广泛应用各类饮料、奶制品和口服液等液体食品及功能食品。
Description
技术领域
本发明属于功能性添加剂制备技术领域,具体涉及一种有良好稳定性的纳米级虾青素乳液及制备方法。
背景技术
类胡萝卜素是一种天然活性成分,具有清除自由基,猝灭单线态氧,预防心血管疾病等生理功能。
虾青素是由4个异戊二烯双键首尾相连而成,共有11个共轭双键,分子式为C40H52O4,相对分子量为596.86,是一种酮式类胡萝卜素。虾青素具有脂溶性,不溶于水,具有极强的色素沉淀能力,作为一种功能性的色素,可被用作着色剂。同时虾青素具有很强的抗氧化功能及抗光敏作用,作为目前发现的天然来源的抗氧化能力最强的物质,更是在延缓衰老、增强抵抗力、防治老年痴呆和癌症方面有独特的作用。
但是由于虾青素的水溶性极差,其应用形态仅局限于胶囊、粉剂。另外由于虾青素自身的独特结构,因此其性质不稳定,易于异构化和降解很大程度上限制了虾青素的应用。
乳液是由油、水、表面活性剂等适当比例自发形成的透明或者半透明的稳定体系,可作为一种载体,广泛应用于食品、医药等领域。目前可以制备乳液的材料较多,如何选择合适的材料,制备出的乳液稳定性好且工艺简单是本领域技术人员需要攻克的难题。
专利CN 108634169 A中公开一种叶黄素纳米乳液的制备方法,用食品级酪蛋白酸钠作为乳化剂对叶黄素进行乳化,经过高速剪切和高压均质后得到叶黄素纳米乳液,但其制备工艺时间偏长,耗费大量工时及其能耗,不利于工业化生产。
专利CN108991522 A一种高负载姜黄素茶油O/W纳米乳液的制备方法,用乙醇作为载体制备得到姜黄素的纳米乳液,但是乙醇的使用会对给后续的脱除带来新的困难,并可能残留在产品中的。同样专利CN 106031705 B,201711419464.6也同样存在这样的问题。CN107874257 A除了用到有机溶剂外还需要从低到高连续4次不同压力的均质,工艺复杂。
专利CN107105694 A亚稳半透明香料纳米乳液和制备的方法,使用0.1-20%的乳化剂,用量太大易造成乳化剂中毒等问题,并通过不同级别的乳化剂和均质压力获得产品,工艺复杂。
鉴于以上各类乳液剂型的产品,制备工艺复杂,工业化困难,应用特性不明朗的缺点,需要一种新的虾青素乳液配方和制备方法,以解决上述问题。
发明内容
为了解决上述问题,本发明提供一种有良好稳定性的纳米虾青素乳液及其制备方法。本发明中所述的纳米虾青素乳液,是含有虾青素、包埋性材料、稀释剂及填充材料和乳化剂组合获得的纳米级乳液产品,其通过经剪切均化等特殊工艺制备而成。
本发明的目的之一,首先在于提供一类新的有良好稳定性的虾青素乳液,由以下组分按质量份数计:10-15份虾青素;10-30份包埋性壁材;8-25份填充材料;0.1-3份主乳化剂;0.01-0.2份助乳化剂;45-55份稀释介质;0-5份抗氧化剂,0-0.5份抑菌剂。
进一步优选的,所述的包埋性壁材为辛烯基琥珀酸单阿拉伯胶酯。优选的,所述的包埋性壁材用量为15-25份。
进一步优选的,所述的填充材料为麦芽糊精、低聚麦芽糖、低聚果糖、木糖醇、赤藓糖醇、固体玉米糖浆、葡萄糖浆、山梨糖醇、蔗糖中的一种或者几种混合物。其中尤为优选固体玉米糖浆。无特殊说明,本说明书中所述及其混合物,指前述各组分中任意2中或2中以上的组分,按照任意比例的混合物。进一步优选的,所述的填充材料用量为10-18份。
进一步优选的,所述的稀释介质为水。本发明中所述的虾青素纳米乳液,将稀释剂和包埋材料及填充材料混合后形成水相,作为连续相对分散相进行乳化包埋。所述的稀释剂的选择可以是甘油、丙二醇、水等具有流动性的液体,但是稀释剂在本发明中并非只作为产品稀释作用,其具有分散和溶解、调整体系粘度等作用。
进一步本发明中另一重要特征在于乳化剂的选则。乳化剂的种类和数量很多,从中选择合适的O/W型乳化剂并不是简单的尝试就能得到合适的效果。在本发明中主乳化剂选用蔗糖脂肪酸酯,其用量优选为0.5-2份,所述的助乳化剂为磷脂,其用量为0.01-0.2份。主乳化剂和助乳化剂的合并使用,对得到稳定、均一的纳米级体系具有关键性作用。本发明中所述的磷脂是丙酮不容物超过50%的浓缩磷脂,包括浓缩葵花磷脂和浓缩大豆磷脂。
进一步优选的,所述的抗氧化剂选自生育酚,脂肪酸抗坏血酸酯,丁基羟基甲苯,丁基羟基茴香醚,丙基没食子酸,叔丁基羟基喹啉,抗坏血酸及其钠盐或其混合物;优选的,所述抗氧化剂的用量为0.1-2份。
进一步优选的,所述的抑菌剂选自苯甲酸、山梨酸及其钠盐或钾盐中的一种或者几种混合物,优选的,用量为0.01-0.2份。
最优选的实施例中,所述的虾青素乳液的组分及质量份数分别为:虾青素15份,包埋性壁材15-25份,填充材料10-18份,主乳化剂5-20份,助乳化剂0.1-2份,水50-55份,抗氧化剂0.1-2份,抑菌剂0.01份。
本发明的另一个目的,旨在提供上述虾青素纳米乳液的制备方法,包括如下步骤:
a)水相的制备:在稀释性介质中,将包埋性壁材、填充物、抑菌剂、乳化剂溶解;
b)油相的制备:将虾青素及抗氧化剂常温搅拌混合;
c)将步骤a)的油相和步骤b)的水相搅拌混合;
d)40-120Mpa条件下均化,即得产品。
当应用于优选方式的纳米虾青素乳液时,其关键的操作步骤在于剪切预乳化和均化压力的选择,即所述方法中的步骤c)如下:将步骤a)的油相和步骤b)的水相搅拌混合后,混合物经过10000~12000转高速剪切1-3分钟,进行预乳化的步骤;优选在40-60Mpa条件下高压均化。
有益效果:
本发明的有良好稳定性的虾青素纳米乳液,其优选实施例所得产品的粒径在500nm左右;其ZETA电位为-47mV(绝对值大于30时认为体系稳定);产品在90-95度加热过程中,含量保留率97%以上;pH3-7范围内稳定;产品37℃加速3个月的含量保留率在99%以上,复水后有微量油花出现,级别为+。本发明以微囊化技术克服了脂溶性虾青素原料在应用中所固有的缺陷,解决了生物利用度低,水溶性差,工艺复杂,工业化困难,应用特性不明朗等问题;壁材及填充材料和乳化剂的组合使用,大大提高了虾青素乳液的稳定性。因此,其可作为一种原料,广泛应用于pH3-7范围内的各类饮料、奶制品和口服液等液体食品及功能食品。
具体实施方式
下述非限制性实施例将进一步阐明本发明,但不应当理解为对本发明任意形式的限定,如无特殊说明,本申请中采用下述方法对产品进行测量和评价。
本发明所述的粒径,采用安东帕纳米粒径仪,Litesize500测定中位粒径。
本发明所述的ZETA电位,采用安东帕纳米粒径仪,Litesize500测定。
本发明中所述的冲调稳定性评价方法为:称量0.5g产品溶解于100ml水中,并用“+”表示冲调完的漂油量,其漂油越多,“+”越多。
本发明所述的pH稳定性的测定方法为使用酸碱调节剂调节体系中的pH,加入乳液后,评价其漂浮沉淀情况,并用“+”表示漂浮沉淀量,其漂浮沉淀越多,“+”越多。
本发明所述产品加速稳定性评价方法为:37℃,室内湿度条件下,测定的不同时间的色素含量以确定其稳定性优劣。含量保留率为不同时间时产品含量和初始含量的比率,以百分比表示。
实施例1:稀释剂对乳液形成的影响
(1)将辛烯基琥珀酸单阿拉伯胶酯30g,葡萄糖浆25g与45g甘油混合搅拌均匀,加入虾青素10g,混合生育酚0.1g,搅拌,乳液粘度10000mcp.s,状态粘稠,不均匀,无法均化得到乳液。
(2)将辛烯基琥珀酸单阿拉伯胶酯30g,葡萄糖浆25g与45g水混合搅拌均匀,加入虾青素10g,混合生育酚0.1g,搅拌,乳液粘度2000mcp.s,状态均一,100Mpa均化后得到虾青素乳液,其粒径在3.5微米;其ZETA电位为-15mV(绝对值大于30时认为体系稳定),37℃放置3天出现分层现象。
(3)将辛烯基琥珀酸单阿拉伯胶酯30g,葡萄糖浆25g与45g丙二醇混合搅拌均匀,加入虾青素10g,混合生育酚0.1g,搅拌,乳液粘度2000mcp.s,状态均一,100Mpa均化后得到虾青素乳液,其粒径在6微米;其ZETA电位为-0.5mV(绝对值大于30时认为体系稳定),37℃放置3h出现分层现象。
(4)将辛烯基琥珀酸单阿拉伯胶酯30g,葡萄糖浆25g与60g水混合搅拌均匀,加入虾青素10g,混合生育酚0.1g,搅拌,乳液粘度1000mcp.s,状态均一,100Mpa均化后得到虾青素乳液,其粒径在2.7微米;其ZETA电位为-4mV(绝对值大于30时认为体系稳定),37℃放置12h出现分层现象。
综上可知,稀释剂的用量对乳液的均一稳定性起到至关重要的作用,合适的粘度体系,才能均化得到乳液,但是过多的水量虽然也能均化得到乳液,但是乳液的方式后很快分层。同时稀释剂的种类选择对形成的乳液效果也有重要影响。
实施例2:包埋性壁材和填充材料的筛选
(1)将辛烯基琥珀酸单阿拉伯胶酯100g,填充材料80g与450g水混合搅拌均匀,加入虾青素100g,混合生育酚1g,山梨酸钾2g,搅拌溶解,120Mpa均化后得到虾青素乳液,不同填充材料,得到的乳液指标见下表1:
表1.乳液指标
(2)将辛烯基琥珀酸淀粉钠(变性淀粉的一种)100g,固体玉米糖浆80g与450g水混合搅拌均匀,加入虾青素100g,混合生育酚5g,山梨酸钾0.5g,搅拌溶解,120Mpa均化后得到虾青素乳液,其粒径在9微米;其ZETA电位为22mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为50%;37℃加速30天,含量保留率为47.5%,乳液分层现象明显。
综上可知,辛烯基琥珀酸单阿拉伯胶酯和固体玉米糖浆的组合是具有较好的热稳定性,60min,90℃保温情况下,其含量保留率为95%。虽然在37℃加速过程中的保留率不是很理想,但是明显优于其他填充材料。
实施例3:乳化剂与助乳化剂的选择
(1)将辛烯基琥珀酸单阿拉伯胶酯250g,固体玉米糖浆100g,蔗糖脂肪酸酯5g和500g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠20g,山梨酸钾0.1g搅拌均匀,120Mpa均化后得到虾青素乳液,其粒径在2.1微米;其ZETA电位为-27mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为94%,37℃加速30天,含量保留率为92%,粒径1.7微米,有微量漂油,漂油量+。加速90天产品分层。
(2)将辛烯基琥珀酸单阿拉伯胶酯250g,固体玉米糖浆100g,蔗糖脂肪酸酯5g,葵花磷脂0.1g和500g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠20g,山梨酸钾0.1g,搅拌均匀,120Mpa均化后得到虾青素乳液,其粒径在1.0微米;其ZETA电位为-41mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为97.2%,37℃加速90天,含量保留率为94%,粒径为1.5微米,有微量漂油,漂油量+++。
(3)将辛烯基琥珀酸单阿拉伯胶酯250g,固体玉米糖浆100g,蔗糖脂肪酸酯5g,大豆磷脂0.1g和500g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠20g,山梨酸钾0.1g,搅拌均匀后经10000转剪切预乳化1min,在经超高压120Mpa均化后得到虾青素乳液,其粒径在600纳米;其ZETA电位为-45mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为98%,37℃加速90天,含量保留率为96.0%,粒径为1.0微米,有微量漂油,漂油量++。
(4)将辛烯基琥珀酸单阿拉伯胶酯250g,固体玉米糖浆100g,蔗糖脂肪酸酯5g,大豆磷脂0.1g和500g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠20g,山梨酸钾0.1g,搅拌均匀后经10000转剪切预乳化1min,在经高压50Mpa均化后得到虾青素乳液,其粒径在500纳米;其ZETA电位为-47mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为98%,37℃加速90天,含量保留率为99.5%,粒径为0.9微米,有微量漂油,漂油量+。
(5)将辛烯基琥珀酸单阿拉伯胶酯250g,固体玉米糖浆100g,磷脂0.1g和500g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠20g,山梨酸钾0.1g,搅拌均匀后经10000转剪切预乳化1min,50Mpa均化后得到虾青素乳液,其粒径在5微米;其ZETA电位为-10mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为70%,37℃加速30天,含量保留率为75%,产品明显分层。
(6)将辛烯基琥珀酸单阿拉伯胶酯250g,固体玉米糖浆100g,5g吐温80和500g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠20g,山梨酸钾0.1g,搅拌均匀后经10000转剪切预乳化1min,50Mpa均化后得到虾青素乳液,其粒径在7微米;其ZETA电位为-17mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为67%,37℃加速30天,含量保留率为55%,产品明显分层。
(7)将辛烯基琥珀酸单阿拉伯胶酯150g,固体玉米糖浆180g,蔗糖脂肪酸酯20g,大豆磷脂2g和550g水混合搅拌均匀,加入虾青素150g,抗坏血酸钠1g,苯甲酸钠0.1g,搅拌均匀后经12000转剪切预乳化3min,60Mpa均化后得到虾青素乳液,其粒径在520纳米;其ZETA电位为-47mV(绝对值大于30时认为体系稳定);90℃加热60min,含量保留率为97.5%,37℃加速90天,含量保留率为99.2%,粒径为0.95微米,有微量漂油,漂油量+。
综上所述,其他乳化剂的选择对产品粒径及稳定性均是不利的。而单独使用蔗糖脂肪酸酯和磷脂均不能达到要求,30天出现分层。蔗糖脂肪酸酯和磷脂的复配使用使得产品的稳定性有明显的提高,加速至90天仍能保持均一状态,含量保留率在97%以上。值得注意的是(2)、(3)、(4)三个对比例,分别加入了助乳化工艺和低压均化工艺,对产品的稳定性和粒径有提高效果。
实施例4:乳液应用效果
将实施例3(4)中的乳液10g,使用柠檬酸和柠檬酸钠调整体系pH,得到pH=3-7范围内的乳液,放置于37℃,加速3个月后,产品稳定性效果见下表2:
表2.产品稳定性效果
漂浮量用“+”表示,析出量越多“+”越多。
综上所述,表1的结果显示按照本发明所述的方法制备的虾青素纳米乳液,在pH3-7范围内仍具有良好的产品稳定性,能够应用于各类饮料产品中。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,本领域的技术人员在本发明披露的技术范围内,可轻易想到的变化或替换,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该以权利要求书的保护范围为准。
Claims (10)
1.一种有良好稳定性的虾青素纳米乳液,其特征在于,由以下组分按质量份数计:10-15份虾青素;10-30份包埋性壁材;8-25份填充材料;0.1-3份主乳化剂;0.01-0.2份助乳化剂;45-55份稀释介质;0-5份抗氧化剂,0-0.5份抑菌剂。
2.根据权利要求1所述的虾青素纳米乳液,其特征在于,所述的包埋性壁材为辛烯基琥珀酸单阿拉伯胶酯,优选的,所述的包埋性壁材用量为15-25份。
3.根据权利要求1所述的虾青素纳米乳液,其特征在于,所述的填充材料为麦芽糊精、低聚麦芽糖、低聚果糖、木糖醇、赤藓糖醇、固体玉米糖浆、葡萄糖浆、山梨糖醇、蔗糖中的一种或者几种混合物。
4.根据权利要求1-3中任一项所述的虾青素纳米乳液,其特征在于,所述的填充材料用量为10-18份。
5.权利要求1所述的虾青素纳米乳液,其特征在于,所述的稀释介质为水。
6.权利要求1所述的虾青素纳米乳液,其特征在于,所述的主乳化剂为蔗糖脂肪酸酯,其用量为0.5-2份,所述的助乳化剂为磷脂。
7.根据权利要求1所述的虾青素纳米乳液,其特征在于,所述的抗氧化剂选自生育酚,脂肪酸抗坏血酸酯,丁基羟基甲苯,丁基羟基茴香醚,丙基没食子酸,叔丁基羟基喹啉,抗坏血酸及其钠盐或其混合物;优选的,所述抗氧化剂的用量为0.1-2份。
8.根据权利要求1所述的虾青素纳米乳液,其特征在于,所述的抑菌剂选自苯甲酸、山梨酸及其钠盐或钾盐中的一种或者几种混合物,优选的用量为0.01-0.2份。
9.如权利要求1所述的虾青素纳米乳液的制备方法,包括以下述步骤:
a)水相的制备:在稀释性介质中,将包埋性壁材、填充物、抑菌剂、乳化剂溶解;
b)油相的制备:将虾青素及抗氧化剂常温搅拌混合;
c)将步骤a)的油相和步骤b)的水相搅拌混合;
d)40-120Mpa条件下均化,即得产品。
10.根据权利要求9所述的虾青素乳液的制备方法,其特征在于,所述步骤c)如下:将步骤a)的油相和步骤b)的水相搅拌混合后,混合物经过10000-12000转高速剪切1-3分钟,进行预乳化的步骤;优选在40-60Mpa条件下均化。
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