CN116268401B - 一种原花青素微胶囊及其制备方法 - Google Patents
一种原花青素微胶囊及其制备方法 Download PDFInfo
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Abstract
本发明提出了一种原花青素微胶囊及其制备方法,属于微胶囊技术领域。从葡萄皮、葡萄籽中提取原花青素得到原花青素溶液,与聚乳酸‑聚己内酯溶液分别用注射泵推动作用下,两股流体碰撞混合,得到原花青素纳米级胶囊粉,然后将原花青素纳米级胶囊粉、维生素E加入食用油中,在明胶‑黄原胶溶液存在下,调节pH值制得原花青素微米级微胶囊粉,然后经过二级包埋,制得原花青素微胶囊。本发明提取原花青素,提高葡萄副产物的利用率,后续微胶囊包埋后得到的原花青素微胶囊含有丰富的原花青素成分,同时可以遮盖原花青素的苦涩酸味,提高其的储存稳定性和生物利用率。
Description
技术领域
本发明涉及微胶囊技术领域,具体涉及一种原花青素微胶囊及其制备方法。
背景技术
微胶囊技术又称为微胶囊包埋技术,或微胶囊造粒技术,是将固体、液体甚至是气体包裹在一个微小的、密闭的胶囊里,从而有效控制所包裹的核心材料释放以至于保护其不受外界条件的影响的工艺过程。通常把构成微胶囊外壳材料称为“壁材”或“包衣”,把包在微胶囊内部物质称为“囊心”或者“芯材”等。芯材可以是固体、液体或气体。我国很早就开始研究将这种技术应用于食品领域,将液体食品粉末化,将食品中的活性成分与环境隔离开来,保护对光、热、水分、氧气等敏感的成分,从而降低和掩盖不良气味等,并取得了较好的效果。目前,微胶囊技术已经在许多领域如食品、医药、化工、生物技术等方面广泛应用。
原花青素是一种有着特殊分子结构的生物类黄酮 ,是清除人体内自由基较为有效的天然抗氧化剂。一般为红棕色粉末,气微、味涩,溶于水和大多有机溶剂。通常存在于植物的果实、种子、花和皮中,在葡萄、山碴、花生、银杏、白桦树、松树等植物中的含量较丰富。其中,葡萄籽原花青素主要由儿茶素、儿茶素没食子酸酯,及其二聚、三聚、四聚等,最高平均聚合度达十八聚体组成。葡萄籽中提取的原花青素可分为低聚原花青素和高聚原花青素。原花青素具有突出的抗氧化活性,是目前所发现的最有效的脂质过氧化抑制剂和自由基清除剂,其抗氧化效果远高于VE和VC,而其中尤其以低聚原花青素抗氧化活性最高。目前,对低聚原花青素提取方法较为成熟,但制备低聚原花青素产品,使之有效成分含量稳定仍鲜有报道。 。
中国专利CN108997294B公开了一种高品质低聚原花青素及其制备方法,其通过将富含原花青素原料反复提取、浓缩、纯化,以提纯低聚原花青素,但仍未能够精准控制产出低聚原花青素产品质量的稳定性。
发明内容
本发明的目的在于提出一种原花青素微胶囊及其制备方法,采用葡萄皮、葡萄籽提取原花青素能够得到含量较多的原花青素成分,提高葡萄副产物的利用率,后续微胶囊包埋后得到的原花青素微胶囊含有丰富的原花青素成分,同时可以遮盖原花青素的苦涩酸味,提高其的储存稳定性和生物利用率。
本发明的技术方案是这样实现的:
本发明提供一种原花青素微胶囊的制备方法,从葡萄皮、葡萄籽中提取原花青素得到原花青素溶液,与聚乳酸-聚己内酯溶液分别用注射泵推动作用下,两股流体碰撞混合,得到原花青素纳米级胶囊粉,然后将原花青素纳米级胶囊粉、维生素E加入食用油中,在明胶-黄原胶溶液存在下,调节pH值制得原花青素微米级微胶囊粉,然后经过二级包埋,制得原花青素微胶囊。
作为本发明的进一步改进,包括以下步骤:
S1.原花青素的提取:将葡萄皮、葡萄籽洗净,混合捣碎,加水反复冻融,向得到浆液中加入含有低共熔溶剂的酸性乙醇水溶液,超声提取,抽滤,浓缩,得到提取液,大孔树脂纯化,得到原花青素溶液;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器的两个入口,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,用孔径为0.1μm的滤膜过滤,洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将步骤S2制得的原花青素纳米级胶囊粉、维生素E加入食用油中,得到纳米胶囊油悬浮液,将明胶-黄原胶溶液和纳米胶囊油悬浮液混合,均质,调节溶液pH值为第一pH值,搅拌反应,调节pH值为第二pH值,加入谷氨酰胺转氨酶,搅拌反应,离心,洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;
S4.包埋:将步骤S3制得的原花青素微小胶囊粉、海藻酸钠、羧甲基纤维素钠加入水中,均质,滴加金属离子溶液,离心,洗涤,冷冻干燥,制得原花青素小微胶囊;
S5.二次包埋:将壳聚糖溶于酸液中后,加入α-酮戊二酸,加热搅拌反应,加入硼氢化钠,继续搅拌反应,加入乙醇,过滤,洗涤,干燥,研细,得到羧基化壳聚糖,加入水中,加入步骤S4制得的原花青素微小胶囊粉混合,均质,滴加金属离子溶液,常温固化,过滤,洗涤,干燥,制得原花青素微胶囊。
作为本发明的进一步改进,步骤S1中所述低共熔溶剂包括氢键受体和氢键供体,所述氢键受体选自甜菜碱、氯化胆碱中的至少一种;所述氢键供体选自尿素、硫脲、苯乙酸、苹果酸、柠檬酸、丁二酸、乙二醇、甘油、丁二醇、木糖醇、氨基酸、葡萄糖、果糖、三氟乙酰胺中的至少一种,所述葡萄皮、葡萄籽的质量比为10-12:12-15;所述反复冻融的操作为先置于-25至-20℃下冰冻2-4h后,解冻后再次重复操作1-2次;所述浆液和含有低共熔溶剂的酸性乙醇水溶液的质量比为1:1-2;所述超声提取的功率为1200-1500W,时间为0.5-1h;所述大孔树脂为AB-8型大孔吸附树脂,洗脱剂为50-60wt%的乙醇溶液;所述原花青素溶液中原花青素含量为55-65wt%。
作为本发明的进一步改进,所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为4-7:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为2-3,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为40-55wt%,氢键受体的含量为10-15wt%。
作为本发明的进一步改进,步骤S2中所述聚乳酸-聚己内酯溶液中聚乳酸的含量为20-25wt%,聚己内酯的含量为17-22wt%,余量为水;所述入口的内径为0.5-1.5mm;所述出口的内径为1.5-2.5mm。
作为本发明的进一步改进,步骤S3中所述明胶-黄原胶溶液中明胶的浓度为25-35wt%,黄原胶的浓度为22-30wt%,余量为水;所述原花青素纳米级胶囊粉、维生素E和食用油的质量比为20-25:3-5:100;所述食用油选自花生油、菜籽油、芝麻油、亚麻籽油、葵花籽油、玉米油、大豆油、鱼油中的至少一种;所述明胶-黄原胶溶液、纳米胶囊油悬浮液、谷氨酰胺转氨酶的质量比为10:4-7:0.4-0.5;所述均质条件为12000-15000r/min,时间为3-5min,所述第一pH值为4.2-4.5,所述第二pH值为6.3-6.7。
作为本发明的进一步改进,步骤S4中所述原花青素微小胶囊粉、海藻酸钠、羧甲基纤维素钠的质量比10:4-7:5-10,所述均质条件为12000-15000r/min,时间为3-5min,所述金属离子溶液为浓度为4-7wt%的氯化钙、氯化铁、氯化铝、氯化镁溶液中的至少一种。
作为本发明的进一步改进,步骤S5中所述酸液为1-2wt%的乙酸溶液,所述壳聚糖、α-酮戊二酸、硼氢化钠的质量比为10:17-25:2-4;所述加热至温度为45-55℃,所述加热搅拌反应的时间为14-17h;所述继续搅拌反应的时间为2-4h;所述常温固化的时间为30-50min;所述羧基化壳聚糖、原花青素微小胶囊粉的质量比为10:5-7;所述均质条件为12000-15000r/min,时间为3-5min,所述金属离子溶液为浓度为4-7wt%的氯化钙、氯化铁、氯化铝、氯化镁溶液中的至少一种。
作为本发明的进一步改进,具体包括以下步骤:
S1.原花青素的提取:将10-12重量份葡萄皮、12-15重量份葡萄籽洗净,混合捣碎,加水反复冻融,向10重量份浆液中加入10-20重量份含有低共熔溶剂的酸性乙醇水溶液,1200-1500W超声提取0.5-1h,抽滤,浓缩,得到提取液,AB-8型大孔吸附树脂纯化,洗脱剂为50-60wt%的乙醇溶液,得到原花青素溶液,原花青素含量为55-65wt%;
所述反复冻融的操作为先置于-25至-20℃下冰冻2-4h后,解冻后再次重复操作1-2次;
所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为4-7:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为2-3,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为40-55wt%,氢键受体的含量为10-15wt%;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器的两个入口,入口内径为0.5-1.5mm,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,出口内径为1.5-2.5mm,用孔径为0.1μm的滤膜过滤,洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;
所述聚乳酸-聚己内酯溶液中聚乳酸的含量为20-25wt%,聚己内酯的含量为17-22wt%,余量为水;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将22-25重量份步骤S2制得的原花青素纳米级胶囊粉、3-5重量份维生素E加入100重量份食用油中,得到纳米胶囊油悬浮液,将100重量份明胶-黄原胶溶液和40-70重量份纳米胶囊油悬浮液混合,12000-15000r/min均质3-5min,调节溶液pH值为4.2-4.5,搅拌反应30-50min,调节pH值为6.3-6.7,加入4-5重量份谷氨酰胺转氨酶,搅拌反应20-40min,离心,洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;
所述明胶-黄原胶溶液中明胶的浓度为25-35wt%,黄原胶的浓度为22-30wt%,余量为水;
S4.包埋:将10重量份步骤S3制得的原花青素微小胶囊粉、4-7重量份海藻酸钠、5-10重量份羧甲基纤维素钠加入100重量份水中,12000-15000r/min均质3-5min,滴加10-20重量份4-7wt%的金属离子溶液,离心,洗涤,冷冻干燥,制得原花青素小微胶囊;
S5.二次包埋:将10重量份壳聚糖溶于100重量份1-2wt%的乙酸溶液中后,加入17-25重量份α-酮戊二酸,加热至45-55℃,搅拌反应14-17h,加入2-4重量份硼氢化钠,继续搅拌反应2-4h,加入乙醇至体系乙醇含量为70-80wt%,过滤,洗涤,干燥,研细,得到羧基化壳聚糖,将10重量份羧基化壳聚糖加入50重量份水中,加入5-7重量份步骤S4制得的原花青素微小胶囊粉混合,12000-15000r/min均质3-5min,滴加5-10重量份4-7wt%的金属离子溶液,常温固化30-50min,过滤,洗涤,干燥,制得原花青素微胶囊。
本发明进一步保护一种上述的制备方法制得的原花青素微胶囊。
本发明具有如下有益效果:
原花青素可以赋予食物丰富的口味和色泽,并且可以延长食物的保质期,也可以作为食品中天然的添加剂,增强食物的稳定性。原花青素能够抵抗紫外线、改善视力、提高关节、动脉和身体组织(如心脏)的灵活性,并通过加强毛细血管、动脉和静脉来改善血液循环。虽然原花青素具有优越的生理活性,但是仍然存在很多局限性,包括其具有苦涩酸味;对温度、pH值、结构等都会对其稳定性产生影响,且其生物利用度低,与可溶性和不溶性复合物的蛋白质的结合会导致各种不利的后果,导致吸收的损害和健康促进潜力的降低因此,直接将原花青素在食用进人体后会不稳定,很难吸收利用并且会很快的排泄到体外,导致原花青素在体内的生物利用度低,限制了其在食品领域的实际应用。
葡萄皮、葡萄籽中含有丰富的原花青素,同时,产量较大,成本低,均为葡萄的副产物,采用这两种原料提取原花青素能够得到含量较多的原花青素成分,提高葡萄的利用率,后续微胶囊包埋后得到的原花青素微胶囊含有丰富的原花青素成分,同时可以遮盖原花青素的苦涩酸味,提高其的储存稳定性,并进入人体后,在胃部不会释放,而在碱性的肠道中缓慢释放,一般而言,大部分蛋白质在胃酸作用下会降解、失活,从而使得原花青素在肠道环境内不会与可溶性和不溶性复合物的蛋白质的结合,提高了原花青素在体内的生物利用度,具有很好的抗氧化、抗衰老等活性,能够抵抗紫外线、改善视力、提高关节、动脉和身体组织(如心脏)的灵活性,并通过加强毛细血管、动脉和静脉来改善血液循环。
采用本发明方法提取原花青素,加入含有低共熔溶剂的酸性乙醇水溶液进行提取,其中,低共熔溶剂中,氢键受体为甜菜碱和氯化胆碱,氢键供体为柠檬酸,一方面可以作为氢键供体用于提取原花青素,另一方面可以调节溶液的pH值在2-3,原花青素在酸性条件下稳定存在,可以替代乙酸或盐酸添加,避免了乙酸或盐酸的刺鼻气味,采用本发明组合的低共熔溶剂对于原花青素提取的效率更高,与酸性乙醇协同作用下,能够高提取率的得到原花青素,本发明低共熔溶剂组合替代了传统柠檬酸-磷酸氢二钠缓冲液,避免了磷酸盐所造成的危害,且效果好于蒸馏水,使制备过程更加绿色、环保。同时,超声波辅助提取法因具有快速、简便、提取时间短,超声波辐射产生的空化效应会导致介质分子的周期性膨胀和压缩循环,加速涡流和内部扩散,增加溶质向溶剂的传质、溶胀和水合,在超声波的作用下气泡形成并破裂,产生温度和压力变化,破坏细胞壁,促进细胞内容物,包括原花青素等释放到基质中,从而对于原花青素的提取有进一步促进作用。
本发明采用多层包埋技术,第一层制备原花青素纳米级胶囊粉,平均粒径在几百纳米左右,粒径较小,该方法通过溶剂与非溶剂的快速混合,使溶解状态的聚合物溶解度下降,从溶液中析出,并将芯材包覆形成微胶囊,具有粒径易于调控、尺寸分布窄、制备时间短(毫秒级)、易于放大与连续化等特优点,聚乳酸和聚己内酯具有生物可降解性,对小分子有较高的渗透性,具有良好的生物相容性和无毒性,将少量的原花青素包埋,避免其他物质的掺杂而使得原花青素分解,减少与外界环境的接触,极大的提高了原花青素的稳定性。
第二层制备原花青素微米级微胶囊粉,将原花青素纳米级胶囊粉与抗氧化的维生素E分散于油相中,然后,在两种带有相反电荷的线性无规则聚合物材料作为壁材(明胶带正电,黄原胶带负电)的作用下,将芯材分散在壁材水溶液中,改变体系pH使带相反电荷的高分子材料间发生静电作用相互吸引、溶解度降低,产生相分离,胶体自溶液中凝聚出来,得到了原花青素微米级微胶囊粉,并将维生素E包埋在内,有助于进一步稳定原花青素,避免其被金属离子或氧化分解。
第三层包埋制备原花青素小微胶囊,将原花青素微米级微胶囊粉在海藻酸钠、羧甲基纤维素钠存在下,在金属离子交联作用下形成壳层,微胶囊包埋可最大限度地保存囊芯物质原有的性能和生物活性,防止营养物质的破坏与损失,同时也具有提高原花青素的稳定性,缓释功能等功效,这次包埋在原壁材的基础上进行加固,并改善微囊在冷冻干燥过程中囊壁产生的部分裂缝和孔洞,以提高微胶囊产品的贮藏稳定性,延长其货架期。
最后一层包埋制备原花青素微胶囊。壳聚糖分子链上带有大量的羟基和氨基,本发明经过α-酮戊二酸对壳聚糖进行改性后,壳聚糖分子链上带有大量的羧基,羧基与金属离子发生配位交联作用形成稳定的结构,将原花青素小微胶囊包裹在微胶囊内部,形成从而形成了缓释结构,送入人体后,羧基化的壳聚糖不易于在胃部被人体分解,从而能在进入肠道后溶胀而使得原花青素小微胶囊被降解释放出来,避免了原花青素在胃部与蛋白质形成不良复合物。
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,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。
图1为本发明原花青素微胶囊的结构示意图;
图2为本发明原花青素微胶囊的制备过程中用的密闭撞击射流混合器的结示意图;
图3为实施例1制得原花青素纳米级胶囊的TEM图;
图4为实施例1制得原花青素微米级微胶囊粉的SEM图;
图5为实施例1制得的原花青素微胶囊的SEM图。
具体实施方式
下面将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,都属于本发明保护的范围。
实施例1
本实施例提供一种原花青素微胶囊的制备方法,包括以下步骤:
S1.原花青素的提取:将10重量份葡萄皮、12重量份葡萄籽洗净,混合捣碎,加100重量份水反复冻融,向10重量份浆液中加入10重量份含有低共熔溶剂的酸性乙醇水溶液,1200W超声提取0.5h,抽滤,浓缩,得到提取液,AB-8型大孔吸附树脂纯化,洗脱剂为50wt%的乙醇溶液,得到原花青素溶液,原花青素含量为55wt%;
所述反复冻融的操作为先置于-25℃下冰冻2h后,解冻融解后再次重复操作1次;
所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为4:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为2,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为40wt%,氢键受体的含量为10wt%;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器(如图2)的两个入口,入口内径为0.5mm,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,出口内径为1.5mm,用孔径为0.1μm的滤膜过滤,清水洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;图3为制得的原花青素纳米级胶囊粉的TEM图,由图可知,该花青素纳米级胶囊粉的粒径在100-200nm之间。
所述聚乳酸-聚己内酯溶液中聚乳酸的含量为20wt%,聚己内酯的含量为17wt%,余量为水;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将22重量份步骤S2制得的原花青素纳米级胶囊粉、3重量份维生素E加入100重量份花生油中,得到纳米胶囊油悬浮液,将100重量份明胶-黄原胶溶液和40重量份纳米胶囊油悬浮液混合,12000r/min均质3min,调节溶液pH值为4.2,搅拌反应30min,调节pH值为6.3,加入4重量份谷氨酰胺转氨酶,搅拌反应20min,3000r/min离心15min,清水洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;图4为制得原花青素微米级微胶囊粉的SEM图,由图可知,该制得原花青素微米级微胶囊粉的粒径在20-50μm之间。
所述明胶-黄原胶溶液中明胶的浓度为25wt%,黄原胶的浓度为22wt%,余量为水;
S4.包埋:将10重量份步骤S3制得的原花青素微小胶囊粉、4重量份海藻酸钠、5重量份羧甲基纤维素钠加入100重量份水中,12000r/min均质3min,滴加10重量份4wt%的氯化铝溶液,3000r/min离心15min,清水洗涤,冷冻干燥,制得原花青素小微胶囊;
S5.二次包埋:将10重量份壳聚糖溶于100重量份1wt%的乙酸溶液中后,加入17重量份α-酮戊二酸,加热至45℃,搅拌反应14h,加入2重量份硼氢化钠,继续搅拌反应2h,加入乙醇至体系乙醇含量为70wt%,过滤,清水洗涤,70℃干燥2h,研细,得到羧基化壳聚糖,将10重量份羧基化壳聚糖加入50重量份水中,加入5重量份步骤S4制得的原花青素微小胶囊粉混合,12000r/min均质3min,滴加5重量份4wt%的氯化铝溶液,常温固化30min,过滤,清水洗涤,70℃干燥2h,制得原花青素微胶囊,其结构示意图如图1。图5为制得的原花青素微胶囊的SEM图,由图可知,该原花青素微胶囊粒径在200-300μm之间,且表面平整光滑。
实施例2
本实施例提供一种原花青素微胶囊的制备方法,包括以下步骤:
S1.原花青素的提取:将12重量份葡萄皮、15重量份葡萄籽洗净,混合捣碎,加100重量份水反复冻融,向10重量份浆液中加入20重量份含有低共熔溶剂的酸性乙醇水溶液,1500W超声提取1h,抽滤,浓缩,得到提取液,AB-8型大孔吸附树脂纯化,洗脱剂为60wt%的乙醇溶液,得到原花青素溶液,原花青素含量为65wt%;
所述反复冻融的操作为先置于-20℃下冰冻4h后,解冻融解后再次重复操作2次;
所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为7:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为3,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为55wt%,氢键受体的含量为15wt%;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器(如图2)的两个入口,入口内径为1.5mm,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,出口内径为2.5mm,用孔径为0.1μm的滤膜过滤,清水洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;
所述聚乳酸-聚己内酯溶液中聚乳酸的含量为25wt%,聚己内酯的含量为22wt%,余量为水;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将25重量份步骤S2制得的原花青素纳米级胶囊粉、5重量份维生素E加入100重量份大豆油中,得到纳米胶囊油悬浮液,将100重量份明胶-黄原胶溶液和70重量份纳米胶囊油悬浮液混合,15000r/min均质5min,调节溶液pH值为4.5,搅拌反应50min,调节pH值为6.7,加入5重量份谷氨酰胺转氨酶,搅拌反应40min,3000r/min离心15min,清水洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;
所述明胶-黄原胶溶液中明胶的浓度为35wt%,黄原胶的浓度为30wt%,余量为水;
S4.包埋:将10重量份步骤S3制得的原花青素微小胶囊粉、7重量份海藻酸钠、10重量份羧甲基纤维素钠加入100重量份水中,15000r/min均质5min,滴加20重量份7wt%的氯化铁溶液,3000r/min离心15min,清水洗涤,冷冻干燥,制得原花青素小微胶囊;
S5.二次包埋:将10重量份壳聚糖溶于100重量份2wt%的乙酸溶液中后,加入25重量份α-酮戊二酸,加热至55℃,搅拌反应17h,加入4重量份硼氢化钠,继续搅拌反应4h,加入乙醇至体系乙醇含量为80wt%,过滤,清水洗涤,70℃干燥2h,研细,得到羧基化壳聚糖,将10重量份羧基化壳聚糖加入50重量份水中,加入7重量份步骤S4制得的原花青素微小胶囊粉混合,15000r/min均质5min,滴加10重量份7wt%的氯化铁溶液,常温固化50min,过滤,清水洗涤,70℃干燥2h,制得原花青素微胶囊,其结构示意图如图1。
实施例3
本实施例提供一种原花青素微胶囊的制备方法,包括以下步骤:
S1.原花青素的提取:将11重量份葡萄皮、13.5重量份葡萄籽洗净,混合捣碎,加100重量份水反复冻融,向10重量份浆液中加入15重量份含有低共熔溶剂的酸性乙醇水溶液,1350W超声提取1h,抽滤,浓缩,得到提取液,AB-8型大孔吸附树脂纯化,洗脱剂为55wt%的乙醇溶液,得到原花青素溶液,原花青素含量为60wt%;
所述反复冻融的操作为先置于-22℃下冰冻3h后,解冻融解后再次重复操作2次;
所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为5:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为2.5,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为47wt%,氢键受体的含量为12wt%;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器(如图2)的两个入口,入口内径为1mm,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,出口内径为2mm,用孔径为0.1μm的滤膜过滤,清水洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;
所述聚乳酸-聚己内酯溶液中聚乳酸的含量为22wt%,聚己内酯的含量为20wt%,余量为水;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将23.5重量份步骤S2制得的原花青素纳米级胶囊粉、4重量份维生素E加入100重量份鱼油中,得到纳米胶囊油悬浮液,将100重量份明胶-黄原胶溶液和55重量份纳米胶囊油悬浮液混合,13500r/min均质4min,调节溶液pH值为4.35,搅拌反应40min,调节pH值为6.5,加入4.5重量份谷氨酰胺转氨酶,搅拌反应30min,3000r/min离心15min,清水洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;
所述明胶-黄原胶溶液中明胶的浓度为30wt%,黄原胶的浓度为27wt%,余量为水;
S4.包埋:将10重量份步骤S3制得的原花青素微小胶囊粉、5重量份海藻酸钠、7重量份羧甲基纤维素钠加入100重量份水中,13500r/min均质4min,滴加15重量份5wt%的氯化钙溶液,3000r/min离心15min,清水洗涤,冷冻干燥,制得原花青素小微胶囊;
S5.二次包埋:将10重量份壳聚糖溶于100重量份1.5wt%的乙酸溶液中后,加入21重量份α-酮戊二酸,加热至50℃,搅拌反应15h,加入3重量份硼氢化钠,继续搅拌反应3h,加入乙醇至体系乙醇含量为75wt%,过滤,清水洗涤,70℃干燥2h,研细,得到羧基化壳聚糖,将10重量份羧基化壳聚糖加入50重量份水中,加入6重量份步骤S4制得的原花青素微小胶囊粉混合,13500r/min均质4min,滴加7重量份5wt%的氯化钙溶液,常温固化40min,过滤,清水洗涤,70℃干燥2h,制得原花青素微胶囊,其结构示意图如图1。
实施例4
与实施例3相比,不同之处在于,所述氢键受体为单一的甜菜碱。
实施例5
与实施例3相比,不同之处在于,所述氢键受体为单一的氯化胆碱。
对比例1
与实施例3相比,不同之处在于,步骤S1中未添加葡萄皮。葡萄籽的添加量为24.5重量份。
对比例2
与实施例3相比,不同之处在于,步骤S1中未添加葡萄籽。葡萄皮的添加量为24.5重量份。
对比例3
与实施例3相比,不同之处在于,步骤S1中含有低共熔溶剂的酸性乙醇水溶液由酸性乙醇水溶液替代,所述酸性乙醇水溶液的pH值为2.5,用乙酸调节,乙醇浓度为47wt%。
对比例4
与实施例3相比,不同之处在于,步骤S1中未进行反复冻融。
对比例5
与实施例3相比,不同之处在于,步骤S1中超声提取由搅拌提取替代。
对比例6
与实施例3相比,不同之处在于,步骤S2中聚乳酸-聚己内酯溶液由聚乳酸溶液替代。所述聚乳酸溶液中聚乳酸的含量为42wt%,余量为水。
对比例7
与实施例3相比,不同之处在于,步骤S2中聚乳酸-聚己内酯溶液由聚己内酯溶液替代。所述聚己内酯溶液中聚己内酯的含量为42wt%,余量为水。
对比例8
与实施例3相比,不同之处在于,未进行步骤S2。
对比例9
与实施例3相比,不同之处在于,步骤S3中未添加维生素E。
对比例10
与实施例3相比,不同之处在于,未进行步骤S3。
对比例11
与实施例3相比,不同之处在于,未进行步骤S4。
对比例12
与实施例3相比,不同之处在于,未进行步骤S5。
测试例1
堆积密度的测定:将实施例1-5和对比例1-12制得的原花青素微胶囊样品装入有刻度的量筒内,并将量筒水平匀速晃动使产品自然沉降,测定样品体积。
休止角的测量:将实施例1-5和对比例1-12制得的原花青素微胶囊样品从漏斗上方缓慢加入,将其自然下落于漏斗之中,在圆板上堆积,测量粉堆积高度H和覆盖半径r,按下列公式计算样品的休止角,β=arctanH/r。
溶胀比的测定:将实施例1-5和对比例1-12制得的原花青素微胶囊样品置于30mL超纯水溶液中,30min后将水中的微胶囊过滤出来并吸干表面水分,测定其质量。
溶胀比=m/m0
式中:m为起始原花青素微胶囊质量;m0为溶胀后微胶囊的质量。
结果见表1。
表1
由上表可知,本发明实施例1-3制得的原花青素微胶囊堆积密度较小,简介反应了原花青素微胶囊的粒径较小,休止角在32.07-32.11°之间,流动性良好,30min后,吸水膨胀比大于1,说明该原花青素微胶囊在水中仍具有良好的吸水膨胀能力。
测试例2
模拟胃液:取0.2g氯化钠、0.7mL浓盐酸,定容至100mL,pH值调至1.2。取0.2g实施例1-5和对比例1-12制得的原花青素微胶囊分别加入到30mL模拟胃液中,再加入0.128g胃蛋白酶,37℃恒温摇床50r/min进行反应,反应进行到2h时取1mL溶液测定原花青素含量,同时补充1mL模拟胃液,最终用氢氧化钠调pH值至6.8,终止消化。
模拟肠消化是取经胃消化的溶液加入胆盐溶液(0.188g胆盐溶于4mL 5mmol/L的磷酸盐缓冲溶液)、1mL11%的氯化钙溶液、1mL胰酶溶液(0.145g胰蛋白酶溶于2.5mL 5mmol/L的磷酸盐缓冲溶液),用氢氧化钠溶液调节pH值=6.8,37℃恒温摇床50r/min进行反应,反应进行到3h时取1mL溶液测定原花青素含量,同时每次补充1mL溶液。
释放率(%)=W0/Wt×100%
式中,Wt为总花青素含量;W0为样品在体外模拟胃消化和体外模拟肠消化后消化液中花青素含量。
结果见表2。
表2
由上表可知,本发明实施例1-3制得的原花青素微胶囊通过包埋技术建立原花青素释放的屏障,保护其不受模拟胃液的影响,使其以更高的数量到达模拟肠液,说明原花青素微胶囊对原花青素在胃肠中的消化具有一定缓释作用。
测试例3 稳定性
1、pH值稳定性
分别将30mg实施例1-5和对比例1-12制得的原花青素微胶囊与20mL pH值为2、10的磷酸盐缓冲溶液混合30min,过滤,取滤液以5000r/min离心10min。收集上清液,测定原花青素含量,以原花青素作对照。计算原花青素保留率。
2、温度稳定性
分别将30mg实施例1-5和对比例1-12制得的原花青素微胶囊与20mL pH值为7的磷酸盐缓冲溶液混合,分别在70℃、90℃搅拌混合30min,取滤液以5000r/min离心10min。收集上清液,测定原花青素含量,以原花青素作对照。计算原花青素保留率。
结果见表3。
表3
由上表可知,本发明实施例1-3制得的原花青素微胶囊具有较好的pH和温度稳定性。
测试例4 抗氧化试验
配制硫酸亚铁溶液(9.0 mmol/L)、乙醇-水杨酸溶液(9.0 mmol/L)和过氧化氢溶液(8.8 mmol/L)。采用水杨酸法(参考文献:蒋方程,李傲然,何静仁,等.不同品种山药的营养成分分析及其水提物的体外抗氧化能力研究[J].食品工业科技,2018,39(4):6-11)测定1mg/mL实施例1-5和对比例1-12制得的原花青素微胶囊对羟基自由基的清除效果,以1mg/mL的维生素C为对照组。
表4
由上表可知,本发明实施例1-3制得的原花青素微胶囊具有良好的抗氧化活性。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种原花青素微胶囊的制备方法,其特征在于,包括以下步骤:
S1.原花青素的提取:将葡萄皮、葡萄籽洗净,混合捣碎,加水反复冻融,向得到浆液中加入含有低共熔溶剂的酸性乙醇水溶液,超声提取,抽滤,浓缩,得到提取液,大孔树脂纯化,得到原花青素溶液;所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为4-7:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为2-3,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为40-55wt%,氢键受体的含量为10-15wt%;所述葡萄皮、葡萄籽的质量比为10-12:12-15;所述浆液和含有低共熔溶剂的酸性乙醇水溶液的质量比为1:1-2;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器的两个入口,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,用孔径为0.1μm的滤膜过滤,洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将步骤S2制得的原花青素纳米级胶囊粉、维生素E加入食用油中,得到纳米胶囊油悬浮液,将明胶-黄原胶溶液和纳米胶囊油悬浮液混合,均质,调节溶液pH值为第一pH值,搅拌反应,调节pH值为第二pH值,加入谷氨酰胺转氨酶,搅拌反应,离心,洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;所述原花青素纳米级胶囊粉、维生素E和食用油的质量比为20-25:3-5:100;所述明胶-黄原胶溶液、纳米胶囊油悬浮液、谷氨酰胺转氨酶的质量比为10:4-7:0.4-0.5;
S4.包埋:将步骤S3制得的原花青素微米级微胶囊粉、海藻酸钠、羧甲基纤维素钠加入水中,均质,滴加金属离子溶液,离心,洗涤,冷冻干燥,制得原花青素微小胶囊粉;所述原花青素微小胶囊粉、海藻酸钠、羧甲基纤维素钠的质量比10:4-7:5-10;
S5.二次包埋:将壳聚糖溶于酸液中后,加入α-酮戊二酸,加热搅拌反应,加入硼氢化钠,继续搅拌反应,加入乙醇,过滤,洗涤,干燥,研细,得到羧基化壳聚糖,加入水中,加入步骤S4制得的原花青素微小胶囊粉混合,均质,滴加金属离子溶液,常温固化,过滤,洗涤,干燥,制得原花青素微胶囊;所述壳聚糖、α-酮戊二酸、硼氢化钠的质量比为10:17-25:2-4;所述羧基化壳聚糖、原花青素微小胶囊粉的质量比为10:5-7。
2.根据权利要求1所述的制备方法,其特征在于,步骤S1中所述反复冻融的操作为先置于-25至-20℃下冰冻2-4h后,解冻后再次重复操作1-2次;所述超声提取的功率为1200-1500W,时间为0.5-1h;所述大孔树脂为AB-8型大孔吸附树脂,洗脱剂为50-60wt%的乙醇溶液;所述原花青素溶液中原花青素含量为55-65wt%。
3.根据权利要求1所述的制备方法,其特征在于,步骤S2中所述聚乳酸-聚己内酯溶液中聚乳酸的含量为20-25wt%,聚己内酯的含量为17-22wt%,余量为水;所述入口的内径为0.5-1.5mm;所述出口的内径为1.5-2.5mm。
4.根据权利要求1所述的制备方法,其特征在于,步骤S3中所述明胶-黄原胶溶液中明胶的浓度为25-35wt%,黄原胶的浓度为22-30wt%,余量为水;所述食用油选自花生油、菜籽油、芝麻油、亚麻籽油、葵花籽油、玉米油、大豆油、鱼油中的至少一种;所述均质条件为12000-15000r/min,时间为3-5min,所述第一pH值为4.2-4.5,所述第二pH值为6.3-6.7。
5.根据权利要求1所述的制备方法,其特征在于,步骤S4中所述均质条件为12000-15000r/min,时间为3-5min,所述金属离子溶液为浓度为4-7wt%的氯化钙、氯化铁、氯化铝、氯化镁溶液中的至少一种。
6.根据权利要求1所述的制备方法,其特征在于,步骤S5中所述酸液为1-2wt%的乙酸溶液,所述加热至温度为45-55℃,所述加热搅拌反应的时间为14-17h;所述继续搅拌反应的时间为2-4h;所述常温固化的时间为30-50min;所述均质条件为12000-15000r/min,时间为3-5min,所述金属离子溶液为浓度为4-7wt%的氯化钙、氯化铁、氯化铝、氯化镁溶液中的至少一种。
7.根据权利要求1所述的制备方法,其特征在于,具体包括以下步骤:
S1.原花青素的提取:将10-12重量份葡萄皮、12-15重量份葡萄籽洗净,混合捣碎,加水反复冻融,向10重量份浆液中加入10-20重量份含有低共熔溶剂的酸性乙醇水溶液,1200-1500W超声提取0.5-1h,抽滤,浓缩,得到提取液,AB-8型大孔吸附树脂纯化,洗脱剂为50-60wt%的乙醇溶液,得到原花青素溶液,原花青素含量为55-65wt%;
所述反复冻融的操作为先置于-25至-20℃下冰冻2-4h后,解冻后再次重复操作1-2次;
所述低共熔溶剂为氢键受体和柠檬酸的混合物,其中,氢键受体包括甜菜碱、氯化胆碱,质量比为4-7:1,柠檬酸的添加量为调节含有低共熔溶剂的酸性乙醇水溶液的pH值为2-3,其中,含有低共熔溶剂的酸性乙醇水溶液中乙醇含量为40-55wt%,氢键受体的含量为10-15wt%;
S2.原花青素纳米级胶囊的制备:配制聚乳酸-聚己内酯溶液,使用注射泵分别将原花青素溶液和聚乳酸-聚己内酯溶液密闭撞击射流混合器的两个入口,入口内径为0.5-1.5mm,在注射泵的推动作用下,两股流体碰撞混合,得到纳米胶囊悬浮液,从出口流出,出口内径为1.5-2.5mm,用孔径为0.1μm的滤膜过滤,洗涤,冷冻干燥,得到原花青素纳米级胶囊粉;
所述聚乳酸-聚己内酯溶液中聚乳酸的含量为20-25wt%,聚己内酯的含量为17-22wt%,余量为水;
S3.原花青素微米级微胶囊粉的制备:将明胶和黄原胶溶于水中,得到明胶-黄原胶溶液,将22-25重量份步骤S2制得的原花青素纳米级胶囊粉、3-5重量份维生素E加入100重量份食用油中,得到纳米胶囊油悬浮液,将100重量份明胶-黄原胶溶液和40-70重量份纳米胶囊油悬浮液混合,12000-15000r/min均质3-5min,调节溶液pH值为4.2-4.5,搅拌反应30-50min,调节pH值为6.3-6.7,加入4-5重量份谷氨酰胺转氨酶,搅拌反应20-40min,离心,洗涤,冷冻干燥,制得原花青素微米级微胶囊粉;
所述明胶-黄原胶溶液中明胶的浓度为25-35wt%,黄原胶的浓度为22-30wt%,余量为水;
S4.包埋:将10重量份步骤S3制得的原花青素微米级微胶囊粉、4-7重量份海藻酸钠、5-10重量份羧甲基纤维素钠加入100重量份水中,12000-15000r/min均质3-5min,滴加10-20重量份4-7wt%的金属离子溶液,离心,洗涤,冷冻干燥,制得原花青素微小胶囊粉;
S5.二次包埋:将10重量份壳聚糖溶于100重量份1-2wt%的乙酸溶液中后,加入17-25重量份α-酮戊二酸,加热至45-55℃,搅拌反应14-17h,加入2-4重量份硼氢化钠,继续搅拌反应2-4h,加入乙醇至体系乙醇含量为70-80wt%,过滤,洗涤,干燥,研细,得到羧基化壳聚糖,将10重量份羧基化壳聚糖加入50重量份水中,加入5-7重量份步骤S4制得的原花青素微小胶囊粉混合,12000-15000r/min均质3-5min,滴加5-10重量份4-7wt%的金属离子溶液,常温固化30-50min,过滤,洗涤,干燥,制得原花青素微胶囊。
8.一种如权利要求1-7任一项所述的制备方法制得的原花青素微胶囊。
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