CN115429775A - 一种姜黄素微胶囊的制备方法 - Google Patents

一种姜黄素微胶囊的制备方法 Download PDF

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CN115429775A
CN115429775A CN202211117772.4A CN202211117772A CN115429775A CN 115429775 A CN115429775 A CN 115429775A CN 202211117772 A CN202211117772 A CN 202211117772A CN 115429775 A CN115429775 A CN 115429775A
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张雪飞
翟姣
杨传伦
郑磊
陈梦姣
邓海涛
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Chambroad Chemical Industry Research Institute Co Ltd
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Abstract

本发明涉及一种姜黄素微胶囊的制备方法,本方法以糊精、海藻酸钠、磷脂等为壁材,姜黄素为芯材,加入适量乳化剂,利用微胶囊造粒仪,采用单喷头包埋法,制备姜黄素微胶囊。与喷雾干燥法相比,该方法条件温和,操作简单,后处理简易,最终得到形状均匀,粒径在1mm的微胶囊颗粒,包埋率80%左右。本发明制得的姜黄素微胶囊不仅具有很好的稳定性,延长了姜黄素产品的货架期,还具有很好的缓释功能。

Description

一种姜黄素微胶囊的制备方法
技术领域
本发明属于食品药品及其制备方法技术领域,具体涉及一种姜黄素微胶囊的制备方法。
背景技术
微胶囊是一种具有聚合物壁壳的微型容器,可以把气体、固体、液体物质进行包埋,将相应的芯材包埋在囊腔内,在一定程度上将芯材物质与外界环境隔绝,还能够保持芯材物质原有的特性和功能。微胶囊技术可以在一定程度上改变物质的稳定性,也解决了一些水溶性差的物质的应用范围。
目前微胶囊的主要实现方法包括:喷雾干燥法、喷雾冷凝法、空气悬浮法、旋转悬浮分离法、油相分离法、水相分离法、挤压法、锐孔法、粉末床法、熔化分散法。文献报道的大部分微胶囊的制备都采用了喷雾干燥法,喷雾干燥法操作简单、易于工业化流水作业、成本低,但是喷雾干燥法包埋率低、能耗大,一些热敏性物质也不适用喷雾干燥。喷雾冷凝法适合室温下为固态的物质,限制性较大。空气悬浮法芯材必须为固体物质,而且有颗粒粘连、碰撞破碎的问题,在一定程度上限制了其使用。文献报道的采用相分离法制备微胶囊的方法主要使用单凝聚法或复凝聚法,主要用于香精、油脂等物质的包埋。文献报道的采用锐孔法制备微胶囊的方法比较简单,制得的胶囊微珠直径大,没有相应的技术手段改变微囊的尺寸,具有一定的限制性。
微胶囊造粒仪的原理是通过锐孔法来制造微胶囊,它可以通过高频震动将海藻酸钠溶液通过喷嘴分散成大小均匀的液滴,经过静电场的分散使液滴表面带上同种电荷,经过固化液的固化形成微胶囊,与文献中的锐孔法相比,采用微胶囊造粒仪得到的微珠粒径小,形状均匀,操作简单,可以实现产品的快速生产。
姜黄素类化合物是从姜科植物姜黄、莪术、郁金的根茎中提取的主要活性成分,天然姜黄素类化合物主要包括姜黄素、脱甲氧基姜黄素、双去甲氧基姜黄素,姜黄素类化合物作为一种天然色素广泛地应用在食品工业中。近几年研究发现,姜黄素还具有很好的药用价值,主要表现在抗氧化、抗炎、抗癌、提高记忆力、降血脂、清除自由基、保护肝脏等。但姜黄素水溶性很差,很难被人体利用和吸收,而且对光比较敏感,易分解,稳定性较差,这导致姜黄素在储藏和应用方面存在一定的局限性,严重限制了姜黄素在食品及药品领域的应用。
姜黄素的稳定性不高、水溶性差,严重限制了姜黄素的应用,微胶囊技术可以在一定程度上提高姜黄素的稳定性和水溶性,拓宽姜黄素的应用范围,为进一步研究姜黄素的特性提供了依据。
发明内容
本发明的目的在于提供一种姜黄素微胶囊的制备方法,该方法主要采用微胶囊造粒仪制备姜黄素微胶囊,该方法操作简单、条件温和,可以快速得到形状均匀、粒径均一的微胶囊,该微胶囊可以很好的保持姜黄素的活性及稳定性。
为实现上述目的,本申请是通过以下技术方案实现的:
一种姜黄素微胶囊的制备方法,包括以下步骤:
(1)姜黄素超微粉末的制备:
将姜黄素与糊精或磷脂中的一种或两种按照质量比10:1-10:0-10充分混合,经超微粉碎得混合粉末;
(2)海藻酸钠溶液的制备:
将0.5-2.0g海藻酸钠溶解在100ml蒸馏水中,常温搅拌8-10h得相应浓度的海藻酸钠溶液;
(3)姜黄素海藻酸钠乳液的制备:
按照质量比1:0.1-0.5:50-100将姜黄素超微粉、乳化剂、海藻酸钠溶液充分混合,经高速剪切、高压均质,得到混合均匀的姜黄素海藻酸钠乳液;
(4)姜黄素微胶囊的制备:
用微胶囊造粒仪通过单喷头包埋法制备姜黄素微胶囊,将均质好的姜黄素海藻酸钠乳液装入耐压瓶中,喷嘴孔径150-750μm,喷头距离固化液20-30cm,通过调节压力旋钮及流速调节阀控制液体进入微胶囊造粒仪的液体量,调节震动频率及静电场使乳液分散成细小液滴,于整个电场下方放置固化液收集分散的液滴,固化5-30min成膜,经过滤、洗涤、干燥得姜黄素微胶囊。
进一步的,步骤(1)中姜黄素超微粉末的主要成分为姜黄素、糊精和/或磷脂,质量比为10:2-8:0-5,优选为10:3-6:0-2,混合物超微粉碎时间为5-10min。
进一步的,若姜黄素超微粉末中包括有糊精时,所述糊精为α-环糊精、β-环糊精或γ-环糊精,优选为γ-环糊精。
进一步的,步骤(2)中的海藻酸钠的浓度为1.0g/100ml,搅拌时间不低于6h。
进一步的,步骤(3)中的乳化剂为吐温-60、吐温-80、单甘油酯、乳酸脂肪酸甘油酯、聚甘油脂肪酸酯中的一种或多种。
进一步的,步骤(3)的剪切速度为4000-6000r/min。
进一步的,步骤(3)中的高压均质是在压力为10-20MPa下均质2-5次,每次均质时间30min。
进一步的,步骤(4)中的微胶囊造粒仪的震动频率为1000Hz,静电场电压为1500V,压力200mbar。
进一步的,步骤(4)中的固化液为质量百分比浓度1%-5%的氯化钙溶液。
进一步的,步骤(4)中的固化液为质量百分比浓度1.5%-3%的氯化钙溶液。
本发明的有益效果是:
本发明提供一种利用微胶囊造粒仪制备姜黄素微胶囊的方法,以海藻酸钠为主要壁材,姜黄素作为芯材,通过添加乳化剂的方式使姜黄素与其他物料形成稳定的乳液,通过调整仪器参数及喷嘴尺寸来调整胶囊的粒径,经过氯化钙溶液的固化后,姜黄素可以很好的包埋在海藻酸钠微囊中,该微胶囊具有很好缓释功效。
与现有技术相比,本发明具有以下优点:
1、操作简单,可以实现快速生产;2、姜黄素包埋率高,得到胶囊粒径均匀,大小合适;3、设备占地面积小,能耗低。
具体实施方式
以下通过实施例对本发明的技术方案进行详细说明,以下的实施例仅用于解释和说明本发明的技术方案,而不能解释为是对本发明技术方案的限制。
实施例1
姜黄素、γ-环糊精、磷脂按质量比10:3:1充分混合,混合物超微粉碎5min得姜黄素超微粉;将姜黄素超微粉、吐温-80、1%海藻酸钠溶液按质量比1:0.3:60的比例混合,以5000r/min的转速剪切5min,剪切后混合液体在压力15MPa条件下均质2次,每次30min得姜黄素乳液;将姜黄素乳液装入仪器配套的耐压瓶中,选取孔径大小300μm的喷头安装各仪器配件,喷头距氯化钙接收液20cm,微胶囊造粒仪振动频率1000Hz,静电场电压1500V,压力200mbar。通过调节液体流速限流阀控制液体进入量,乳液经过电场分散成小液滴,滴入到质量浓度2%氯化钙固化液中,固化10min,过滤,洗涤,干燥得姜黄素微胶囊,粒径1.1-1.3mm,包埋率达到78.33%。
实施例2
姜黄素、γ-环糊精按质量比10:2充分混合,混合物超微粉碎10min得姜黄素超微粉;将姜黄素超微粉、吐温-80、聚甘油脂肪酸酯、1%海藻酸钠溶液按质量比1:0.2:0.1:80的比例混合,以5500r/min的转速剪切5min,剪切后混合液体在压力20MPa条件下均质4次,每次30min得姜黄素乳液;将姜黄素乳液装入仪器配套的耐压瓶中,选取孔径大小200μm的喷头安装各仪器配件,喷头距氯化钙接收液25cm,微胶囊造粒仪振动频率1000Hz,静电场电压1500V,压力200mbar。通过调节液体流速限流阀控制液体进入量,乳液经过电场分散成小液滴,滴入到质量浓度3%氯化钙固化液中,固化15min,过滤,洗涤,干燥得姜黄素微胶囊,粒径1mm-1.2mm,包埋率达到75.82%。
实施例3
姜黄素、α-环糊精按质量比10:5充分混合,混合物超微粉碎8min得姜黄素超微粉;将姜黄素超微粉、单甘油酯、乳酸脂肪酸甘油酯、1%海藻酸钠溶液按质量比1:0.1:0.1:100的比例混合,以6000r/min的转速剪切5min,剪切后混合液体在压力10MPa条件下均质3次,每次30min得姜黄素乳液;将姜黄素乳液装入仪器配套的耐压瓶中,选取孔径大小450μm的喷头安装各仪器配件,喷头距氯化钙接收液30cm,微胶囊造粒仪振动频率1000Hz,静电场电压1500V,压力200mbar。通过调节液体流速限流阀控制液体进入量,乳液经过电场分散成小液滴,滴入到质量浓度1.5%氯化钙固化液中,固化30min,过滤,洗涤,干燥得姜黄素微胶囊,粒径1.1mm-1.4mm,包埋率达到73.29%。
实施例4
姜黄素、β-环糊精、磷脂按质量比10:2:1充分混合,混合物超微粉碎10min得姜黄素超微粉;将姜黄素超微粉、吐温-80、1%海藻酸钠溶液按质量比1:0.3:100的比例混合,以5000r/min的转速剪切5min,剪切后混合液体在压力20MPa条件下均质2次,每次30min得姜黄素乳液;将姜黄素乳液装入仪器配套的耐压瓶中,选取孔径大小200μm的喷头安装各仪器配件,喷头距氯化钙接收液25cm,微胶囊造粒仪振动频率1000Hz,静电场电压1500V,压力200mbar。通过调节液体流速限流阀控制液体进入量,乳液经过电场分散成小液滴,滴入到质量浓度3%氯化钙固化液中,固化15min,过滤,洗涤,干燥得姜黄素微胶囊,粒径0.9mm-1.1mm,包埋率达到82.54%。
以上所述仅是本发明的优选实施方式对本发明的详细说明,但是并非用以限定本发明,对于本技术领域的技术人员来说,在不脱离本发明的精神和范围内,还可以做出若干修改和改进,因此本发明的保护范围应以权利要求书所述范围为准。

Claims (10)

1.一种姜黄素微胶囊的制备方法,其特征在于,包括以下步骤:
(1)姜黄素超微粉末的制备:
将姜黄素与糊精或磷脂中的一种或两种按照质量比10:1-10:0-10充分混合,经超微粉碎得混合粉末;
(2)海藻酸钠溶液的制备:
将0.5-2.0g海藻酸钠溶解在100ml蒸馏水中,常温搅拌8-10h得相应浓度的海藻酸钠溶液;
(3)姜黄素海藻酸钠乳液的制备:
按照质量比1:0.1-0.5:50-100将姜黄素超微粉、乳化剂、海藻酸钠溶液充分混合,经高速剪切、高压均质,得到混合均匀的姜黄素海藻酸钠乳液;
(4)姜黄素微胶囊的制备:
用微胶囊造粒仪通过单喷头包埋法制备姜黄素微胶囊,将均质好的姜黄素海藻酸钠乳液装入耐压瓶中,喷嘴孔径150-750μm,喷头距离固化液20-30cm,通过调节压力旋钮及流速调节阀控制液体进入微胶囊造粒仪的液体量,调节震动频率及静电场使乳液分散成细小液滴,于整个电场下方放置固化液收集分散的液滴,固化5-30min成膜,经过滤、洗涤、干燥得姜黄素微胶囊。
2.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(1)中姜黄素超微粉末的主要成分为姜黄素、糊精和/或磷脂,质量比为10:2-8:0-5,混合物超微粉碎时间为5-10min。
3.根据权利要求2所述的姜黄素微胶囊的制备方法,其特征在于,若姜黄素超微粉末中包括有糊精时,所述糊精为α-环糊精、β-环糊精或γ-环糊精。
4.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(2)中的海藻酸钠的浓度为1.0g/100ml,搅拌时间不低于6h。
5.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(3)中的乳化剂为吐温-60、吐温-80、单甘油酯、乳酸脂肪酸甘油酯、聚甘油脂肪酸酯中的一种或多种。
6.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(3)的剪切速度为4000-6000r/min。
7.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(3)中的高压均质是在压力为10-20MPa下均质2-5次,每次均质时间30min。
8.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(4)中的微胶囊造粒仪的震动频率为1000Hz,静电场电压为1500V,压力200mbar。
9.根据权利要求1所述的姜黄素微胶囊的制备方法,其特征在于,步骤(4)中的固化液为质量百分比浓度1%-5%的氯化钙溶液。
10.根据权利要求9所述的姜黄素微胶囊的制备方法,其特征在于,步骤(4)中的固化液为质量百分比浓度1.5%-3%的氯化钙溶液。
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