CN109430864A - 一种蓝莓花青素微胶囊的制备方法 - Google Patents
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Abstract
本发明提供了一种蓝莓花青素微胶囊及其制备方法，包括如下步骤：将亲水胶体充分溶解在蒸馏水中，然后加入羧甲基淀粉，搅拌使之溶解均匀；放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材；在微胶囊的壁材中加入预先称量的蓝莓花青素，搅拌均匀，得总混合物；将总混合物在高速剪切机中剪切，使之混合均匀，再将此混合物进行冷冻干燥，取出研磨过筛，制得蓝莓花青素微胶囊。本发制备的微胶囊具有良好的协同性和食品安全性，制备方法可以提高包埋率、耐热稳定性和降低成本。
Description
技术领域
本发明属于属于微胶囊领域，具体涉及一种蓝莓花青素微胶囊的制备方法。
背景技术
蓝莓，又名越橘，是杜鹃花科越桔属多年生常绿灌木。蓝莓花青素以其众所周知的促进健康及富含花青素等特点近年来备受关注。花青素是一种水溶性的植物色素，可以增强蓝莓的颜色，而且它们还具有多种生理活性功能，如抗氧化、促进视红素再合成、提高免疫力、抗心血管疾病、抗衰老等。
蓝莓花青素广泛应用于食品、天然色素、化妆品、药品等领域，但花青素分子极不稳定，易降解，尤其对光、温度、氧、酶活性和各种贮存条件都很敏感。在食品加工过程中，特别是在氧的存在下，花青素的稳定性随着温度的升高而降低，最终导致热降解产生棕色产物。已有文献报道花青素提取物在贮藏过程中抗氧化能力或活性会发生变化。因此，提高蓝莓花青素的稳定性是一个亟待解决的重要问题。
目前，提高蓝莓花青素稳定性的机制主要是交联反应和微胶囊化。交联反应存在一些缺陷，如反应的精确控制困难，以及在提高稳定性的过程中对相互作用机制缺乏了解。微胶囊化技术可以用在固体颗粒(微球)或液体小泡中进行固定和载运生物活性化合物，以保护和稳定生物活性化合物。微胶囊化有利于对光和热敏感的分子，如花青素，可以保持稳定性，提高其保质期。微胶囊化是一种快速发展的技术，具有高度专业化和低成本的优点。
在食品工业中，低温真空冷冻干燥是一种适合于热敏性颜料包埋的方法，有不同的载体材料被用于真空低温冷冻干燥来包埋花青素，如明胶、乳清蛋白、麦芽糊精、壳聚糖等，但这些材料成本较高、制备过程复杂，且合成物质和一些基于动物来源产品的安全性已引起用户的关注，所以许多研究者正试图寻求一种天然安全的可再生资源的材料用于包埋蓝莓花青素的微胶囊高分子载体。羧甲基淀粉是一种重要的淀粉衍生物，由淀粉游离羟基与羧甲基基团(-CH2COOH)醚化反应合成。羧甲基淀粉具有许多独特的性能，如良好的生物相容性、冷水可溶性、较高的糊稳定性和透明度等。因此，羧甲基淀粉是一种可生物降解、亲水且相对廉价的绿色高分子材料，在工业上引起了广泛的关注。
然而，没有一种单一的包埋材料能够对特定的应用提供有效的功能效果，如抗氧化性和耐热稳定性，也不能提供更高的包埋率。
为了提高蓝莓花青素的包埋率和稳定性，选择羧甲基淀粉-亲水胶体复配体系作为真空冷冻干燥微胶囊的壁材，目前在国内还没有关于相关的报道和产品。
发明内容
一种蓝莓花青素微胶囊的制备方法，其特征在于，包括如下步骤：
步骤一，室温下，将亲水胶体充分溶解在蒸馏水中，然后加入羧甲基淀粉，搅拌使之溶解均匀；
步骤二，将羧甲基淀粉和亲水胶体混合溶液放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材；
步骤三，然后在微胶囊的壁材中加入预先称量的蓝莓花青素，搅拌均匀，得总混合物；
步骤四，将总混合物在高速剪切机中剪切，使之混合均匀，再将此混合物进行冷冻干燥，取出研磨过筛，制得蓝莓花青素微胶囊。
进一步，所述的亲水胶体为黄原胶、阿拉伯胶、海藻酸钠、瓜尔胶或其他可食用的亲水胶体中的一种或多种。
进一步，所述的羧甲基淀粉与亲水胶体的质量比为30-150∶1。
进一步，所述的蓝莓花青素和微胶囊的壁材的质量比为1∶2-10。
进一步，总混合物的固形物质量浓度在2-12％。
进一步，将总混合物在高速剪切机中，以10000r/min的速度下剪切4min，使之混合均匀，再将此混合物进行-78℃低温冷冻12h，然后取出在真空冷冻干燥机内进行脱水干燥42h，取出研磨过筛，制得蓝莓花青素微胶囊。
一种蓝莓花青素微胶囊，由上述制备方法制得。
淀粉-亲水胶体复配体系作为微胶囊壁材具有良好的协同性和食品安全性，可以提高包埋率、耐热稳定性和降低成本等作用。因此，利用淀粉-亲水胶体复配扩大淀粉的应用范围已成为一种发展趋势。
本发明具体效果主要体现在以下三个方面：
1.在热重分析中，随着温度的升高，蓝莓花青素质量损失显著增加，在218℃温度下，蓝莓花青素的质量保留率为75.92％，普通蓝莓花青素微胶囊质量保留率为85.28％，而本发明蓝莓微胶囊的质量保留率为92.02％。本发明蓝莓花青素微胶囊在高温下总质量损失小，失重速度慢，提高了蓝莓花青素的热稳定性(见图1)；
2.本发明蓝莓花青素微胶囊在荧光倒置显微镜下发出红色荧光，蓝莓花青素较为均匀的分布在微胶囊中，周围几乎未见散落的未包埋的花青素，证明本发明制备的蓝莓花青素微胶囊具有较高的包埋率(见图2)；
3.5℃条件下保存30天后的蓝莓花青素含量仅为60.56％，普通蓝莓花青素微胶囊含量为64.18％，通过本发明制备的蓝莓花青素微胶囊含量为90.47％；37℃条件下保存30天后的蓝莓花青素含量仅为32.40％，普通蓝莓花青素微胶囊含量为45.61％，通过本发明制备的蓝莓花青素微胶囊含量为76.11％。可以发现通过该方法制得的蓝莓花青素微胶囊，具有较好的贮藏稳定性(见图3)。
附图说明
图1，蓝莓花青素标准品、普通蓝莓花青素微胶囊和本发明实施例1制得的蓝莓花青素微胶囊在温度升高过程中的质量保留率比较图。
图2，通过荧光倒置显微镜观察花青素在本发明蓝莓花青素微胶囊中的分布情况和蓝莓花青素微胶囊外观。
图3a，运用本发明实施例1制备的蓝莓花青素微胶囊在5℃条件分别贮藏15天和30天后的花青素含量；图3b，运用本发明实施例1制备的蓝莓花青素微胶囊在30℃条件下分别贮藏15天和30天后的花青素含量。
具体实施方式
实施例1
室温下，将0.195g黄原胶充分溶解在200mL蒸馏水中，然后加入17.55g羧甲基淀粉，搅拌使之溶解均匀，再将羧甲基淀粉和黄原胶混合溶液放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材。然后在羧甲基淀粉-黄原胶复配体系壁材中加入4.44g蓝莓花青素，搅拌均匀。将总混合物在高速剪切机中，以10,000r/min的速度下剪切4min，使之混合均匀，再将此混合物进行-78℃低温冷冻12h，然后取出在真空冷冻干燥机内进行脱水干燥42h，取出研磨过筛，制得蓝莓花青素微胶囊。该微胶囊的蓝莓花青素包埋率为97.38％，5℃条件下贮存30天后蓝莓花青素含量为90.47％，37℃条件下贮存30天后蓝莓花青素含量为76.11％，达到保护和提高蓝莓花青素稳定性的效果。(本实施例是目前实验中效果最好的复配比例和胶体种类)
实施例2
室温下，将0.272g阿拉伯胶充分溶解在200mL蒸馏水中，然后加入8.16羧甲基淀粉，搅拌使之溶解均匀，再将羧甲基淀粉和阿拉伯胶混合溶液放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材。然后在羧甲基淀粉-阿拉伯胶复配体系壁材中加入2.108g蓝莓花青素，搅拌均匀。将总混合物在高速剪切机中，以10,000r/min的速度下剪切4min，使之混合均匀，再将此混合物进行-78℃低温冷冻12h，然后取出在真空冷冻干燥机内进行脱水干燥42h，取出研磨过筛，制得蓝莓花青素微胶囊。该微胶囊的蓝莓花青素包埋率为94.72％，5℃条件下贮存30天后蓝莓花青素含量为86.32％，37℃条件下贮存30天后蓝莓花青素含量为70.29％，达到保护和提高蓝莓花青素稳定性的效果。
实施例3
室温下，将0.173g瓜尔胶充分溶解在200mL蒸馏水中，然后加入10.38g羧甲基淀粉，搅拌使之溶解均匀，再将羧甲基淀粉和瓜尔胶混合溶液放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材。然后在羧甲基淀粉-瓜尔胶复配体系壁材中加入2.11g蓝莓花青素，搅拌均匀。将总混合物在高速剪切机中，以10,000r/min的速度下剪切4min，使之混合均匀，再将此混合物进行-78℃低温冷冻12h，然后取出在真空冷冻干燥机内进行脱水干燥42h，取出研磨过筛，制得蓝莓花青素微胶囊。该微胶囊的蓝莓花青素包埋率为95.31％，5℃条件下贮存30天后蓝莓花青素含量为83.51％，37℃条件下贮存30天后蓝莓花青素含量为68.27％，达到保护和提高蓝莓花青素稳定性的效果。
实施例4
室温下，将0.129g海藻酸钠充分溶解在200mL蒸馏水中，然后加入12.90g羧甲基淀粉，搅拌使之溶解均匀，再将羧甲基淀粉和海藻酸钠混合溶液放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材。然后在羧甲基淀粉-海藻酸钠复配体系壁材中加入4.34g蓝莓花青素，搅拌均匀。将总混合物在高速剪切机中，以10,000r/min的速度下剪切4min，使之混合均匀，再将此混合物进行-78℃低温冷冻12h，然后取出在真空冷冻干燥机内进行脱水干燥42h，取出研磨过筛，制得蓝莓花青素微胶囊。该微胶囊的蓝莓花青素包埋率为96.20％，5℃条件下贮存30天后蓝莓花青素含量为88.64％，37℃条件下贮存30天后蓝莓花青素含量为72.33％，达到保护和提高蓝莓花青素稳定性的效果。
所有上述的首要实施这一知识产权，并没有设定限制其他形式的实施这种新产品和/或新方法。本领域技术人员将利用这一重要信息，上述内容修改，以实现类似的执行情况。但是，所有修改或改造基于本发明新产品属于保留的权利。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。
Claims (7)
1.一种蓝莓花青素微胶囊的制备方法，其特征在于，包括如下步骤：
步骤一，室温下，将亲水胶体充分溶解在蒸馏水中，然后加入羧甲基淀粉，搅拌使之溶解均匀；
步骤二，将羧甲基淀粉和亲水胶体混合溶液放置在4℃温度下的冰箱内24小时，使混合物充分水合，作为微胶囊的壁材；
步骤三，然后在微胶囊的壁材中加入预先称量的蓝莓花青素，搅拌均匀，得总混合物；
步骤四，将总混合物在高速剪切机中剪切，使之混合均匀，再将此混合物进行冷冻干燥，取出研磨过筛，制得蓝莓花青素微胶囊。
2.根据权利要求1所述的一种蓝莓花青素微胶囊的制备方法，其特征在于，所述的亲水胶体为黄原胶、阿拉伯胶、海藻酸钠、瓜尔胶或其他可食用的亲水胶体中的一种或多种。
3.根据权利要求1所述的一种蓝莓花青素微胶囊的制备方法，其特征在于，所述的羧甲基淀粉与亲水胶体的质量比为30-150∶1。
4.根据权利要求1所述的一种蓝莓花青素微胶囊的制备方法，其特征在于，所述的蓝莓花青素和微胶囊的壁材的质量比为1∶2-10。
5.根据权利要求4所述的一种蓝莓花青素微胶囊的制备方法，其特征在于，总混合物的固形物质量浓度在2-12％。
6.根据权利要求1所述的一种蓝莓花青素微胶囊的制备方法，其特征在于，将总混合物在高速剪切机中，以10000r/min的速度下剪切4min，使之混合均匀，再将此混合物进行-78℃低温冷冻12h，然后取出在真空冷冻干燥机内进行脱水干燥42h，取出研磨过筛，制得蓝莓花青素微胶囊。
7.一种蓝莓花青素微胶囊，由上述1-6任一项所述的蓝莓花青素微胶囊的制备方法制得。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109907299A (zh) * | 2019-03-21 | 2019-06-21 | 安徽农业大学 | 一种双重响应型淀粉基纳米乳液及其制备方法 |
| CN111544365A (zh) * | 2020-06-10 | 2020-08-18 | 合肥师范学院 | 一种蓝莓护色唇釉及其制备方法 |
| WO2021073094A1 (zh) * | 2019-10-13 | 2021-04-22 | 浙江大学 | 以原花色素为壁材的鱼油微胶囊及制备方法 |
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| CN113995015A (zh) * | 2021-11-17 | 2022-02-01 | 合肥工业大学 | 一种控制酸奶后酸化的方法 |
| CN114711408A (zh) * | 2021-12-31 | 2022-07-08 | 南通奥凯生物技术开发有限公司 | 一种冷冻干燥法制备微胶囊化柚皮油的方法 |
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| CN109907299A (zh) * | 2019-03-21 | 2019-06-21 | 安徽农业大学 | 一种双重响应型淀粉基纳米乳液及其制备方法 |
| WO2021073094A1 (zh) * | 2019-10-13 | 2021-04-22 | 浙江大学 | 以原花色素为壁材的鱼油微胶囊及制备方法 |
| CN111544365A (zh) * | 2020-06-10 | 2020-08-18 | 合肥师范学院 | 一种蓝莓护色唇釉及其制备方法 |
| CN112931764A (zh) * | 2021-02-08 | 2021-06-11 | 陕西师范大学 | 一种基于紫花苜蓿花朵花色苷的微胶囊制作方法 |
| CN113995015A (zh) * | 2021-11-17 | 2022-02-01 | 合肥工业大学 | 一种控制酸奶后酸化的方法 |
| CN114711408A (zh) * | 2021-12-31 | 2022-07-08 | 南通奥凯生物技术开发有限公司 | 一种冷冻干燥法制备微胶囊化柚皮油的方法 |
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