CN112244279A - 富勒烯固态自乳化材料及其制备方法和用途 - Google Patents
富勒烯固态自乳化材料及其制备方法和用途 Download PDFInfo
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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
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Abstract
本发明涉及富勒烯固态自乳化材料及其制备方法和用途。该乳化材料的配方为：富勒烯3‑7份，脂质12‑30份，乳化剂8‑25份，助乳化剂1‑10份，固体吸附剂30‑80份。上述各成分混合溶解后形成富勒烯固态自乳化材料。该材料具有良好的水溶性，稳定性，且制备工艺简单可控，重复性好可以应用于含富勒烯功能食品的制备。
Description
技术领域
本发明涉及化工材料及制备方法，特别涉及富勒烯固态自乳化材料及其制备方法和用途。
背景技术
富勒烯(Fullerene，C60)是单质碳的同素异形体。其结构是由12个五边形和20个六边形组成的一个中空的32面体，密度为1.678g/cm3，熔点＞553K。C60外观呈深黄固体，随厚度不同颜色可呈棕色到黑色。富勒烯具有很高的抗氧化能力，是维生素C的125倍，其作用原理与超氧化物歧化酶(SOD)类似，同时其在捕捉自由基分子的能力和速度方面均高于β-胡萝卜素。此外，富勒烯的安全性也很高，并且已在医药、化妆品和食品等领域有一定的研究。
医药方面，富勒烯具有很强的光动力活性、清除自由基活性，并可以作为基因载体及药物载体，这使得它能在治疗肿瘤及由氧化应激导致的疾病等方面发挥重要作用。化妆品方面，富勒烯对自由基的作用主要表现在除了像维生素C能提供即时抗氧化作用，还能像海绵一样持续有效地吸附自由基，并且富勒烯为细胞提供长效保护罩，提高细胞自身抵御损伤的能力。
在食品领域，富勒烯可以通过胃肠道吸收，清除体内自由基，并且也可作为抗氧化剂通过延缓脂肪酸的自动氧化过程来提高油酸及其食品的稳定性，延长保质期。然而，富勒烯在水、大多数油脂以及极性溶剂中溶解度均极差，通常只能用芳香性溶剂，如甲苯，氯苯，或非芳香性溶剂二硫化碳溶解。而且，富勒烯光稳定性差，生物利用度低，这导致富勒烯在食品中的应用大大受到限制。目前，通过化学改性的富勒烯如水溶性富勒烯和油溶性富勒烯其抗氧化性等性能会受到很大的影响，因此，需要通过其他更好的方法解决富勒烯的应用缺陷。
自乳化体系是由脂质和乳化剂组成用于负载油溶性活性成分，分在散在水中时可自发形成O/W纳米乳液。自乳化体系可明显增加活性成分的吸收和利用，且制备工艺简单，适合规模化生产。自乳化体系可分为液体自乳化体系和固体自乳化体系。然而，液体自乳化体系具有脂含量高，口服适应性差，稳定性差等缺陷。如果经固体吸附剂物理吸附液体自乳化体系形成的固体自乳化体系可以克服液体自乳化体系的各种缺陷。
发明内容
发明目的：本发明的目的是提供一种富勒烯固态自乳化材料，该材料提高了富勒烯的溶解度和稳定性，提高了富勒烯的生物利用度。
本发明的另一目的是提供所述富勒烯固态自乳化材料的制备方法和用途。
技术方案：本发明的富勒烯固态自乳化材料，包括如下重量份数的原料：
进一步地，所述的脂质为玉米油、橄榄油、大豆油、月见草油、澳洲坚果油、辛酸/癸酸甘油三酯、三乙酸甘油酯、三油酸甘油酯中的一种或几种的混合。
进一步地，所述的乳化剂为吐温20、吐温60、吐温80、硬脂醇聚醚-6、硬脂醇聚醚-21、硬脂醇聚醚-25、聚甘油6-硬脂酸酯、聚甘油10-硬脂酸酯中的一种或几种的混合。
进一步地，所述的助乳化剂为聚甘油蓖麻醇酯、甘油、磷脂、聚乙二醇-4000、聚乙二醇-30二聚羟基硬脂酸酯中的一种或几种的混合。
进一步地，所述的固体吸附剂为二氧化硅、无水磷酸氢钙、多孔淀粉、硅酸镁铝中的任意一种。
所述的富勒烯固态自乳化材料的制备方法，包括以下步骤：
(1)按配方比例称取富勒烯，脂质，乳化剂和助乳化剂，混合搅拌，将富勒烯溶解形成富勒烯液体自乳化材料；
(2)将富勒烯液体自乳化材料冷却至室温，加入固体吸附剂，进行物理混合，形成富勒烯固体自乳化材料。
所述的富勒烯固态自乳化材料在制备功能性食品中的用途。
有益效果：通过富勒烯固体自乳化材料的配方、富勒烯的添加量等条件，可制备含量为3-7％的富勒烯固体自乳化材料；本发明制备的富勒烯固体自乳化材料，具有很高含量的富勒烯，可达到发挥功效的浓度；本发明采用富勒烯固体自乳化材料包裹富勒烯，显著提高了富勒烯的水溶性和稳定性，从而提高其口服生物利用度；本发明固体材料具有较好的离心稳定性和物理稳定性；
本发明制备的富勒烯固态自乳化材料，并且具有较高的包封率(＞99％)和较好的缓释效果，提高了富勒烯的生物利用度。
附图说明
图1为本发明方法的流程示意图；
图2为本发明产品的离心稳定性测试图；
图3为本发明产品的储存稳定性测试图；
图4为本发明产品的体外模拟消化粒径变化图。
具体实施方式
实施例1
本实施例的材料配方如下：
该实施例的制备步骤如下：
1、准确称取富勒烯5.0g，玉米油20.0g，月见草油5.5g，吐温80 6.0g，吐温608.0g，聚甘油蓖麻醇酯8.5g，在60℃，300rpm磁力搅拌1h，直至富勒烯完全溶解，形成富勒烯液体自乳化；
2、将固体吸附剂二氧化硅57.0g与富勒烯液体自乳化在常温下均匀混合，形成富勒烯固体自乳化材料；
3、该富勒烯固体自乳化材料水分散后，经粒径电位分析仪测定其平均粒径为101.37±4.12nm。并25℃下室温放置1个月后其平均粒径为110.23±2.16nm，即粒径变化无明显差异，储存稳定性良好。
实施例2
本实施例的材料配方如下：
该实施例的制备步骤如下：
1、准确称取富勒烯7.0g，橄榄油8.3g，三乙酸甘油酯21.2g，吐温20 1.0g，硬脂醇聚醚-6 9.5g，聚甘油蓖麻醇酯2.5g，在72℃，500rpm磁力搅拌1h，直至富勒烯完全溶解，形成富勒烯液体自乳化；
2、将固体吸附剂无水磷酸氢钙50.5g与富勒烯液体自乳化在常温下均匀混合，形成富勒烯固体自乳化材料；
3、该富勒烯固体自乳化材料水分散后，经粒径电位分析仪测定其平均粒径为132.21±4.34nm。并25℃下室温放置1个月后其平均粒径为139.11±5.09nm，即粒径变化无明显差异，储存稳定性良好。
实施例3
本实施例的材料配方如下：
该实施例的制备步骤如下：
1、准确称取富勒烯3.0g，辛酸/癸酸甘油三酯18.5g，聚甘油6-硬脂酸酯7.0g，聚甘油10-硬脂酸酯2.5g，磷脂3.0g，在68℃，400rpm磁力搅拌1h，直至富勒烯完全溶解，形成富勒烯液体自乳化；
2、将固体吸附剂多孔淀粉66.0g与富勒烯液体自乳化在常温下均匀混合，形成富勒烯固体自乳化材料；
3、该富勒烯固体自乳化材料水分散后，经粒径电位分析仪测定其平均粒径为98.92±2.07nm。并25℃下室温放置1个月后其平均粒径为101.33±3.25nm，即粒径变化无明显差异，储存稳定性良好。
性能测试：
采用本发明的产品进行离心稳定性和储存稳定性测试，见图2和3。
在不同离心时间下富勒烯固体自乳化材料稀释后的粒径和PDI变化如图2所示：纳米载体的粒径变化均在10nm左右，而PDI的变化也不大，说明富勒烯固体自乳化载体的离心稳定性较好。
如图3所示，在25℃储存期间，富勒烯固体自乳化材料稀释后的粒径增大了约10-20nm，而PDI的变化在0.05左右，表明富勒烯固体自乳化材料储存在室温下具有良好的物理稳定性。
如图4所示，胃液消化后，粒径变化不大，肠液消化后，粒径普遍增大了10-20nm。这可能与肠液中的胆盐和游离脂肪酸有关。肠液阶段消化实验结束后，进一步对富勒烯纳米乳液的生物利用度进行了评价。富勒烯原药的生物可及度为0.009％，生物可及度为38.39％；富勒烯固态自乳化后可将其生物可及度提高到了41.03％，这说明富勒烯固态自乳化材料提高了富勒烯的生物可及率。
Claims (7)
1.一种富勒烯固态自乳化材料，其特征在于：包括如下重量份数的原料：
2.根据权利要求1所述的富勒烯固态自乳化材料，其特征在于：所述的脂质为玉米油、橄榄油、大豆油、月见草油、澳洲坚果油、辛酸/癸酸甘油三酯、三乙酸甘油酯、三油酸甘油酯中的一种或几种的混合。
3.根据权利要求1所述的富勒烯固态自乳化材料，其特征在于：所述的乳化剂为吐温20、吐温60、吐温80、硬脂醇聚醚-6、硬脂醇聚醚-21、硬脂醇聚醚-25、聚甘油6-硬脂酸酯、聚甘油10-硬脂酸酯中的一种或几种的混合。
4.根据权利要求1所述的富勒烯固态自乳化材料，其特征在于：所述的助乳化剂为聚甘油蓖麻醇酯、甘油、磷脂、聚乙二醇-4000、聚乙二醇-30二聚羟基硬脂酸酯中的一种或几种的混合。
5.根据权利要求1所述的富勒烯固态自乳化材料，其特征在于：所述的固体吸附剂为二氧化硅、无水磷酸氢钙、多孔淀粉、硅酸镁铝中的任意一种。
6.权利要求1-5任一项所述的富勒烯固态自乳化材料的制备方法，其特征在于：包括以下步骤：
(1)按配方比例称取富勒烯，脂质，乳化剂和助乳化剂，混合搅拌，将富勒烯溶解形成富勒烯液体自乳化材料；
(2)将富勒烯液体自乳化材料冷却至室温，加入固体吸附剂，进行物理混合，形成富勒烯固体自乳化材料。
7.权利要求1-5任一项所述的富勒烯固态自乳化材料在制备功能性食品中的用途。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104434797A (zh) * | 2014-12-02 | 2015-03-25 | 中国药科大学 | 一种氟苯尼考固体自乳化制剂 |
| CN109258934A (zh) * | 2018-03-27 | 2019-01-25 | 厦门福慈生物科技有限公司 | 富勒烯微囊粉作为饲料添加剂的应用 |
| CN109481463A (zh) * | 2017-09-12 | 2019-03-19 | 北京福纳康生物技术有限公司 | 一种口服富勒烯乳剂、制备方法及应用 |
| CN109924491A (zh) * | 2019-04-01 | 2019-06-25 | 东南大学 | 一种二氢杨梅素固态自乳化材料及其制备方法和应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104434797A (zh) * | 2014-12-02 | 2015-03-25 | 中国药科大学 | 一种氟苯尼考固体自乳化制剂 |
| CN109481463A (zh) * | 2017-09-12 | 2019-03-19 | 北京福纳康生物技术有限公司 | 一种口服富勒烯乳剂、制备方法及应用 |
| CN109258934A (zh) * | 2018-03-27 | 2019-01-25 | 厦门福慈生物科技有限公司 | 富勒烯微囊粉作为饲料添加剂的应用 |
| CN109924491A (zh) * | 2019-04-01 | 2019-06-25 | 东南大学 | 一种二氢杨梅素固态自乳化材料及其制备方法和应用 |
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