CN113331398A - 一种β-胡萝卜素-淀粉-壳聚糖微胶囊及制备方法 - Google Patents
一种β-胡萝卜素-淀粉-壳聚糖微胶囊及制备方法 Download PDFInfo
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Abstract
本发明属于微胶囊制备技术领域，具体涉及一种β‑胡萝卜素‑淀粉‑壳聚糖微胶囊及制备方法，将制备好的碱性淀粉乳，低温下与分散在醇中的β‑胡萝卜素复合，保温一段时间后，离心，洗涤，去上清，低温干燥后得到初包物。向一定质量的初包物中添加壳聚糖溶液，充分混匀，真空冷冻干燥即得β‑胡萝卜素‑淀粉‑壳聚糖微胶囊。本发明提供的方法在碱性环境下包埋，β‑胡萝卜素稳定且装载量较高，所用壁材为不同直链含量的淀粉，制备简单。
Description
技术领域
本发明属于微胶囊制备技术领域，具体涉及一种β-胡萝卜素-淀粉-壳聚糖微胶囊及制备方法。
背景技术
β-胡萝卜素是自然界中广泛存在的油溶性色素之一，它是一种天然抗氧化剂，是人体重要营养素VA的前体，在许多天然食物如胡萝卜、菠菜、木瓜、芒果等中含量丰富。但其含大量不饱和双键，光、热、氧等会促进其氧化降解，极大限制了应用范围。选择合适的运载体系是重点研究方向之一。
目前，主要的β-胡萝卜素运载体系有脂质体、乳液、环糊精和淀粉基微胶囊等。脂质体是将芯材包封于磷脂、胆固醇等类脂质双分子层形成的薄膜中间所制成的超微型球体，有较强的细胞亲和力，储藏过程易发生沉淀。乳液是将油相与水相充分混匀制备的均匀分散液，提高了芯材生物利用率，但易出现絮凝分层。环糊精是将乳化均质后的芯材与壁材充分混匀后所得微粒，其保护效果强，但水溶性差。淀粉基微胶囊是在一定温度将淀粉乳与芯材按一定比例添加形成的粉末状颗粒，对光氧不稳定芯材有保护作用，但壁材多为直链淀粉，限制了芯材含量，且与芯材复合过程中多涉及高温处理，芯材损失率高。
发明内容
为了解决上述技术问题，本发明提供一种β-胡萝卜素-淀粉-壳聚糖微胶囊及制备方法，低成本、易操作、耗能低、损失小、储运方便、水分散性好，是对现有β-胡萝卜素包埋技术的发展。本发明技术方案是将制备好的碱性淀粉乳，低温下与分散在醇中的β-胡萝卜素复合，保温一段时间后，离心，洗涤，去上清，低温干燥后得到初包物。向一定质量初包物添加壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。
本发明具体是这样实现的，提供一种β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，包括如下步骤：
1)β-胡萝卜素分散液制备：将β-胡萝卜素分散于醇中，混合均匀；
2)淀粉乳制备：将淀粉分散在碱性溶液中，搅拌均匀，低温振荡一定时间；
3)复合：将步骤1)中得到的β-胡萝卜素分散液滴加到步骤2)制备的淀粉乳中，搅拌均匀，保温；
4)调节步骤3)得到的复合液的pH，然后进行离心，洗涤，低温烘干，得到初包物；
5)向步骤4)所得初包物中添加壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。
优选地，所述步骤1)中，β-胡萝卜素分散液中β-胡萝卜素的浓度为0.1-0.5mg/mL，所述醇为乙醇。
进一步优选，所述步骤2)中淀粉乳中淀粉的浓度为1-5％，淀粉中直链淀粉的含量为55-75％，碱性溶液pH范围9-14，低温为45-75℃，振荡时间为10-60min，振荡培养速率为200-300r/min。
进一步优选，其特征在于，所述步骤2)中，淀粉为玉米淀粉。
进一步优选，所述步骤3)中保温时间为10-60min，振荡培养速率为200-300r/min。
进一步优选，所述步骤4)中，复合液的pH调节为中性，洗涤溶液为无水乙醇，洗涤次数2-5次，干燥温度为35-60℃，时间为6-12h。
进一步优选，所述步骤5)中，向0.05-0.08g的初包物中添加5-10mL壳聚糖溶液，壳聚糖溶液浓度为0.2-0.5％。
本发明还提供根据上述方法制备的β-胡萝卜素-淀粉-壳聚糖微胶囊。
与现有技术相比，本发明的优点在于：
1)所用壁材为不同直链含量的淀粉，制备简单；
2)碱性环境下β-胡萝卜素稳定且装载量较高；
3)复合温度低且时间短，β-胡萝卜素损失率低；
4)在β-胡萝卜素-淀粉微胶囊基础上，添加壳聚糖溶液，提高其水分散性、密封性和结构强度；
5)包埋后淀粉颗粒结构完整，结晶结构完整，淀粉破坏率低。
附图说明
图1为β-胡萝卜素在酸性条件、中性条件和碱性条件下的稳定性；
图2为各个对比例和实施例得到的β-胡萝卜素-玉米淀粉-壳聚糖微胶囊载药量；
图3为室温敞口、不避光放置14d的本发明制备的微胶囊和β-胡萝卜素的稳定性比较结果；
图4为玉米淀粉(A)、初包物(B)和壳聚糖-高直链玉米淀粉-β-胡萝卜素微胶囊(C)放大4000倍微观结构图；
图5为β-胡萝卜素(图中标号1)、β-胡萝卜素-玉米淀粉微胶囊(图中标号2)、β-胡萝卜素-玉米淀粉-壳聚糖微胶囊(图中标号3)放置一定时间后的水分散稳定性结果图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，下面结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用于解释本发明，并不用于限定本发明。
对比例1、
准确称取0.06g玉米淀粉(直链淀粉含量20-25％)，溶解于2mL蒸馏水后，在温度为65℃，250r/min的水浴摇床保温1h，滴加2mL 0.3mg/mLβ-胡萝卜素无水乙醇溶液，保温1h，冷却至室温，离心去上清，无水乙醇洗涤，低温烘干即得β-胡萝卜素-淀粉微胶囊粉末，向其添加5mL 0.3％壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。用丙酮-石油醚(1：1)萃取微胶囊中β-胡萝卜素，在450nm测吸光度，计算其含量。
对比例2、
准确称取0.06g玉米淀粉(直链淀粉1-5％)，溶解于2mL蒸馏水后在温度为65℃，250r/min水浴摇床中保温1h后，滴加2mL 0.3mg/mL的β-胡萝卜素无水乙醇溶液，保温1h，冷却至室温后离心去上清，无水乙醇洗涤，低温烘干即得β-胡萝卜素-淀粉微胶囊粉末，向其添加5mL 0.3％壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。用丙酮-石油醚(1：1)萃取微胶囊中β-胡萝卜素，在450nm测吸光度，计算其含量。
对比例3、
准确称取0.06g玉米淀粉(直链淀粉含量55-75％)，溶解于2mL蒸馏水后在温度为65℃，250r/min的水浴摇床中保温1h后，滴加2mL 0.3mg/mL的β-胡萝卜素无水乙醇溶液，保温1h，冷却至室温后离心去上清，无水乙醇洗涤，低温烘干即得β-胡萝卜素微胶囊粉末，向其添加5mL 0.3％壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。用丙酮-石油醚(1：1)萃取微胶囊中β-胡萝卜素，在450nm测吸光度，计算其含量。
实施例1、
准确称取0.06g玉米淀粉(直链淀粉20-25％)溶解于2mL氢氧化钠溶液后在温度为65℃，250r/min的水浴摇床中保温1h后，滴加2mL 0.3mg/mL的β-胡萝卜素无水乙醇溶液，保温1h，用盐酸调节pH为中性，冷却至室温离心去上清，无水乙醇洗涤，低温烘干即得β-胡萝卜素微胶囊粉末，向其添加5mL0.3％壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。用丙酮-石油醚(1：1)萃取微胶囊中β-胡萝卜素，测定吸光度，计算其含量。
实施例2、
准确称取0.06g玉米淀粉(直链淀粉含量1-5％)溶解于2mL氢氧化钠溶液后在温度为65℃转速250r/min的水浴摇床中保温1h后，滴加2mL0.3mg/mL的β-胡萝卜素无水乙醇溶液，保温1h，用盐酸调节pH为中性，冷却至室温离心去上清，无水乙醇洗涤，低温烘干即得β-胡萝卜素微胶囊粉末，向其添加5mL 0.3％壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。用丙酮-石油醚(1：1)萃取微胶囊中β-胡萝卜素，测定吸光度，计算其含量。
实施例3、
准确称取0.06g玉米淀粉(直链淀粉55-75％)溶解于2mL氢氧化钠溶液后在温度为65℃转速250r/min的水浴摇床中保温1h后，滴加2mL 0.3mg/mL的β-胡萝卜素无水乙醇溶液，保温1h，用盐酸调节pH为中性，冷却至室温离心去上清，无水乙醇洗涤，低温烘干即得β-胡萝卜素微胶囊粉末，向其添加5mL0.3％壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。用丙酮-石油醚(1：1)萃取微胶囊中β-胡萝卜素，测定吸光度，计算其含量。
参考图1，为β-胡萝卜素在酸性环境、中性环境和碱性环境条件下稳定性结果图，通过静置2h，测定吸光度，计算保留率，可知β-胡萝卜素在中性环境和碱性环境都能保持良好的稳定性。
参考图2，为对比例1、对比例2、对比例3、实施例1、实施例2、实施例3中计算出的不同方法制备的β-胡萝卜素-淀粉-壳聚糖微胶囊中的β-胡萝卜素的含量，可以知道，实施例3制备的β-胡萝卜素-淀粉-壳聚糖微胶囊中的β-胡萝卜素的含量最高，即碱性条件下、淀粉中直链淀粉含量在55-75％范围内。因此选择碱性条件。
参考图3，为室温敞口、不避光放置14d的本发明实施例3制备的微胶囊和β-胡萝卜素的稳定性比较结果，可以知道，本发明制备的微胶囊中β-胡萝卜素稳定性较高，有良好的保留率。
参考图4，为玉米淀粉(A)、初包物(B)和壳聚糖-高直链玉米淀粉-β-胡萝卜素微胶囊(C)放大4000倍微观结构图，C图中，外层类薄膜结构为壳聚糖，通过3个图对比可知，本发明提供的方法对淀粉结构的损伤很小，淀粉颗粒完整性强。
参考图5，为β-胡萝卜素(1)、β-胡萝卜素-玉米淀粉微胶囊(2)、β-胡萝卜素-玉米淀粉-壳聚糖微胶囊(3)放置一定时间后的水分散稳定性结果图，可以知道，从0天到10天，每隔两天拍照记录，β-胡萝卜素-玉米淀粉-壳聚糖微胶囊保持良好的水分散性。
最后，需要注意的是，以上列举的仅是本发明的具体实施例，显然，本发明不仅限于以上实施例子，还可以有许多变形。本领域的科研人员从本发明公开的内容直接或间接联想到的所有形变，均应认为是本发明的保护范围。
Claims (8)
1.一种β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，包括如下步骤：
1)β-胡萝卜素分散液制备：将β-胡萝卜素分散于醇中，混合均匀；
2)淀粉乳制备：将淀粉分散在碱性溶液中，搅拌均匀，低温振荡一段时间；
3)复合：将步骤1)中得到的β-胡萝卜素分散液滴加到步骤2)制备的淀粉乳中，搅拌均匀，保温；
4)调节步骤3)得到的复合液的pH，然后进行离心，洗涤，低温烘干，得初包物；
5)向步骤4)所得初包物添加壳聚糖溶液，充分混匀，真空冷冻干燥即得β-胡萝卜素-淀粉-壳聚糖微胶囊。
2.根据权利要求1所述的β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，所述步骤1)中，β-胡萝卜素分散液中β-胡萝卜素的浓度为0.1-0.5mg/mL，所述醇为乙醇。
3.根据权利要求1所述的β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，所述步骤2)中淀粉乳的浓度为1-5％，淀粉中直链淀粉的含量为55-75％，碱性溶液pH范围9-14，低温为45-75℃，振荡时间为10-60min，振荡培养速率为200-300r/min。
4.根据权利要求3所述的β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，所述步骤2)中，淀粉为玉米淀粉。
5.根据权利要求1所述的β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，所述步骤3)中持续保持所述步骤2)中的温度，保温时间为10-60min，同时振荡培养，速率为200-300r/min。
6.根据权利要求1所述的β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，所述步骤4)中，复合液的pH调节为中性，洗涤溶液为无水乙醇，洗涤次数2-5次，干燥温度为35-60℃，时间为6-12h。
7.根据权利要求1所述的β-胡萝卜素-淀粉-壳聚糖微胶囊的制备方法，其特征在于，所述步骤5)中，向0.05-0.08g的初包物中添加5-10mL壳聚糖溶液，壳聚糖溶液浓度为0.2-0.5％。
8.根据权利要求1或2或3或4或5或6或7提供的方法制备的β-胡萝卜素-淀粉-壳聚糖微胶囊。
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