CN107467672A - 一种亚铁复合凝胶微球的制备方法 - Google Patents
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Abstract
本发明公开了一种亚铁复合凝胶微球的制备方法，属于保健品和药物制剂领域，该方法首先采用内源乳化法制备海藻酸钠‑铁凝胶，然后再用酪蛋白酸钠对凝胶微球进行二次包埋。本发明制备的亚铁复合凝胶微球粒径均匀，分散性好，不易发生团聚粘连，平均粒径小于100μm，在酸碱条件下性质稳定，不易被氧化生成三价铁，添加到豆浆等食品中具有良好的外观和口感，而且感官特性更加稳定，本发明还能降低豆浆等食品在储存期内的酸价和过氧化值，防止产品酸败变质。
Description
技术领域
本发明涉及亚铁凝胶微球的制备方法，属于保健品和药物制剂领域。
背景技术
亚铁常作为优质的补铁剂用于药品、保健品，但由于亚铁易被氧化成三价铁，因此会对药品或保健食品的色泽、口感和稳定性等产生不利的影响。另外，有些亚铁如富马酸亚铁/琥珀酸亚铁难溶于水，易沉降，作为铁强化剂添加到食品中有令人不适的铁腥味，消费者依从性差，严重影响其生物吸收效率。
凝胶微球是常用的药物载体，通常是采用挤压法将海藻酸钠溶液逐滴挤入CaCl2溶液中，生成粒径为1-2mm的凝胶颗粒。乳化凝胶法是制备分散均一的微米级凝胶微粒的有效方法，如采用外源乳化法将CaCl2加入到大豆油-海藻酸钠油包水乳液中制备凝胶微粒，其凝胶球粒径在10-150μm范围内，但该方法容易破坏乳液的平衡体系，使乳滴聚结从而形成大块凝胶。为了克服挤压法制备凝胶球粒径过大，以及外源乳化法中氯化钙加入引起的乳滴聚结等缺陷，一般采用内源乳化法制备分散性好的微米级凝胶微粒。但是内源乳化法通常是应用于难溶性钙的包埋，目前，该法尚未应用于对亚铁进行包埋。
发明内容
本发明的目的是提供一种亚铁复合凝胶微球的制备方法，首先采用内源乳化法制备海藻酸钠-铁凝胶，然后再用酪蛋白酸钠对凝胶微球进行二次包埋，从而提高亚铁的稳定性并改善其口感。
上述目的是通过以下技术方案实现的：
一种亚铁复合凝胶微球的制备方法，包括以下步骤：
1)取重量浓度为0.5～3％海藻酸钠水溶液，加入亚铁化合物，搅拌混匀，制成悬浮液，所述海藻酸钠水溶液与亚铁化合物的重量比为3～10∶1；
2)向悬浮液中加入3～8倍体积的中链甘油三酯或者植物油，高速均质5～10min，同时缓慢滴加酸，直至形成凝胶颗粒，然后离心弃除油层；
3)向分离的凝胶颗粒中加入1～5倍重量的酪蛋白酸钠水溶液，所述酪蛋白酸钠水溶液的重量浓度为1～4％，高速均质5～10min，然后离心，将沉淀加少量水分散稀释后喷雾干燥，即得。
优选地，所述亚铁化合物可溶于酸，难溶或微溶于水，优选富马酸亚铁、琥珀酸亚铁。
优选地，所述酸为盐酸、磷酸、醋酸、柠檬酸、苹果酸、富马酸、酒石酸中的一种或多种。
优选地，所述植物油为大豆油。
优选地，步骤1)中，所述海藻酸钠水溶液的重量浓度为1％，所述海藻酸钠水溶液与亚铁化合物的重量比为6∶1。
优选地，步骤2)中，所述中链甘油三酯或者植物油的体积是悬浮液的5倍。
优选地，步骤3)中，所述酪蛋白酸钠水溶液的重量是凝胶颗粒的3倍，所述酪蛋白酸钠水溶液的重量浓度为1.5％。
本发明首先利用海藻酸钠能与二价离子发生交联生成凝胶的特性，通过加酸使乳滴水相中荷载的难溶性亚铁化合物离解生成二价铁离子，直接利用二价铁离子与海藻酸钠原位置换聚合形成海藻酸钠-铁凝胶，从而减少外源钙的引入，提高了铁的荷载率。
此外，本发明还利用酪蛋白酸钠在酸性环境中(约pH4.0)带正电，其可通过静电作用吸附在海藻酸钠-铁凝胶球表面，实现了对凝胶微球的二次包埋，可以进一步提高矿物质铁的荷载稳定性，并改善其外观和气味。酪蛋白酸钠具有良好的乳化活性和稳定性，可使富铁凝胶微粒在食品中均匀分散。另外，酪蛋白酸钠的引入还可增加凝胶微粒的蛋白质含量，提高其营养价值。
本发明制备的亚铁复合凝胶微球粒径均匀，分散性好，不易发生团聚粘连，平均粒径小于100μm；在酸碱条件下性质稳定，不易被氧化生成三价铁；添加到豆浆等食品中具有良好的外观和口感，而且感官特性更加稳定；本发明还能降低豆浆等食品在储存期内的酸价和过氧化值，防止产品酸败变质。
附图说明
图1是本发明复合凝胶微球的显微镜镜检照片。
图2是本发明复合凝胶微球的粒径分布图。
图3是富马酸亚铁在水、Vc、酸和碱环境中的稳定性对比(从左至右溶剂依次为水、Vc、HCl和NaOH)。
图4是富马酸亚铁凝胶微球在水、Vc、酸和碱环境中的稳定性对比(从左至右依次为富马酸亚铁溶于水，富马酸亚铁凝胶微球溶于水、Vc、HCl和NaOH)。
具体实施方式
下面通过实施例对本发明进行详细地说明。
实施例1
1)取重量浓度为1％的海藻酸钠水溶液，加入富马酸亚铁，搅拌混匀，制成悬浮液，所述海藻酸钠水溶液与富马酸亚铁的重量比为6∶1；
2)向悬浮液中加入5倍体积的大豆油，8000rpm转速下高速均质10min，同时缓慢滴加醋酸，直至形成凝胶颗粒，然后离心弃除油层；
3)向分离的凝胶颗粒中加入3倍重量的酪蛋白酸钠水溶液，所述酪蛋白酸钠水溶液的重量浓度为1.5％，高速均质10min，然后离心，将沉淀加少量水分散稀释后喷雾干燥，即得。
实施例2
1)取重量浓度为2％的海藻酸钠水溶液，加入富马酸亚铁，搅拌混匀，制成悬浮液，所述海藻酸钠水溶液与富马酸亚铁的重量比为4∶1；
2)向悬浮液中加入3倍体积的中链甘油三酯，高速均质5min，同时缓慢滴加稀盐酸，直至形成凝胶颗粒，然后离心弃除油层；
3)向分离的凝胶颗粒中加入1倍重量的酪蛋白酸钠水溶液，所述酪蛋白酸钠水溶液的重量浓度为4％，高速均质5min，然后离心，将沉淀加少量水分散稀释后喷雾干燥，即得。
实施例3
1)取重量浓度为0.5％的海藻酸钠水溶液，加入琥珀酸亚铁，搅拌混匀，制成悬浮液，所述海藻酸钠水溶液与琥珀酸亚铁的重量比为8∶1；
2)向悬浮液中加入8倍体积的中链甘油三酯，高速均质10min，同时缓慢滴加磷酸，直至形成凝胶颗粒，然后离心弃除油层；
3)向分离的凝胶颗粒中加入5倍重量的酪蛋白酸钠水溶液，所述酪蛋白酸钠水溶液的重量浓度为1％，高速均质10min，然后离心，将沉淀加少量水分散稀释后喷雾干燥，即得。
试验例
1.粒径形态与分布
以富马酸亚铁为例，将制得的复合凝胶微球置于4倍显微镜下观察，结果如图1所示，可见微球形态均匀稳定呈球形，分散性较好，边缘清晰无团聚粘连表现。
图2是微球的粒径分布图，相同均质条件下，本发明制得的微球平均粒径小于100μm。
2.酸碱稳定性
观察富马酸亚铁在水、Vc、酸和碱环境中的稳定性，分别在水、Vc、HCl、NaOH中加入4％富马酸亚铁，静置24h前后效果如图3，富马酸亚铁在水中无明显变化，会快速沉降；加入Vc、HCl和NaOH中均有明显的颜色变化，说明富马酸亚铁在Vc和酸碱环境中都极不稳定。
而本发明制得的复合凝胶微球在水、Vc、酸和碱环境中的稳定性如图4所示，可以看到，微球溶于水中呈均一的乳白色悬浊液，无原有的红褐色沉淀，加入Vc、HCl和NaOH后依然较为稳定，未产生明显的颜色变化，说明富马酸亚铁经微囊化后明显改善了其酸碱稳定性。
3.对豆浆样本的感官和质量影响
含实施例1～3复合凝胶微球的豆浆粉样本：每份样品包含30mg(以铁含量计)复合凝胶微球、18g大豆粉。
含普通富马酸亚铁的豆浆粉样本：每份样品包含91.1mg富马酸亚铁(含铁30mg)、18g大豆粉，用作对比。
以上样品用聚乙烯塑料袋独立包装后置于40℃，湿度75％环境中加速观察三个月，每隔一段时间用50℃热水100mL进行冲调，观察其溶解状态，鉴定其滋气味。同时检测其酸价和过氧化值。
1)感官试验结果：添加实施例1～3复合凝胶微球的豆浆粉样本在加速60天内，冲调后为淡黄色液体，浓郁的豆浆香味，无异味，无铁腥味，无沉淀。而添加普通富马酸亚铁的豆浆粉样本在50天内冲调后为淡黄色液体，浓郁的豆浆香味，微弱的铁腥味，有明显的红褐色沉淀；在60天冲调后为淡黄色液体，明显的哈喇味，微弱的铁腥味，有明显的红褐色沉淀。表明本发明制得的豆浆粉感官稳定性更好，储存期更长。
2)酸价和过氧化值测定：对添加实施例1～3复合凝胶微球的豆浆粉样本和对比样本进行酸价和过氧化值测定，结果见表1。
表1豆浆粉样本的酸价和过氧化值测定
从以上结果可以看出，对比样本的酸价和过氧化值均比较高，说明该产品更容易酸败变质；而本发明样品在加速60天后，酸价和过氧化值仍比较稳定。
Claims (7)
1.一种亚铁复合凝胶微球的制备方法，其特征在于包括以下步骤：
1)取重量浓度为0.5～3％海藻酸钠水溶液，加入亚铁化合物，搅拌混匀，制成悬浮液，所述海藻酸钠水溶液与亚铁化合物的重量比为3～10∶1；
2)向悬浮液中加入3～8倍体积的中链甘油三酯或者植物油，高速均质5～10min，同时缓慢滴加酸，直至形成凝胶颗粒，然后离心弃除油层；
3)向分离的凝胶颗粒中加入1～5倍重量的酪蛋白酸钠水溶液，所述酪蛋白酸钠水溶液的重量浓度为1～4％，高速均质5～10min，然后离心，将沉淀加少量水分散稀释后喷雾干燥，即得。
2.如权利要求1所述亚铁复合凝胶微球的制备方法，其特征在于：所述亚铁化合物可溶于酸，难溶或微溶于水，优选富马酸亚铁或琥珀酸亚铁。
3.如权利要求1所述亚铁复合凝胶微球的制备方法，其特征在于：所述酸为盐酸、磷酸、醋酸、柠檬酸、苹果酸、富马酸、酒石酸中的一种或多种。
4.如权利要求1所述亚铁凝胶微球的制备方法，其特征在于：所述植物油为大豆油。
5.如权利要求1所述亚铁复合凝胶微球的制备方法，其特征在于：步骤1)中，所述海藻酸钠水溶液的重量浓度为1％，所述海藻酸钠水溶液与亚铁化合物的重量比为6∶1。
6.如权利要求1所述亚铁复合凝胶微球的制备方法，其特征在于：步骤2)中，所述中链甘油三酯或者植物油的体积是悬浮液的5倍。
7.如权利要求1所述亚铁复合凝胶微球的制备方法，其特征在于：步骤3)中，所述酪蛋白酸钠水溶液的重量是凝胶颗粒的3倍，所述酪蛋白酸钠水溶液的重量浓度为1.5％。
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