CN107811298B - 一种水溶性营养素微胶囊及其制备方法 - Google Patents
一种水溶性营养素微胶囊及其制备方法 Download PDFInfo
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- CN107811298B CN107811298B CN201711249420.3A CN201711249420A CN107811298B CN 107811298 B CN107811298 B CN 107811298B CN 201711249420 A CN201711249420 A CN 201711249420A CN 107811298 B CN107811298 B CN 107811298B
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Abstract
本发明公开了一种水溶性营养素微胶囊,其中的水溶性活性成分部分或全部以水溶液形式存在,且活性成分的粒径很小,利于在生物体内释放、吸收。本发明中所述的水溶性营养素微胶囊以高熔点油脂和流散介质作为微胶囊的包埋壁材,相比传统的水溶性胶体,隔绝空气效果更好,且更能耐受高湿度环境、油脂环境和机械加工环境,极大提高了水溶性营养素的稳定性。本发明还涉及了该水溶性营养素微胶囊的制备方法。
Description
技术领域
本发明属于食品、保健品、动物饲料领域,具体涉及一种水溶性营养素微胶囊及其制备方法。
背景技术
本发明所述的水溶性营养素包括水溶性维生素,如维生素C、维生素B族等;矿物质盐,如Fe2+盐、碘酸盐等;氨基酸,如蛋氨酸等。
为了使水溶性营养素能稳定储藏、保持其生物活性或者改变其颜色、气味、口感等问题,本领域技术人员通常把其制备成微胶囊。微胶囊化的营养素,可将活跃的营养素保护起来,使其免受外界的湿度、氧气、光线等因素的影响,还能解决如Fe2+带来的颜色、口感等问题。同时,作为添加剂,微胶囊化的营养素还能避免与最终产品中的其它活性成分的接触,如碳水化合物、氨基酸等,可以有效减弱与其它活性成分的相互影响。同时,现有技术中,微胶囊化的水溶性营养素还存在稳定性、包埋率不高等问题。
如中国专利CN105852133A,其公开了一种B族维生素微胶囊,具体的将核黄素、硫胺素、叶酸和烟酰胺溶解,得到芯材溶液;再将所述芯材溶液加入到羧甲基纤维素溶液中,分散后得到微乳液;将所述微乳液加入到明胶溶液中,分散、均质后进行真空冷冻干燥,得到B族维生素微胶囊。该方法使用了水溶性胶体为壁材,在实际使用时遇到水环境会快速崩解溶出,不利用复合营养素产品的二次加工。
专利WO2005067730A1公开了一种包含硫酸盐颗粒的微胶囊,具体的,使硫酸盐颗粒分散在气态流体中,然后使用不同凝固点的油脂对其进行包埋。但是该方法所包埋的硫酸盐颗粒为粗颗粒形态,不利于生物体消化吸收;同时外围的油脂层在遇到油环境会迅速崩解溶出,不利于复合营养素产品的二次加工。
常见的制备水溶性营养素微胶囊的方法还有直接将活性水溶液制成乳液,再进行喷雾干燥的,如文献“微胶囊化硫酸亚铁的研究,邵士凤等,食品开发与机械,2008,NO.4,P99-102”。现有技术中,常规乳化、喷雾干燥或者上述专利文献中所报道的方法,水溶性营养素的包埋率都不高,通常在胶囊表面会有5~15%的残留(其中水溶性维生素通常会有8-15%的残留),这在复合营养素产品的二次加工时都是非常不利的。
发明内容
本发明的目的在于解决现有技术制备的水溶性营养素微胶囊稳定性不高且不利于复杂加工环境的问题,提供了一种高稳定性、高包埋率且适合不同加工环境的水溶性营养素微胶囊及其制备方法。
一种水溶性营养素微胶囊,包括芯材和包覆于芯材表面的壁材,以重量百分比计,组成为:
所述的高熔点油脂和流散介质分布于壁材中。
本发明中,所述的壁材中同时含有高熔点油脂和流散介质,两者有机结合,形成致密的保护层,在加工时不管是碰到油环境还是水环境,都能保持较好的稳定性,不容易发生崩解,便于加工。
其中,所述的高熔点油脂的凝固点大于40℃。
所述的抗氧化剂包括水溶性抗氧化剂和/或油溶性抗氧化剂,在微胶囊中,水溶性抗氧化剂主要分布于内部的芯材中,油溶性抗氧化剂主要分布于外部的壁材中,两者可以同时存在,也可以只含有一种。
乳化剂主要位于壁材中,残留水份主要位于芯材中,残留水分的存在可以提高生物利用度。
本发明还提供了该水溶性营养素微胶囊的制备方法,其过程是:将包含水溶性营养素、水溶性抗氧化剂的水相和包含油溶性抗氧化剂、乳化剂的熔融高熔点油脂油相进行乳化,得到的油包水型乳化液进行真空脱水,脱除大部分水分得到脱水油包水型乳化分散液;将上述脱水油包水型乳化分散液在布满流散介质的喷雾造粒冷却床中进行喷雾造粒,过筛,即得到水溶性营养素微胶囊。
本发明所述的水溶性营养素为维生素C、维生素B族、矿物质盐、水溶性氨基酸。所述的矿物质盐为作为标准GB2760和GB14880中规定的可用于食品添加剂的矿物质盐,可以为钙、钠、钾、铁、锌、亚铁、铜、铬、镁、锰的磷酸盐、乳酸盐、柠檬酸盐、葡萄糖酸盐、硫酸盐、焦磷酸盐、氯化盐、碳酸盐、碘化物、亚硒酸盐等。
上述的水溶性营养素优选为不稳定营养素,具体的可以为维生素C、维生素B1、维生素B2、维生素B6、叶酸、维生素B12、烟酸、L-硒-甲基硒代半胱氨酸、蛋氨酸、碘酸钠、亚硒酸钠、硫酸亚铁、富马来酸亚铁、葡萄糖酸亚铁、碘化亚铜中的一种或多种。
本发明所述的高熔点油脂为凝固点大于40℃的蜡、硬化油/脂肪、高级脂肪酸中的一种或多种,所述的高熔点油脂在室温(25℃左右)储存条件下为固体,作为本发明微胶囊的主要壁材成分,很好地保护了囊内活性成分的稳定性。
所述的蜡可以为动物蜡、植物蜡和合成蜡或者化学改性的动物蜡、植物蜡,例如食品级石蜡、微晶蜡、蜂蜡、小烛树蜡、棕榈蜡、褐煤酸酯蜡、鲸蜡、羊毛蜡、萨索尔蜡、日本蜡等。
所述的硬化油/脂肪可以为所述油相中使用的油脂,例如氢化棉籽油和氢化大豆油等。
所述的高级脂肪酸为C16-C24的饱和或者不饱和的脂肪酸,例如软脂酸、珠光脂酸、硬脂酸、花生酸、山嵛酸等。
本发明所述的抗氧化剂为生育酚、生育酚棕榈酸酯、异抗坏血酸、异抗坏血酸钠、L-抗坏血酸-6-棕榈酸酯、没食子酸丙酯、BHA、BHT、TBHQ、茶多酚、茶多酚棕榈酸酯、硫代二丙酸二月桂酯、硫辛酸中的一种或多种。作为优选的,所述的抗氧化剂为生育酚、生育酚棕榈酸酯、茶多酚棕榈酸酯、异抗坏血酸、异抗坏血酸钠、L-抗坏血酸-6-棕榈酸酯、硫辛酸中的一种或多种。
本发明所述的乳化剂为脂肪酸蔗糖酯、维生素E聚乙二醇琥珀酸酯、吐温、司盘、脂肪酸甘油酯、卵磷脂中的一种或多种。
所述的流散介质为淀粉、二氧化硅、碳酸钙、磷酸钙、磷酸氢钙中的一种或多种。
所述的淀粉为马铃薯淀粉、玉米淀粉、糯玉米淀粉、小麦淀粉、大麦淀粉、裸麦淀粉、稻米淀粉、高粱淀粉、甘薯淀粉、木薯淀粉、红薯淀粉或豆类淀粉中的一种或多种。
本发明还提供了一种水溶性营养素微胶囊的制备方法,具体地包括如下步骤:
1)将水溶性营养素和水溶性抗氧化剂溶于水中配成水相;
2)将油溶性抗氧化剂、乳化剂与熔融高熔点油脂混合得到油相;
3)将步骤1)得到的水相和步骤2)得到的油相进行乳化得到油包水型乳化液;
4)将步骤3)得到的油包水型乳化液进行真空脱水,脱除大部分水分得到脱水油包水型乳化分散液;
5)将步骤4)得到的脱水油包水型乳化分散液在布满流散介质的喷雾造粒冷却床中进行喷雾造粒,过筛,即得到水溶性营养素微胶囊。
上述制备方法可在氮气保护下进行。使用氮气保护,可以排除环境中氧对营养素的影响,保证在微胶囊制备过程中营养素的稳定性。
上述步骤1)中所用的水可预先进行脱氧处理,进一步排除环境中氧的影响。
上述步骤3)中所述的乳化方法为高速剪切、微射流、超重力、空化乳化等。
上述步骤4)中所述的真空脱水过程在高熔点油脂熔融温度以上,真空度为-0.05MPa~-0.09MPa条件下进行。特别的是,在高速剪切条件下,可以将步骤3)和步骤4)在同一个装置中进行,也就是在同一装置中进行乳化和脱水。
上述步骤4)中所述的真空脱水过程可通过控制真空度和温度来控制所需脱除水分的量,同时可以通过计量脱出水分的量来确定乳化液中剩余的水分量。作为优选的,上述步骤4)中脱除体系中的水分至体系中水分重量占比为0.1~10%。作为优选的,上述步骤4)中所述的真空脱水过程在刮膜蒸发器中进行。
上述步骤5)中所述的喷雾造粒在高熔点油脂的凝固点温度下进行。此时,高熔点油脂会发生自凝固,形成由油脂为壁材的微胶囊。在油脂凝固的同时,微胶囊表面会吸附流散介质,形成致密的油脂层和流散介质层,从而保证微胶囊中水溶性营养素的稳定性。
同现有技术相比,本发明的有益效果体现在:
1)本发明以高熔点油脂和流散介质作为微胶囊的包埋壁材,相比传统的水溶性胶体,隔绝空气效果更好,且更能耐受高湿度环境、油脂环境和机械加工环境,极大提高了水溶性营养素的稳定性;
2)本发明所述的水溶性营养素微胶囊中的水溶性活性成分部分或全部以水溶液形式存在,且活性成分的粒径很小,更利于在生物体内释放、吸收;
3)本发明所述的水溶性营养素微胶囊制备工艺简单,由于不需要完全脱除水分,使其能耗较传统工艺更低。
具体实施方式
以下采用具体实施例的方式进一步详细地说明本发明,然而,本发明不限于以下所述的实施例。
实施例1
维生素B1微胶囊的制备
1)将15Kg维生素B1溶于50Kg水中配成水相;
2)将2Kg生育酚、7Kg司盘-40、1Kg吐温-40和熔融的55Kg棕榈蜡(熔点为81℃)混合均匀,得到油相;
3)将步骤1)得到的水相和步骤2)得到的油相打到微射流乳化器中进行连续乳化,得到油包水型乳化液;
4)将步骤3)得到的油包水型乳化液打到刮膜蒸发器中,在85℃、-0.05MPa条件下进行真空连续刮膜脱水,得到脱水油包水型乳化分散液。脱水毕,通过计量脱出水的量,可计算得到乳化液中剩余6Kg的水;
5)将步骤4)得到的脱水油包水型乳化液在布满马铃薯淀粉颗粒的喷雾造粒冷却塔中进行喷雾造粒(喷雾造粒冷却塔内温度为20℃),过筛,即得到维生素B1微胶囊。
检测分析得到最终维生素B1微胶囊重量组成如下:
维生素B1 14.15%,棕榈蜡51.89%,生育酚1.89%,司盘-40 6.61%,吐温-400.94%,水分5.66%,马铃薯淀粉18.86%。
实施例2
叶酸微胶囊的制备
1)将20kg叶酸溶于35kg水中配成水相;
2)将3Kg茶多酚棕榈酸酯、1Kg吐温-60、4Kg司盘-60和熔融的60Kg食品级石蜡(熔点为48℃)混合溶解,得到油相;
3)将步骤1)得到的水相和步骤2)所得到的油相同时通入超重力旋转床,在55℃下进行超重力乳化,在超重力旋转床出口处得到油包水型乳化液;
4)将步骤3)得到的油包水型乳化液打到刮膜蒸发器中,在55℃、-0.09MPa条件下进行连续真空刮膜脱水,得到脱水油包水型乳化分散液。脱水毕,通过计量脱出的水量,可以计算得到乳化液中剩余的水量为10.5Kg;
5)将步骤4)得到的脱水油包水型乳化分散液在布满玉米淀粉和二氧化硅颗粒的喷雾造粒冷却塔中进行喷雾造粒(喷雾造粒冷却塔内温度为15℃),过筛,即得到叶酸微胶囊。
检测分析得到最终叶酸微胶囊重量组成如下:
叶酸17.17%,食品级石蜡51.50%,茶多酚棕榈酸酯2.58%,吐温-600.86%,司盘-60 3.43%,水分9.01%,玉米淀粉14.12%,二氧化硅1.33%。
实施例3
L-硒-甲基硒代半胱氨酸微胶囊的制备
1)将30KgL-硒-甲基硒代半胱氨酸、1Kg异抗坏血酸钠溶于40Kg水中配成水相;
2)将3Kg维生素E棕榈酸酯、10Kg司盘-20、熔融的40kg珠光脂酸(熔点为60℃)和30kg硬酯酸(熔点为70℃)混合均匀,得到油相;
3)将步骤1)得到的水相和步骤2)所得到的油相同时通入多级串联空化乳化器中进行乳化(空化乳化器中温度为75℃,压力为400Mpa),在出口处得到油包水型乳化液;
4)将步骤3)得到的油包水型乳化液打到刮膜蒸发器中,在80℃、-0.06MPa条件下进行连续真空刮膜脱水。脱水毕,通过计量脱出的水量,可以计算得到乳化液中剩余7.5Kg的水;
5)将步骤4)得到的乳化液在布满二氧化硅颗粒的喷雾造粒冷却塔中进行喷雾造粒(喷雾造粒冷却塔内温度为25℃),过筛,即得到L-硒-甲基硒代半胱氨酸微胶囊。
检测分析得到最终L-硒-甲基硒代半胱氨酸微胶囊重量组成如下:
L-硒-甲基硒代半胱氨酸21.98%,珠光脂酸29.30%,硬脂酸21.98%,异抗坏血酸钠0.73%,维生素E棕榈酸酯2.20%,司盘-20 7.33%,水分5.49%,二氧化硅11.00%。
实施例4
硫酸亚铁微胶囊的制备
1)将150g硫酸亚铁、20g硫辛酸溶于300g水中配成水相;
2)将10g维生素E棕榈酸酯、60g三聚甘油单硬脂酸脂和600g熔融山嵛酸(熔点为76℃)加入乳化釜中搅拌均匀,在80℃、10000rpm剪切转速下,将上述步骤1)的水相通过滴加方式加入乳化釜中,加毕继续剪切乳化30分钟,得到油包水型乳化液;
3)将步骤2)得到的油包水型乳化液在80℃、3000rpm剪切速度下,逐渐拉真空开始脱水,直到真空度达到-0.06MPa,停止脱水,得到脱水油包水乳化分散液。通过计量脱出的水量,可以计算得到此油包水型乳化分散液中剩余110g的水;
4)将步骤3)得到的油包水型乳化分散液在布满磷酸钙颗粒的喷雾造粒冷却塔中进行喷雾造粒(喷雾造粒冷却塔内温度为20℃),过筛,即得到硫酸亚铁微胶囊。
检测分析得到最终硫酸亚铁微胶囊重量组成如下:
硫酸亚铁13.02%,山嵛酸52.06%,硫辛酸1.74%,维生素E棕榈酸酯0.87%,三聚甘油单硬脂酸脂5.20%,水分9.76%,磷酸钙17.35%。
实施例5
维生素B1微胶囊的制备
1)将150g维生素B1溶于500g水中配成水相;
2)将20g生育酚、50g司盘-60、30g卵磷脂、450g熔融棕榈蜡(熔点为81℃)和100g熔融微晶蜡(熔点为88℃)加入乳化釜中,搅拌均匀后,在90℃、10000rpm剪切转速下,将上述步骤1)的水相通过滴加方式加入乳化釜中,加毕继续剪切乳化30分钟,得到油包水型乳化液;
3)将步骤2)得到的油包水型乳化液在90℃、3000rpm剪切速度下,逐渐拉真空开始脱水,直到真空度达到-0.05MPa,停止脱水,得到脱水油包水乳化分散液。通过计量脱出的水量,可以计算得到此油包水型乳化分散液中剩余55g的水;
4)将步骤3)得到的脱水油包水乳化分散液在布满马铃薯淀粉颗粒的喷雾造粒冷却塔中进行喷雾造粒(喷雾造粒冷却塔内温度为20℃),过筛,即得到维生素B1微胶囊。
检测分析得到最终维生素B1微胶囊重量组成如下:
维生素B1 14.22%,棕榈蜡42.65%,微晶蜡9.48%,生育酚1.90%,司盘-604.74%,卵磷脂2.84%,水分5.21%,马铃薯淀粉18.96%。
实施例6-10
根据实施例1的制备方法,调整水溶性营养素、抗氧化剂、高熔点油脂、乳化剂、乳化液中的水、流散助剂等的质量,制备得到的微胶囊具体组成如下表1所示。
表1
对比例1
维生素B1微胶囊的制备
80℃下,将150g维生素B1、20g生育酚和630g辛烯基琥珀酸淀粉酯溶于1000g水,在10000rpm剪切转速下进行乳化1小时,得到水包油型乳化液。
将上述乳化液喷雾到布满马铃薯淀粉颗粒的流化床中吸附造粒,得到表面由淀粉包覆的微胶囊。在60℃下进行流态化干燥,过筛,得到维生素B1微胶囊。
检测分析得到最终维生素B1微胶囊重量组成如下:
维生素B1 14.24%,辛烯基琥珀酸淀粉酯59.80%,生育酚1.90%,水分4.13%,马铃薯淀粉19.93%。
稳定性对比
在复合营养素产品加工过程中,一般会将不同的营养素微胶囊加水混合后,进行二次加工。为了更好地对比本发明的效果,取实施例1、实施例5和对比例1制备得到的维生素B1微胶囊各100g,分别在微胶囊表面喷水10g,然后在不同温度条件下加热3小时,比较维生素B1含量的变化情况(加热后产品维生素B1含量与加热前产品维生素B1含量的比值即为表中所示的含量保留率)。结果如下表2所示。
表2不同实施例的稳定性数据
由表2的结果可知,当采用高熔点油脂作为原料,将水溶性营养素形成油包水乳化分散液后,再进行制粒,可以有效地提高营养素微胶囊的稳定性。
Claims (10)
1.一种水溶性营养素微胶囊,包括芯材和包覆于芯材表面的壁材,其特征在于,以重量百分比计,组成为:
水溶性营养素 1-40%
高熔点油脂 50-90%
抗氧化剂 1-3%
乳化剂 1-10%
残留水份 0.1-10%
流散介质 6-20%
所述的高熔点油脂和流散介质分布于壁材中;
残留水份主要位于芯材中;
所述的高熔点油脂为凝固点大于40℃的蜡、硬化油/脂肪、高级脂肪酸中的一种或多种;
所述的流散介质为淀粉、二氧化硅、碳酸钙、磷酸钙、磷酸氢钙中的一种或多种;
所述的水溶性营养素微胶囊的制备方法,步骤如下:
(1)将包含水溶性营养素、水溶性抗氧化剂的水相和包含油溶性抗氧化剂、乳化剂的熔融高熔点油脂油相进行乳化,得到的油包水型乳化液;
(2)将步骤(1)得到的油包水型乳化液进行真空脱水,脱除大部分水分得到脱水油包水型乳化分散液;
(3)将上述脱水油包水型乳化分散液在布满流散介质的喷雾造粒冷却床中进行喷雾造粒,过筛,即得到水溶性营养素微胶囊。
2.根据权利要求1所述的水溶性营养素微胶囊,其特征在于,所述的水溶性营养素为维生素C、维生素B族、矿物质盐、水溶性氨基酸中的一种或多种。
3.根据权利要求2所述的水溶性营养素微胶囊,其特征在于,所述的水溶性营养素为维生素C、维生素B1、维生素B2、维生素B6、叶酸、维生素B12、烟酸、L-硒-甲基硒代半胱氨酸、蛋氨酸、碘酸钠、亚硒酸钠、硫酸亚铁、富马来酸亚铁、葡萄糖酸亚铁、碘化亚铜中的一种或多种。
4.根据权利要求1所述的水溶性营养素微胶囊,其特征在于,所述的抗氧化剂为生育酚、异抗坏血酸、异抗坏血酸钠、L-抗坏血酸-6-棕榈酸酯、没食子酸丙酯、BHA、BHT、TBHQ、茶多酚、茶多酚棕榈酸酯、硫代二丙酸二月桂酯、硫辛酸中的一种或多种。
5.根据权利要求1所述的水溶性营养素微胶囊,其特征在于,所述的乳化剂为脂肪酸蔗糖酯、维生素E聚乙二醇琥珀酸酯、吐温、司盘、脂肪酸甘油酯、卵磷脂中的一种或多种。
6.根据权利要求1所述的水溶性营养素微胶囊,其特征在于,所述的淀粉为马铃薯淀粉、玉米淀粉、糯玉米淀粉、小麦淀粉、大麦淀粉、裸麦淀粉、稻米淀粉、高粱淀粉、甘薯淀粉、木薯淀粉、红薯淀粉、豆类淀粉中的一种或多种。
7.一种如权利要求1~6任一项所述的水溶性营养素微胶囊的制备方法,其特征在于,步骤如下:
(1)将包含水溶性营养素、水溶性抗氧化剂的水相和包含油溶性抗氧化剂、乳化剂的熔融高熔点油脂油相进行乳化,得到的油包水型乳化液;
(2)将步骤(1)得到的油包水型乳化液进行真空脱水,脱除大部分水分得到脱水油包水型乳化分散液;
(3)将上述脱水油包水型乳化分散液在布满流散介质的喷雾造粒冷却床中进行喷雾造粒,过筛,即得到水溶性营养素微胶囊。
8.根据权利要求7所述的水溶性营养素微胶囊的制备方法,其特征在于,步骤(1)中,所述的乳化方法为高速剪切、微射流、超重力、空化乳化中的一种,乳化过程在高熔点油脂熔点温度以上进行。
9.根据权利要求7所述的水溶性营养素微胶囊的制备方法,其特征在于,步骤(2)中,所述的真空脱水过程在高熔点油脂熔点温度以上,真空度为-0.05MPa~-0.09MPa条件下进行。
10.根据权利要求7所述的水溶性营养素微胶囊的制备方法,其特征在于,所述的水溶性营养素微胶囊的制备在氮气保护下进行,所用的水预先经过脱氧处理。
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