CN113368046B - 油包水包油纳米乳液及其制备方法 - Google Patents
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Abstract
本发明公开了油包水包油纳米乳液的制备方法。本发明所提供的油包水包油纳米乳液的制备方法,包括如下步骤:(1)将乙酸异戊酯、乙醇和油相混合制得混合油相,再向所述混合油相中加入EL‑35或Tween 80,进行搅拌,得到液体A;(2)在搅拌条件下向所述步骤(1)得到的液体A中逐滴加入水,制得水包油纳米乳液;(3)将所述步骤(2)制得的水包油纳米乳液和乙醇混合,制得混合水相,再向所述混合水相中加入EL‑35,进行搅拌,得到液体B;(4)在搅拌条件下向所述步骤(3)得到的液体B中逐滴加入乙酸异戊酯,制得油包水包油型纳米乳液。本发明的方法能制备出外观透明、性质稳定的油包水包油型纳米乳液。
Description
技术领域
本发明涉及纳米乳液的制备方法,特别地涉及油包水包油纳米乳液及其制备方法。
背景技术
纳米乳液是由水、油和双亲分子按照一定比例混合形成的一种热力学稳定的分散体系,可用以包埋亲脂性的活性成分,在食品、制药、农业和其他工业化学品领域被广泛应用。纳米乳液与乳液相比,分散相质点小且均匀,外观呈透明或半透明状。传统乳液制备过程中需要进行高速搅拌、高压均质、超声等操作,能量利用效率低下,且制备出的多重纳米乳液粒径过大,稳定性差。而低能乳化法利用体系组分释放的化学能制备乳液,由于较少的能量输入、简单的仪器装置和低廉的成本等优点,在近年来引起了广泛关注。
油包水包油纳米乳液通常使用两步乳化法来制备,第一步利用亲水性乳化剂制备水包油型纳米乳液,在第二步中将其作为水相,混合亲油性乳化剂后滴加油相,最终获得油包水包油型纳米乳液。由于该纳米乳液中存在两种性质截然相反的界面,因此,需要引入两种不同的乳化剂分别稳定水包油界面和油包水界面,两个界面上的乳化剂分子处于动态平衡,可能发生迁移从而影响多重结构的形成和活性成分的包覆。
目前,对于油包水包油的研究尚且停留在微米级别,温度控制程序复杂,需要大量的能量输入,还未发现关于低能乳化法制备油包水包油型纳米乳液的相关报道。
发明内容
有鉴于此,本发明的主要目的是提供油包水包油纳米乳液及其制备方法。
本发明所提供的油包水包油纳米乳液的制备方法,包括如下步骤:
(1)将乙酸异戊酯、乙醇和油相混合制得混合油相,再向所述混合油相中加入EL-35或Tween 80,进行搅拌,得到液体A;
(2)在搅拌条件下向所述步骤(1)得到的液体A中逐滴加入水,制得水包油纳米乳液;
(3)将所述步骤(2)制得的水包油纳米乳液和乙醇混合,制得混合水相,再向所述混合水相中加入EL-35,进行搅拌,得到液体B;
(4)在搅拌条件下向所述步骤(3)得到的液体B中逐滴加入乙酸异戊酯,制得油包水包油型纳米乳液。
优选地,所述步骤(1)的油相包括油脂或脂肪酸;
进一步优选地,所述油脂为牡丹籽油;所述脂肪酸为含有质量浓度为60%α-亚麻酸的混合脂肪酸或纯度为99%的α-亚麻酸。
优选地,所述步骤(1)中所述乙酸异戊酯、乙醇和油相的质量比为8:1:1~2:2:1。
更优选地,所述步骤(1)中所述乙酸异戊酯、乙醇和油相的质量比为8:1:1~4:2:1。
在一些实施方式中,所述步骤(1)中所述乙酸异戊酯、乙醇和油相的质量比为8:1:1。
在另外一些实施方式中,所述步骤(1)中所述乙酸异戊酯、乙醇和油相的质量比为4:2:1。
还有一些实施方式中,所述步骤(1)中所述乙酸异戊酯、乙醇和油相的质量比为2:2:1。
乙酸异戊酯碳链较短,易于包埋且是牡丹籽油及脂肪酸的良好溶剂。乙醇为助表面活性剂,且为食品中安全性较高的允许添加的组分。
优选地,所述步骤(1)中加入EL-35或Tween 80的质量是所述混合油相质量的1.5倍~12倍。
更优选地,所述步骤(1)中加入EL-35或Tween 80的质量是所述混合油相质量的3倍~12倍。
EL-35或Tween 80均为食品中可添加的安全性高的乳化剂,同时含有疏水性基团和亲水性基团,且亲水亲油值(HLB)适合该体系。
优选地,所述步骤(2)中加入水的质量是所述液体A质量的1倍~10倍。
更优选地,所述步骤(2)中加入水的质量是所述液体A质量的3倍~10倍。
对制得均一、透明的水包油纳米乳液最关键的因素是加水量及加水速度。
优选地,所述步骤(3)中所述水包油纳米乳液和所述乙醇的质量比为1:1~8:1。
更优选地,所述步骤(3)中所述水包油纳米乳液和所述乙醇的质量比为4:1~8:1。
乙醇作为助表面活性剂,可以调整水的极性,改变表面活性剂的亲水亲油平衡值,参与形成胶束。
优选地,所述步骤(3)中加入EL-35的质量是所述混合水相质量的1.5倍~12倍。
更优选地,所述步骤(3)中加入EL-35的质量是所述混合水相质量的3倍~12倍。
EL-35是表面活性剂,具有亲水和亲油基团,能降低表面张力。
优选地,所述步骤(4)中加入乙酸异戊酯的质量是所述液体B质量的1倍~6倍。
乙酸异戊酯作为O/W/O纳米乳液的外油相,起到隔绝氧气的效果。
优选地,所述步骤(1)的搅拌是在温度为20℃~35℃、转速为300rpm~600rpm的条件下搅拌30min~60min;
优选地,所述步骤(2)的搅拌速度为300rpm~600rpm;
优选地,所述步骤(3)的搅拌是在温度为40℃~70℃、转速为300rpm~500rpm的条件下搅拌30min~40min;
优选地,所述步骤(4)的搅拌速度为300rpm~500rpm。
所述的方法制备得到的油包水包油纳米乳液也属于本发明的保护范围。
本发明使用单一的亲水性表面活性剂,通过温度控制实现乳化剂亲水性和疏水性和转化,避免了乳化剂的迁移造成的结构破坏问题,由此制备的纳米乳液稳定性高,同时具有纳米尺寸的粒径和良好的分散特性。本发明制备的具备油包水包油结构的纳米乳液可以同时递送水溶性和油溶性的活性成分,控制释放速度,特别是对内油相中的活性成分,能实现高效保护,例如α-亚麻酸,应用前景广阔。
在此基础上建立的多重纳米乳液体系凭借其独特的“两膜三相”多隔室结构,有效实现了药物释放、靶向递送和活性成分保护,例如α-亚麻酸等。与水包油纳米乳液和油包水纳米乳液相比,由于两层界面的形成,油包水包油纳米乳液为内油相提供了更为封闭的内环境,有效降低了外部环境因素(如氧气、温度、光等)对包埋物的影响,能有效控制释放和稳定脂溶性活性成分,例如α-亚麻酸。
本发明的优点是:
(1)本发明制备的食品级油包水包油纳米乳液外观澄清透明,具有纳米尺寸的分散粒径,储藏稳定性良好。
(2)本发明制备的油包水包油型纳米乳液能有效负载和保护不同溶解性的营养物质,降低外部环境对包埋物的影响。
(3)本发明采用单一的亲水性表面活性剂,所制得的油包水包油型纳米乳液结构稳定性高。
(4)本发明采用低能乳化法,无需大量能量输入,无需复杂设备处理,能量损耗低,符合节能环保理念。同时,本发明的方法无高温高压处理,简单易行,工艺效率高。
附图说明
为了说明而非限制的目的,现在将根据本发明的优选实施例、特别是参考附图来描述本发明,其中:
图1为在4℃条件下60%混合脂肪酸乙酸异戊酯溶液和60%混合脂肪酸O/W/O纳米乳液相对氧化稳定性测定结果图。
图2为在25℃条件下60%混合脂肪酸乙酸异戊酯溶液和60%混合脂肪酸O/W/O纳米乳液相对氧化稳定性测定结果图。
图3为在4℃条件下99%α-亚麻酸乙酸异戊酯溶液和99%α-亚麻酸O/W/O纳米乳液相对氧化稳定性测定结果图。
图4为在25℃条件下99%α-亚麻酸乙酸异戊酯溶液和99%α-亚麻酸O/W/O纳米乳液相对氧化稳定性测定结果图。
具体实施方式
EL-35是聚氧乙烯(35)蓖麻油的缩写;EL-35购自上海源叶生物科技有限公司,产品目录号S30627。
Tween是聚氧乙烯脱水山梨醇单油酸酯的缩写;Tween购自国药集团化学试剂有限公司,产品目录号30189828。
牡丹籽油购自晨光生物科技基团股份有限公司,产品目录号Q/HCG 0017S。
α-亚麻酸纯度为60%的混合脂肪酸:通过牡丹籽油皂化、冷冻结晶制得,具体制备方法参考专利文献CN110642711B。
纯度为99%的α-亚麻酸:是指混合脂肪酸中含有质量浓度为60%的α-亚麻酸,通过如下方法制备得到:牡丹籽油皂化水解得到混合脂肪酸,混合脂肪酸冷冻结晶得到质量百分比浓度为60-70%α-亚麻酸,然后柱层析得到高纯度99%左右α-亚麻酸。
以下结合附图和实施例对本发明作进一步的详细说明。下述是实施例中使用的原料,如无特殊说明,均是可以商业购买得到的。
实施例1、制备食用级油包水包油型纳米乳液
食用级油包水包油型纳米乳液的制备方法,包括如下步骤:
(1)按照质量比8:1:1,分别取80mg乙酸异戊酯、10mg乙醇和10mg牡丹籽油混合,制得混合油相,再加入混合油相质量1.5倍,即150mg EL-35或Tween 80混合于小烧杯中,加入转子,调整转速为300rpm,在温度为20℃条件下搅拌30min;
(2)保持300rpm的搅拌速度,逐滴加入水,加入水的质量为步骤(1)获得的液体总质量的1倍,即250mg,得到均一、透明的水包油微乳液;
(3)按照质量比8:1,称取80mg步骤(2)获得的水包油纳米乳液,与10mg乙醇混合,制得混合水相,再加入混合水相质量1.5倍,即135mg EL-35混合于小烧杯中,加入转子,调整转速为300rpm,在温度为40℃条件下搅拌30min;
(4)保持300rpm的搅拌速度,逐滴加入质量为步骤(3)获得的液体总质量1倍的乙酸异戊酯,即225mg,制得均一、稳定的食品级水包油包水型纳米乳液。
所得纳米乳液粒径为107.57nm,PDI(polydispersity Index)为0.586。测量方法如下:
用纳米粒度及Zeta电位仪(Nano Zetasizer,英国)分别测定样品的平均粒径和多分散性指数(PDI)。将样品吸取至石英四面透光池,加样时避免气泡的生成,体系分散剂设定为水,仪器平衡时间设定为100s,测试角度为173°,每个样品重复测量3次。
实施例2、制备食用级油包水包油型纳米乳液
食用级油包水包油型纳米乳液的制备方法,包括如下步骤:
(1)按照质量比4:2:1,分别取60mg乙酸异戊酯、30mg乙醇和15mg混合脂肪酸中含有质量浓度为60%的α-亚麻酸搅拌均匀,制得混合油相,再加入混合油相质量3倍,即315mgEL-35或Tween 80混合于小烧杯中,加入转子,调整转速为400rpm,在温度为25℃条件下搅拌40min;
(2)保持400rpm的搅拌速度,逐滴加入水,加入水的质量为步骤(1)获得的液体总质量3倍,即1260mg,得到均一、透明的水包油纳米乳液;
(3)按照质量比4:1,称取步骤(2)获得的水包油纳米乳液60mg,与15mg乙醇混合,制得混合水相,再加入混合水相质量3倍,即225mg EL-35混合于小烧杯中,加入转子,调整转速为400rpm,在温度为50℃条件下搅拌35min;
(4)保持400rpm的搅拌速度,逐滴加入质量为步骤(3)获得的液体总质量3倍的乙酸异戊酯,即900mg,得到均一、稳定的食品级油包水包油纳米乳液,即60%混合脂肪酸油包水包油纳米乳液。
所得纳米乳液粒径为99.2nm,PDI(polydispersity Index)为0.482。测量方法同实施例1。
实施例3、制备食用级油包水包油型纳米乳液的制备方法
食用级油包水包油型纳米乳液的制备方法,包括如下步骤:
(1)按照质量比2:2:1,分别取60mg乙酸异戊酯、60mg乙醇和30mg纯度为99%的α-亚麻酸搅拌均匀,制得混合油相,再加入混合油相质量12倍,即1800mg EL-35或Tween 80混合于小烧杯中,加入转子,调整转速为600rpm,在温度为35℃条件下搅拌60min;
(2)保持600rpm的搅拌速度,逐滴加入水,加入水的总质量为步骤(1)获得的液体总质量10倍,即19500mg,得到均一、透明的水包油纳米乳液;
(3)按照质量比1:1,称取60mg步骤(2)获得的水包油纳米乳液,与60mg乙醇混合,制得混合水相,再加入混合水相质量12倍,即1440mg EL-35混合于小烧杯中,加入转子,调整转速为500rpm,在温度为70℃条件下搅拌40min;
(4)保持500rpm的搅拌速度下,逐滴加入乙酸异戊酯,加入乙酸异戊酯的质量为步骤(3)获得的液体总质量6倍,即9360mg,得到均一、稳定的食品级油包水包油纳米乳液,即99%α-亚麻酸油包水包油纳米乳液。
所得纳米乳液粒径为93.68.2nm,PDI(polydispersity Index)为0.453。测量方法同实施例1。
实施例4、测定油包水包油纳米乳液稳定性
对实施例2-3制得的60%混合脂肪酸油包水包油纳米乳液和99%α-亚麻酸油包水包油纳米乳液进行如下氧化稳定性研究。具体操作如下:
制备60%混合脂肪酸O/W/O纳米乳液和99%α-亚麻酸O/W/O纳米乳液,根据纳米乳液混合油相配制相同质量比的乙酸异戊酯油溶液。将样品置于带螺旋盖的离心管中,分别在4℃和25℃恒温下保持30天。在储藏期间每两天通过UV-3300测量油溶液及纳米乳液样品中的α-亚麻酸含量。相对氧化稳定性计算公式为:
相对氧化稳定性=试样储存当天的α-亚麻酸含量/试样初始α-亚麻酸含量×100%
试验结果如图1-4所示,从图中可以看出,在不同温度下,O/W/O纳米乳液对α-亚麻酸均有良好的保护作用。油包水包油纳米乳液降低了温度和氧气对油脂的氧化作用,油脂的相对氧化稳定性显著提高。
上述具体实施方式,并不构成对本发明保护范围的限制。本领域技术人员应该明白的是,取决于设计要求和其他因素,可以发生各种各样的修改、组合、子组合和替代。任何在本发明的精神和原则之内所作的修改、等同替换和改进等,均应包含在本发明保护范围之内。
Claims (3)
1.油包水包油纳米乳液的制备方法,包括如下步骤:
(1)将乙酸异戊酯、乙醇和油相混合制得混合油相,再向所述混合油相中加入EL-35或Tween 80,进行搅拌,得到液体A;
(2)在搅拌条件下向所述步骤(1)得到的液体A中逐滴加入水,制得水包油纳米乳液;
(3)将所述步骤(2)制得的水包油纳米乳液和乙醇混合,制得混合水相,再向所述混合水相中加入EL-35,进行搅拌,得到液体B;
(4)在搅拌条件下向所述步骤(3)得到的液体B中逐滴加入乙酸异戊酯,制得油包水包油型纳米乳液;
所述步骤(1)的油相包括油脂或脂肪酸;所述油脂为牡丹籽油;所述脂肪酸为含有质量浓度为60%α-亚麻酸的混合脂肪酸或纯度为99%的α-亚麻酸;
所述步骤(1)中所述乙酸异戊酯、乙醇和油相的质量比为8:1:1~2:2:1;
所述步骤(1)中加入EL-35或Tween 80的质量是所述混合油相质量的1.5倍~12倍;
所述步骤(2)中加入水的质量是所述液体A质量的1倍~10倍;
所述步骤(3)中所述水包油纳米乳液和所述乙醇的质量比为1:1~8:1;
所述步骤(3)中加入EL-35的质量是所述混合水相质量的1.5倍~12倍;
所述步骤(4)中加入乙酸异戊酯的质量是所述液体B质量的1倍~6倍。
2.根据权利要求1所述的油包水包油纳米乳液的制备方法,其特征在于:
所述步骤(1)的搅拌是在温度为20℃~35℃、转速为300rpm~600rpm的条件下搅拌30min~60min;
所述步骤(2)的搅拌速度为300rpm~600rpm;
所述步骤(3)的搅拌是在温度为40℃~70℃、转速为300rpm~500rpm的条件下搅拌30min~40min;
所述步骤(4)的搅拌速度为300rpm~500rpm。
3.权利要求1或2所述的方法制备得到的油包水包油纳米乳液。
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