CN110916163B - 一种基于环糊精的复合乳化剂及其制备方法和应用 - Google Patents
一种基于环糊精的复合乳化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种基于环糊精的复合乳化剂及其乳状液的制备方法和应用,所述乳化剂由下述质量份的原料制成:水100份,植物油0.1~0.25份,环糊精1.6~1.8份,高分子填充剂0.5~1.0份;通过将植物油分散于环糊精水溶液中制备环糊精/油包合物的悬浮液,再加入高分子填充剂,经过高速剪切或高压均质使其充分混合,最后经过喷雾干燥或冷冻干燥获得该复合乳化剂;将复合乳化剂与植物油按照油水比混合后,经过高速剪切和高压均质即可得到高稳定的乳状液。本发明制备工艺简单高效、条件温和,制得的复合乳化剂乳化能力强,获得的乳状液稳定性高、流动性良好,可以有效抑制单一环糊精乳液絮凝问题。
Description
技术领域
本发明属于食品添加剂技术领域,具体涉及一种基于环糊精的复合乳化剂及其制备方法和应用。
背景技术
环糊精(Cyclodextrin)是由葡萄糖单元通过1,4-α-糖苷键连接形成的“锥筒”状分子,其中由6、7或8个吡喃葡萄糖单元构成的α-环糊精、β-环糊精和γ-环糊精最为常见。环糊精通过空腔结构可与油分子形成包合物用于稳定乳液,由于其良好的生物相容性,可成为化学合成表面活性剂的有效替代品。然而,环糊精表面含有大量的羟基,其乳液具有快速聚集和絮凝等缺陷(Mathapa B G, Paunov V N.Cyclodextrin stabilized emulsionsand cyclodextrinosomes.Physical Chemistry Chemical Physics,2013,15:17903-17914)。为了改善环糊精乳液的絮凝稳定性,通常采用的方法是对环糊精表面进行酯化反应,从而引入包括辛烯基琥珀酸和十八烯基琥珀酸等疏水基团(胡艳娜.辛烯基琥珀酸环糊精酯/姜黄素包合物的制备及其在Pickering乳液中的应用研究.广州:华南理工大学食品科学与工程学院,2017;Xi Y,Luo Z,Lu X,et al.Modulation of Cyclodextrin ParticleAmphiphilic Properties to Stabilize Pickering Emulsion.Journal ofAgricultural and Food Chemistry,2018,66(1):228-237)。上述酯化反应通常所需条件比较苛刻:使用的溶剂多为有机溶剂,或者反应时间长,步骤繁琐;同时也降低了环糊精的溶解度。
鉴于此,需要开发一种制备方法简单、分散性高的环糊精复合乳化剂,用于制备高稳定性乳状液。
发明内容
为了克服现有技术的缺点和不足,本发明提供了一种基于环糊精的复合乳化剂及其乳状液的制备方法和应用。本发明引入的高分子填充剂能与包合物粒子共同吸附在界面上使界面张力更低,以形成粒径更小分布更均匀的液滴;同时通过增加连续相的粘度来削弱液滴间的相互吸引,从而有效抑制乳液的絮凝。
为实现上述目的,本发明所采取的技术方案为:
一种基于环糊精的复合乳化剂,所述乳化剂由下述质量份的原料制成:水 100份,植物油0.1~0.25份,环糊精1.6~1.8份,高分子填充剂0.5~1.0份。
作为优选,所述环糊精为α-环糊精(α-CD)、β-环糊精(β-CD)、γ-环糊精(γ-CD)中的至少一种。
作为优选,所述植物油为大豆油、牡丹籽油、元宝枫籽油中的至少一种。
作为优选,所述高分子填充剂为酪蛋白酸钠、乳清蛋白、甲基纤维素中的至少一种。
本发明还提供了上述基于环糊精的复合乳化剂的制备方法,包括下述步骤:将植物油分散于环糊精水溶液中制备包合物悬浮液,再加入高分子填充剂,经过高速剪切或高压均质使其充分混合,最后经过干燥获得复合乳化剂。
所述的包合物是由环糊精和油分子包合而成,包合物进一步组装成胶体粒子。
作为优选,高速剪切速率为10000~16000rpm,剪切时间为1~5min;高压均质压力为300~700bar,均质次数为2~5次。
作为优选,所述的基于环糊精的复合乳化剂的制备方法,具体包括下述步骤:
(1)包合物的制备:室温下将β-环糊精加入到50质量份水中充分溶解,再将植物油加入其中,油水两相混合后,在12000~13000r/min转速下高速剪切 3min,在500~700bar的压力下均质3次乳化得到由β-环糊精和油分子自组装形成的胶体粒子;
(2)高分子填充剂的引入:将酪蛋白酸钠在室温下溶解于50质量份水中,搅拌两小时后放入4℃冰箱24h使其充分水合后加入到包合物悬浮液中,在 12000~13000r/min转速下高速剪切1min,在500~700bar的压力下均质2~3次使其充分混合;
(3)复合乳化剂的制备:将步骤(2)获得的混悬液经过喷雾干燥或者冷冻干燥后得到复合乳化剂。
另外,本发明还提供了上述基于环糊精的复合乳化剂的应用,其可用于高稳定乳状液的制备。
作为优选,将复合乳化剂与植物油按照油水比混合后,经过高速剪切和高压均质得到乳状液。
作为优选,将0.01~0.05质量份的复合乳化剂和油水比1:9或2:8的植物油和水经过10000~14000r/min转速高速剪切1min后,300~700bar高压均质3~5 次得到乳状液。
相对于现有技术,本发明的有益效果在于:
1、高分子填充剂能与包合物粒子共同吸附在油水界面上,能够有效降低界面张力,以形成粒径更小分布更均匀的液滴;同时增加连续相的粘度削弱液滴间的相互吸引;
2、改变高分子填充剂的添加方式、工艺参数、浓度等可有效调控乳液的絮凝行为,以满足不同条件下的应用效果;
3、本发明制备工艺简单、条件温和,获取的复合乳化剂乳化能力强,乳液稳定性高;并且所用原料具有环境友好、生物相容性高的优点。
附图说明
图1为实施例1、2、3制备的乳状液的小瓶图;
图2为实施例1制备的乳状液的光学显微镜图。
具体实施方式
下面通过实施例,对本发明的技术方案作进一步具体的说明,这些实施例是对本发明的说明而作,不是对本发明的限制。基于本申请中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本申请保护的范围。
下列实施例中涉及的物料均可从商业渠道获得。各组分用量均以质量份计。
实施例1
基于环糊精的复合乳化剂及其乳状液的制备
(1)包合物的制备:室温下将1.6质量份的β-CD加入到50份水中充分溶解,再将0.1质量份的大豆油加入其中,油水两相混合后,在13000r/min转速下高速剪切3min,在700bar的压力下均质3次得到包合物悬浮液;
(2)高分子填充剂的引入:将1.0质量份的酪蛋白酸钠在室温下溶解于50 份水中,搅拌两小时后放入4℃冰箱24h使其充分水合后加入到包合物悬浮液中,在13000r/min转速下高速剪切1min,在700bar的压力下均质3次使其充分混合;
(3)复合乳化剂的制备:将步骤(2)获得的混悬液经过喷雾干燥或者冷冻干燥后得到复合乳化剂;
(4)乳状液的制备:将0.05质量份的步骤(3)获得的复合乳化剂和10质量份的大豆油,90质量份的水经过13000r/min转速高速剪切1min后,700bar 高压均质3次得到乳状液。
制备的乳状液的小瓶图参照图1,制备的乳状液的光学显微镜参照图2。
实施例2
基于环糊精的复合乳化剂及其乳状液的制备
(1)包合物的制备:室温下将1.6质量份的β-CD加入到50份水中充分溶解,再将0.1质量份的元宝枫籽油加入其中,油水两相混合后,在13000r/min转速下高速剪切3min,在500bar的压力下均质3次乳化得到包合物悬浮液;
(2)高分子填充剂的引入:将1.0质量份的酪蛋白酸钠在室温下溶解于50 份水中,搅拌两小时后放入4℃冰箱24h使其充分水合后加入到包合物悬浮液中;在13000r/min转速下高速剪切1min,在500bar的压力下均质3次使其充分混合。
(3)复合乳化剂的制备:将步骤(2)获得的混悬液经过喷雾干燥或者冷冻干燥后得到复合乳化剂;
(4)乳状液的制备:将0.03质量份的步骤(3)获得的复合乳化剂和10 质量份的元宝枫籽油,90质量份的水经过12000r/min转速高速剪切1min后, 500bar高压均质3次得到乳状液。
实施例3
基于环糊精的复合乳化剂及其乳状液的制备
(1)包合物的制备:室温下将1.8质量份的β-CD加入到50份水中充分溶解,再将0.1质量份的牡丹籽油加入其中,油水两相混合后,在12000r/min转速下高速剪切3min,在500bar的压力下均质3次乳化得到包合物悬浮液;
(2)高分子填充剂的引入:将0.8质量份的酪蛋白酸钠在室温下溶解于50 份水中,搅拌两小时后放入4℃冰箱24h使其充分水合后加入到包合物悬浮液中;在12000r/min转速下高速剪切1min,在500bar的压力下均质2次使其充分混合;
(3)复合乳化剂的制备:将步骤(2)获得的混悬液经过喷雾干燥或者冷冻干燥后得到复合乳化剂。
(4)乳状液的制备:将0.03质量份的步骤(3)获得的复合乳化剂和10质量份的牡丹籽油,90质量份的水经过12000r/min转速高速剪切1min后,500bar 高压均质3次得到乳状液。
效果说明:
实施例1、实施例2、实施例3制备的乳状液的小瓶图参照图1,实施例1 制备的乳状液的光学显微镜参照图2,可以观察到液滴高度分散在连续相中,液滴粒径均一,没有出现液滴聚集现象。
通常用分层指数(creaming index,CI)来表示乳液的稳定性,CI侧面反映了乳液液滴在水相中的聚集状态。小瓶底部出现的水相称为清液层,上层的白色部分为乳析层。CI越高,乳液液滴间越呈分散状态,其稳定性越高。
CI(%)=(HC/HE)×100 (1)
式中:HC—乳析层高度;
HE—乳液的总高度
通过实施例1、2、3所制备的乳状液的分层指数如表1所示,其中单一乳化剂是指仅包括环糊精。
表1
上述实例制得的乳状液的分层指数均为100%,说明酪蛋白酸钠可以有效抑制环糊精的絮凝。
实施例1、2、3中所制备乳状液的平均粒径如表2所示,表2是采用马尔文激光粒度仪测定的上述实施例制备的乳状液的平均粒径。
表2
由表2可知,复合乳化剂稳定的乳状液粒径显著低于单一乳化剂组。说明酪蛋白酸钠有助于形成更小粒径的液滴。
实施例1、2、3所制备界面膜的油水界面张力如表3所示,表3为采用视频光学接触角测量仪获取的上述实施例中复合乳化剂的界面张力值。
表3
由表3可知,单一乳化剂组的界面张力均高于复合乳化剂组,说明酪蛋白酸钠能显著降低界面张力。
实施例1、2、3中所制备乳状液的弹性模量如表4所示,在流变学测试中,通过在固定频率下对样品施加应变获取应力响应,再将应力分解为弹性模量和粘性模量部分,其中弹性模量与乳液液滴的絮凝程度有关,弹性模量值越高,表明乳液液滴絮凝越严重。
表4
由表4可知复合乳化剂组的弹性模量显著低于单一乳化剂,表明其乳液絮凝得到明显抑制。
实施例1、2、3中所制备乳状液的屈服应变值如表5所示,屈服应变点为弹性模量与粘性模量曲线的交点,屈服应变值越高,表明乳液结构越均匀。
表5
由表5可知复合乳化剂组的屈服应变值显著高于单一乳化剂,表明其乳液结构更均匀。
Claims (5)
1.一种基于环糊精的复合乳化剂,其特征在于:所述乳化剂由下述质量份的原料制成:水100份,植物油0.1~0.25份,环糊精1.6~1.8份,高分子填充剂0.5~1.0份;所述环糊精为β-环糊精,所述高分子填充剂为酪蛋白酸钠;
所述乳化剂通过下述步骤制备得到:
(1)包合物的制备:室温下将β-环糊精加入到50质量份水中充分溶解,再将植物油加入其中,油水两相混合后,在12000~13000r/min转速下高速剪切3min,在500~700bar的压力下均质3次乳化得到由β-环糊精和油分子自组装形成的胶体粒子;
(2)高分子填充剂的引入:将酪蛋白酸钠在室温下溶解于50质量份水中,搅拌两小时后放入4℃冰箱24h使其充分水合后加入到包合物悬浮液中,在10000~16000rpm转速下高速剪切1~5min,在300~700bar的压力下均质2~5次使其充分混合;
(3)复合乳化剂的制备:将步骤(2)获得的混悬液经过喷雾干燥或者冷冻干燥后得到复合乳化剂。
2.根据权利要求1所述的基于环糊精的复合乳化剂,其特征在于:所述植物油为大豆油、牡丹籽油、元宝枫籽油中的至少一种。
3.权利要求1~2任一种所述基于环糊精的复合乳化剂的应用,其特征在于用于乳状液的制备。
4.根据权利要求3所述基于环糊精的复合乳化剂的应用,其特征在于:将复合乳化剂与植物油按照油水比混合后,经过高速剪切和高压均质得到乳状液。
5.根据权利要求3所述基于环糊精的复合乳化剂的应用,其特征在于:将0.01~0.05质量份的复合乳化剂和油水比1:9或2:8的油和水经过10000~14000r/min转速高速剪切1min后,300~700bar高压均质3~5次得到乳状液。
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