CN109156810A - 一种基于酯化大豆多糖的纳米乳液及其制备方法 - Google Patents
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Abstract
本发明属于乳液制备技术领域,公开了一种基于酯化大豆多糖的纳米乳液及其制备方法。将大豆多糖溶液经超声处理后加入辛烯基琥珀酸酐,在pH为8.0~9.0条件下进行酯化反应,干燥得到酯化大豆多糖;将所得酯化大豆多糖溶解于去离子水中,得到酯化大豆多糖溶液,搅拌条件下加入植物油,得到混合液;将所得混合液在10000~15000rpm条件下高速剪切3~5min,然后在300~500bar压力下高压微射流均质1~3次,得到基于酯化大豆多糖的纳米乳液。本发明所得酯化大豆多糖提高了大豆多糖的乳化性能和应用范围;并通过高压微射流均质处理,使乳液达到乳化稳定性更高的纳米级别。
Description
技术领域
本发明属于乳液制备技术领域,具体涉及一种基于酯化大豆多糖的纳米乳液及其制备方法。
背景技术
纳米乳液是一种乳液液滴粒径在20-500nm并呈现动力学稳定的胶体分散体系。也被称为细乳液,超细乳液,不稳定的微乳液和亚微米乳液。比普通的O/W乳液具有粒径小稳定性高等优点。经常应用于个人护理品、化妆品领域与纳米功能性食品的生产。高能乳化法是制备纳米乳液最常用的一种方法,在一定压力下,通过高速剪切的作用使分散相以细小的液滴分散在连续相中。高压微射流纳米均质机是一种能在短时间内实现高速撞击、剪切、气蚀、瞬间压降等作用达到乳液的细化、均质,获得超精细的纳米乳液的仪器。
乳化剂是指能够改善乳化体系中各个构成相之间的界面张力,从而形成均匀分散体或乳化体的一种表面活性成分。在乳液的形成中具有决定性作用。具有乳化性的多糖大多具有相似的性质:高度分支化,高分子量,具有亲水的碳水化合物骨架及疏水性的蛋白质成分或非极性基团。辛烯基琥珀酸淀粉酯(OSA-Starch)是由于疏水基团的引入,使得改性淀粉具有乳化活性,常作为一种改性多糖可应用于水包油乳液中。大豆可溶性多糖(SoySoluble Polysaccharides,SSPS)是从大豆分离蛋白生产的副产品中提取的生物高聚物,包含一个带负电荷的主要由鼠李糖半乳糖醛酸聚糖高度分支化的主链、中性的支链以及少量的蛋白质分子,因此具有乳化性,已被证明能够稳定水包油乳剂,且其乳液稳定不受pH、离子强度的影响,但由于其蛋白成分含量太低,其乳化稳定性较差。已有研究表明,以SSPS作为乳化剂的乳液在储藏过程中出现分层现象。
目前研究表明,对于多糖类为乳化剂稳定的乳液,多糖种类很少,且其在保存后的长期稳定性还不令人满意。
发明内容
针对以上现有技术存在的缺点和不足之处,本发明的首要目的在于提供一种基于酯化大豆多糖的纳米乳液的制备方法。
本发明的另一目的在于提供一种通过上述方法制备得到的基于酯化大豆多糖的纳米乳液。
本发明目的通过以下技术方案实现:
一种基于酯化大豆多糖的纳米乳液的制备方法,包括如下制备步骤:
(1)将大豆多糖溶液经超声处理后加入辛烯基琥珀酸酐,在pH为8.0~9.0条件下进行酯化反应,干燥得到酯化大豆多糖;
(2)将步骤(1)所得酯化大豆多糖溶解于去离子水中,得到酯化大豆多糖溶液,搅拌条件下加入植物油,得到混合液;
(3)将步骤(2)中所得混合液在10000~15000rpm条件下高速剪切3~5min,然后在300~500bar压力下高压微射流均质1~3次,得到基于酯化大豆多糖的纳米乳液。
优选地,步骤(1)中所述超声处理的条件为:频率30~50kHz,温度30~40℃,时间为10~40min。
优选地,步骤(1)中所述辛烯基琥珀酸酐与大豆多糖加入的质量比为1:(7~8)。
优选地,步骤(1)中所述酯化反应的时间为30~40min。
优选地,步骤(1)中所述干燥的方法为喷雾干燥或冷冻干燥。
优选地,步骤(2)中所述溶解于去离子水的条件为:40~50℃水浴条件下搅拌加热1~2h至完全溶解。
优选地,步骤(2)中所述酯化大豆多糖溶液的质量浓度为2%~6%。
优选地,步骤(2)中所述植物油选自大豆油、玉米油或色拉油。
优选地,步骤(2)中所述植物油的加入量为混合液质量的20%~30%。
一种基于酯化大豆多糖的纳米乳液,通过上述方法制备得到。
本发明的原理为:超声处理大豆多糖,使大豆多糖结构链在溶液中展开,有利于酸酐渗透到多糖结构中,强化了酯化反应的发生。通过化学修饰,将辛烯基琥珀酸酐(OctenylSuccinic Anhydride,OSA)与大豆多糖(SSPS)进行酯化反应,生成酯化大豆多糖OSA-SSPS,引入疏水性的OSA基团,从而增加乳化性及乳化稳定性。另一方面,酯化大豆多糖粒径的增大使得其在乳液中的空间位阻作用增强,形成较厚的空间稳定层。并通过高压微射流处理后,OSA-SSPS乳化的乳液粒径范围为100~300nm之间,使得乳液的储藏效果大大提升。
本发明的制备方法及所得到的产物具有如下优点及有益效果:
(1)本发明所得酯化大豆多糖(OSA-SSPS)的乳化性能明显优于原来的SSPS,提高了SSPS的乳化性能和应用范围;
(2)本发明对以酯化大豆多糖乳化的乳液进行高压微射流均质处理,使乳液达到乳化稳定性更高的纳米级别;
(3)本发明的制备方法不添加有毒有害试剂,绿色安全。
附图说明
图1为本发明实施例3以及对比例1~2所得的纳米乳液的粒径分布图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
以下实施例中所使用的可溶性大豆多糖购于福建省泉州市味博食品有限公司。高压微射流纳米均质机型号为Microfluidizer M-110EH。粒径分布利用Mastersizer 3000微米粒度仪测出。
实施例1
(1)制备大豆多糖溶液,将溶液放入超声波清洗器中,控制超声波频率为30kHz进行30℃循环水浴10min,将OSA添加到SSPS溶液中,以OSA:SSPS为1:7的质量比例进行酯化反应,反应pH为8.0,反应时间为30min,冷冻干燥得到酯化大豆多糖。
(2)将酯化大豆多糖加入到去离子水中,40℃水浴条件下加热2h至完全溶解,得到40ml质量分数为2%的酯化大豆多糖溶液;然后边搅拌边在酯化大豆多糖溶液中加入大豆油,得到大豆油的最终质量浓度为20%的混合液。
(3)将混合液在高速剪切机下以10000rpm转速剪切2min,然后在高压微射流纳米均质机中300bar压力下均质3次,得到基于酯化大豆多糖的纳米乳液。所得纳米乳液的粒径为292nm。
实施例2
(1)制备大豆多糖溶液,将溶液放入超声波清洗器中,控制超声波频率为40kHz进行35℃循环水浴20min,将OSA添加到SSPS溶液中,以OSA:SSPS为1:7.5的质量比例进行酯化反应,反应pH为8.5,反应时间为35min,冷冻干燥得到酯化大豆多糖。
(2)将酯化大豆多糖加入到去离子水中,45℃水浴条件下加热1.5h至完全溶解,得到40ml质量分数为3%的酯化大豆多糖溶液;然后边搅拌边在酯化大豆多糖溶液中加入大豆油,得到大豆油的最终质量浓度为25%的混合液。
(3)将混合液在高速剪切机下以13000rpm转速剪切4min,然后在高压微射流纳米均质机中400bar压力下均质2次,得到基于酯化大豆多糖的纳米乳液。所得纳米乳液的粒径为266nm。
实施例3
(1)制备大豆多糖溶液,将溶液放入超声波清洗器中,控制超声波频率为40kHz进行40℃循环水浴30min,将OSA添加到SSPS溶液中,以OSA:SSPS为1:8的质量比例进行酯化反应,反应pH为9.0,反应时间为40min,冷冻干燥得到酯化大豆多糖。
(2)将酯化大豆多糖加入到去离子水中,40℃水浴条件下加热1h至完全溶解,得到40ml质量分数为4%的酯化大豆多糖溶液;然后边搅拌边在酯化大豆多糖溶液中加入大豆油,得到大豆油的最终质量浓度为30%的混合液。
(3)将混合液在高速剪切机下以15000rpm转速剪切5min,然后在高压微射流纳米均质机中500bar压力下均质1次,得到基于酯化大豆多糖的纳米乳液。所得纳米乳液的粒径为209nm。所得纳米乳液的粒径分布图如图1所示。
实施例4
(1)制备大豆多糖溶液,将溶液放入超声波清洗器中,控制超声波频率为50kHz控制温度在进行30℃循环水浴40min,将OSA添加到SSPS溶液中,以OSA:SSPS为1:7的质量比例进行酯化反应,反应pH为8.5,反应时间为35min,喷雾干燥得到酯化大豆多糖。
(2)将酯化大豆多糖加入到去离子水中,50℃水浴条件下加热1h至完全溶解,得到40ml质量分数为6%的酯化大豆多糖溶液;然后边搅拌边在酯化大豆多糖溶液中加入大豆油,得到大豆油的最终质量浓度为30%的混合液。
(3)将混合液在高速剪切机下以15000rpm转速剪切5min,然后在高压微射流纳米均质机中300bar压力下均质3次,得到基于酯化大豆多糖的纳米乳液。所得纳米乳液的粒径为174nm。
对比例1
(1)将辛烯基琥珀酸淀粉酯(OSA-Starch)加入到去离子水中,40℃水浴条件下加热1h至完全溶解,得到40ml质量分数为4%的酯化淀粉溶液;然后边搅拌边在酯化淀粉溶液中加入大豆油,得到大豆油的最终质量浓度为25%的混合液。
(2)将混合液在高速剪切机下以13000rpm转速剪切4min,然后在高压微射流纳米均质机中400bar压力下均质2次,得到基于酯化淀粉的纳米乳液。所得纳米乳液的粒径为256nm。所得纳米乳液的粒径分布图如图1所示。
对比例2
(1)将水溶性大豆多糖加入到去离子水中,40℃水浴条件下加热1h至完全溶解,得到40ml质量分数为4%的大豆多糖溶液;然后边搅拌边在大豆多糖溶液中加入大豆油,得到大豆油的最终质量浓度为25%的混合液。
(2)将混合液在高速剪切机下以13000rpm转速剪切4min,然后在高压微射流纳米均质机中400bar压力下均质2次,得到基于大豆多糖的纳米乳液。所得纳米乳液的粒径为1725nm。所得纳米乳液的粒径分布图如图1所示。
由以上实施例及对比例的结果可以看出,本发明所得基于酯化大豆多糖的纳米乳液相比酯化淀粉的纳米乳液及未酯化的大豆多糖纳米乳液具有更小的粒径,具有更好的乳化稳定性。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (10)
1.一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于包括如下制备步骤:
(1)将大豆多糖溶液经超声处理后加入辛烯基琥珀酸酐,在pH为8.0~9.0条件下进行酯化反应,干燥得到酯化大豆多糖;
(2)将步骤(1)所得酯化大豆多糖溶解于去离子水中,得到酯化大豆多糖溶液,搅拌条件下加入植物油,得到混合液;
(3)将步骤(2)中所得混合液在10000~15000rpm条件下高速剪切3~5min,然后在300~500bar压力下高压微射流均质1~3次,得到基于酯化大豆多糖的纳米乳液。
2.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(1)中所述超声处理的条件为:频率30~50kHz,温度30~40℃,时间为10~40min。
3.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(1)中所述辛烯基琥珀酸酐与大豆多糖加入的质量比为1:(7~8)。
4.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(1)中所述酯化反应的时间为30~40min。
5.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(1)中所述干燥的方法为喷雾干燥或冷冻干燥。
6.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于步骤(2)中所述溶解于去离子水的条件为:40~50℃水浴条件下搅拌加热1~2h至完全溶解。
7.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(2)中所述酯化大豆多糖溶液的质量浓度为2%~6%。
8.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(2)中所述植物油选自大豆油、玉米油或色拉油。
9.根据权利要求1所述的一种基于酯化大豆多糖的纳米乳液的制备方法,其特征在于:步骤(2)中所述植物油的加入量为混合液质量的20%~30%。
10.一种基于酯化大豆多糖的纳米乳液,其特征在于:通过权利要求1~9任一项所述的方法制备得到。
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