CN106667910B - 一种谷维素鱼油纳米乳液及其制备方法和应用 - Google Patents
一种谷维素鱼油纳米乳液及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及纳米乳液技术领域,公开了一种谷维素鱼油纳米乳液及其制备方法和应用。所述谷维素鱼油纳米乳液由以下质量百分数的物质组成:表面活性剂的含量为10%~12%,油相的含量为8%~11%,谷维素为油相质量的0.1%~1.8%,其余为水相;其中,所述油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的20%~40%。所述谷维素鱼油纳米乳液采用自乳化法(即低能量法)制备得到。谷维素鱼油纳米乳液的粒径均匀,乳液稳定不分层,浊度小等。谷维素鱼油纳米乳液中含有鱼油,能够提高谷维素的溶解度与生物利用度,又能与谷维素联合防止炎症。
Description
技术领域
本发明涉及纳米乳液技术领域,更具体的,涉及一种谷维素鱼油纳米乳液及其制备方法和应用。
背景技术
谷维素(C40H58O4)是从米糠毛油及其皂脚中提取的一种天然维生素类有机化合物,其主要成分是环木菠萝烯醇阿魏酯、2, 4-亚甲基环木菠萝醇阿魏酸。最新研究发现,谷维素除了具有清除自由基、抗氧化、降血脂、降血糖、抑制癌细胞生长等营养和药用功能外,还具有良好的抗炎生理功能。研究人员在临床上联合应用谷维素与其它抗炎药物防治炎症,发现谷维素能增强疗效。由于传统抗炎药物往往存在一定副作用,临床应用受到很大限制。目前市售的谷维素制剂尚无法有效解决脂溶性谷维素在体内溶解度和吸收率低、代谢降解又较快等缺点。因此,选择一种既能提高谷维素的溶解度与生物利用度,又能与谷维素联合作用的生物活性脂质尤为重要。
目前,增加谷维素溶解度的产品形式可概括为油性组合物、谷维素纳米颗粒、谷维素脂质体、谷维素微胶囊、谷维素自微乳制剂。然而,关于谷维素的纳米乳液的研究尚未见报道。制备纳米乳液的方法最常见的是高能量法(如高压均质法、微射流或超声波均质法)。然而,采用高能量输入设备(如高压均质机、微射流均质机)的均质工艺存在不仅能耗高、设备昂贵等问题,而且容易促进不饱和化合物发生氧化反应。
发明内容
本发明要解决的技术问题在于克服上述缺陷,提供一种谷维素鱼油纳米乳液的制备方法。
本发明的另一目的在于提供一种谷维素鱼油纳米乳液。
本发明的另一目的在于提供一种谷维素鱼油纳米乳液的应用。
本发明通过以下技术方案实现:
一种谷维素鱼油纳米乳液,由以下质量百分数的物质组成:
表面活性剂的含量为10%~12%,油相的含量为8%~11%,谷维素为油相质量的0.1%~1.8%,其余为水相;
其中,所述油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的20%~40%;
所述表面活性剂由吐温与司班20组成,表面活性剂的HLB值为11.8~15.0;
所述水相中酸度调节剂的浓度为0.01%~1%,防腐剂的浓度为0.01%~0.1%。
优选地,所述谷维素为油相质量的1%;所述鱼油的质量为油相的30%;所述表面活性剂的HLB值为13.4。
优选地,所述谷维素鱼油纳米乳液中表面活性剂的含量为10%,油相的含量为10%。
优选地,所述鱼油为甘油酯型鱼油、乙酯型鱼油。
优选地,所述谷维素鱼油纳米乳液粒径为5 nm ~160nm。本发明采用鱼油中n-3多不饱和脂肪酸(n-3PUFA)具有降低血清中甘油三酯、胆固醇和低密度脂蛋白含量、抗癌和抗炎等作用。
一种谷维素鱼油纳米乳液的制备方法,包括以下步骤:
S1. 有机相的制备:取谷维素置于含有油相、表面活性剂的容器中,搅拌至谷维素完全溶解;其中,谷维素为油相质量的0.1%~1.8%;所述油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的20%~40%;所述表面活性剂由吐温与司班20组成,表面活性剂的HLB值为11.8~15.0;
S2. 水相的制备:取酸度调节剂和防腐剂溶于纯水,水相中酸度调节剂的浓度为0.01%~1%,防腐剂的浓度为0.01%~0.1%;
S3. 自乳化法制备谷维素鱼油纳米乳液:将有机相以0.5~1.2滴秒的速度滴入持续搅拌的水相中,搅拌转数为700~1200rmin,温度为28±2℃;有机相滴加完毕后搅拌均匀得到谷维素鱼油纳米乳液;
所述谷维素鱼油纳米乳液中表面活性剂的含量为10%~12%,油相的含量为8%~11%。
优选地,S2中水相的将酸度调节剂和防腐剂添加到水中,并充分搅拌溶解。
为了获得稳定、不分层的纳米乳液,优选地,司班系列中只适合用司班20。司班40-85粘度更大,且HLB小(6.7-1.8)不利于形成粒径(<160nm)较小的乳液。
优选地,所述吐温为吐温20、吐温40、吐温60或吐温80。优选地,所述吐温为吐温80。
优选地,所述酸度调节剂为柠檬酸、乳酸、酒石酸、苹果酸、柠檬酸钠或柠檬酸钾中的一种或几种。所述酸度调节剂用于调节谷维素鱼油纳米乳液的pH。
优选地,所述防腐剂为山梨酸及其盐类、脱氢乙酸及其钠盐类、苯甲酸钠等。
优选地,所述有机相以1滴秒的速度滴入持续搅拌的水相中。有机相滴加的速度增大将导致乳液粒径变大,进一步导致乳液不稳定容易分层。
一种所述谷维素鱼油纳米乳液在制备乳制品或功能饮料方面的应用。
与现在有技术相比,本发明具有以下有益效果:
本发明采用自乳化法(即低能量法)制备谷维素鱼油纳米乳液,这种方法在加工纳米乳液过程中不需要太高的温度和机械剪切力,不会对谷维素和富含多不饱和脂肪酸的鱼油的化学稳定性产生潜在影响。
由于鱼油的分子大(其中的脂肪酸碳链长),通常采用低能量法是不能获得较稳定粒径较小的纳米乳液。本发明创造性的将鱼油及谷维素溶于MCT(中碳链饱和脂肪酸甘油三酯)后,意想不到地实现了采用自乳化法获得谷维素鱼油纳米乳液。
本发明制备得到的谷维素鱼油纳米乳液中乳液的粒径均匀,乳液稳定不分层,浊度小等。
谷维素鱼油纳米乳液中含有鱼油,能够提高谷维素的溶解度与生物利用度,又能与谷维素联合在多种生理功能方面发挥联合或协同作用,如预防炎症、降低血脂。
本发明得到的谷维素鱼油纳米乳液中因谷维素含量较高及其与鱼油发挥联合或协同作用而具有非常高的营养价值和生理功能。
具体实施方式
下面结合具体实施例进一步说明本发明。除非特别说明,本发明实施例中采用的原料和方法为本领域常规市购的原料和常规使用的方法。
以下各实施例或对比例的样品经以下方法进行性能检测:
1、外观及物理稳定性
吸取7mL谷维素鱼油纳米乳液于10mL冻干瓶中,将谷维素鱼油纳米乳液样品在室温下放置24h后,测定粒径的变化。接着,记录谷维素鱼油纳米乳液放置7天的外观变化,包括透明度、颜色、分层等。
2、粒径
将制备的谷维素鱼油纳米乳液用激光粒度仪测定平均粒径,每个样品平行测定2次。操作参数设置:测定温度为25℃,设定平衡时间为70s,每次扫描13次。为了避免多重散射的影响,所有乳液均稀释500倍后再进行测定。稀释液为1%的柠檬酸和0.1%苯甲酸钠水溶液。
3、浊度
谷维素鱼油纳米乳液的浊度通过采用紫外分光光度计在全波长下测定不同条件下制备的纳米乳液的吸光度获得。用移液枪准确移取0.25mL谷维素鱼油纳米乳液于25mL容量瓶中,用稀释液定容至刻度,混匀后用移液枪移取3mL稀释过的乳液于石英比色皿中,使用紫外分光光度计在200~800nm波长下测定吸光度。样品吸光度平行测定三次。读取600nm的吸光度,浊度计算公式为r=2.303×A×VL。
式中:r-浊度,A-吸光度,V-稀释倍数,L-比色皿宽度(本实验为1cm)
实施例1
一种谷维素鱼油纳米乳液的制备方法,包括以下步骤:
S1. 有机相的制备:取谷维素置于含有油相、表面活性剂的容器中,搅拌至谷维素完全溶解;其中,谷维素为油相质量的0.1%;油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的20%;所述表面活性剂由吐温80与司班20组成,表面活性剂的HLB值为14.4;
S2. 水相的制备:取乳酸和山梨酸溶于纯水,水相中乳酸的浓度为0.01%,苯甲酸钠的浓度为0.1%;S2中水相的将乳酸和山梨酸添加到水中,并充分搅拌溶解。
S3. 自乳化法制备谷维素鱼油纳米乳液:将有机相以0.5滴秒的速度滴入持续搅拌的水相中,搅拌转数为700rmin,温度为28±2℃;有机相滴加完毕后搅拌均匀得到谷维素鱼油纳米乳液;
谷维素鱼油纳米乳液中表面活性剂的含量为10%,油相的含量为8%。
检测谷维素鱼油纳米乳液的外观、浊度、粒径、物理稳定性。实验结果如表2所示。
实施例2
一种谷维素鱼油纳米乳液的制备方法,包括以下步骤:
S1. 有机相的制备:取谷维素置于含有油相、表面活性剂的容器中,搅拌至谷维素完全溶解;其中,谷维素为油相质量的1%;油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的30%;所述表面活性剂由吐温80与司班20组成,表面活性剂的HLB值为13.4;
S2. 水相的制备:取柠檬酸和苯甲酸钠溶于纯水,水相中柠檬酸的浓度为0.05%,苯甲酸钠的浓度为0.08%;S2中水相的将柠檬酸和苯甲酸钠添加到水中,并充分搅拌溶解。
S3. 自乳化法制备谷维素鱼油纳米乳液:将有机相以1滴秒的速度滴入持续搅拌的水相中,搅拌转数为850rmin,温度为28±2℃;有机相滴加完毕后搅拌均匀得到谷维素鱼油纳米乳液;
谷维素鱼油纳米乳液中表面活性剂的含量为10%,油相的含量为10%。
检测谷维素鱼油纳米乳液的外观、浊度、粒径、物理稳定性。实验结果如表2所示。
实施例3
一种谷维素鱼油纳米乳液的制备方法,包括以下步骤:
S1. 有机相的制备:取谷维素置于含有油相、表面活性剂的容器中,搅拌至谷维素完全溶解;其中,谷维素为油相质量的1.8%;油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的40%;所述表面活性剂由吐温40与司班20组成,表面活性剂的HLB值为15.0;
S2. 水相的制备:取酒石酸和脱氢乙酸溶于纯水,水相中柠檬酸的浓度为1%,苯甲酸钠的浓度为0.01%;S2中水相的将酒石酸和脱氢乙酸添加到水中,并充分搅拌溶解。
S3. 自乳化法制备谷维素鱼油纳米乳液:将有机相以1滴秒的速度滴入持续搅拌的水相中,搅拌转数为1200rmin,温度为28±2℃;有机相滴加完毕后搅拌均匀得到谷维素鱼油纳米乳液;
谷维素鱼油纳米乳液中表面活性剂的含量为12%,油相的含量为11%。
检测谷维素鱼油纳米乳液的外观、浊度、粒径、物理稳定性。实验结果如表2所示。
对比例1~8
对比例1~8的制备方法与实施例2相似,不同点在于如表1所示:
表1
项目 | 对比例1 | 对比例2 | 对比例3 | 对比例4 | 对比例5 | 对比例6 | 对比例7 | 对比例8 |
谷维素为油相质量分数,% | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
鱼油的质量为油相的质量分数,% | 19 | 41 | 30 | 30 | 30 | 60 | 30 | 30 |
表面活性剂的HLB值 | 11.8 | 15.0 | 11.8 | 15.5 | 15.0 | 13.4 | 8.6 | 13.4 |
有机相滴加速度,滴秒 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
表面活性剂的含量,% | 10 | 10 | 10 | 10 | 9 | 13 | 10 | 10 |
油相的含量,% | 10 | 10 | 10 | 10 | 10 | 10 | 7 | 12 |
分别检测对比例1~8制备得到谷维素鱼油纳米乳液的外观、浊度、粒径、物理稳定性。实验结果如表2所示。
对比例9
一种谷维素鱼油纳米乳液的制备方法,包括以下步骤:
取谷维素溶于中链甘油三酯和鱼油组成的油相中,加入表面活性剂,然后加水搅拌后制得。其中,谷维素为油相质量的1%;鱼油的质量为油相的30%;表面活性剂由吐温80与司班20组成,表面活性剂的HLB值为13.4;水中柠檬酸的浓度为0.05%,苯甲酸钠的浓度为0.08%。搅拌转数为850rmin,温度为28±2℃。谷维素鱼油纳米乳液中表面活性剂的含量为10%,油相的含量为10%。
检测谷维素鱼油纳米乳液的外观、浊度、粒径、物理稳定性。实验结果如表2所示。
对比例10
一种谷维素鱼油纳米乳液的制备方法,包括以下步骤:
S1. 有机相的制备:取谷维素置于含有油相、表面活性剂的容器中,搅拌至谷维素完全溶解;其中,谷维素为油相质量的1%;油相为鱼油;表面活性剂由吐温80与司班20组成,表面活性剂的HLB值为13.4;
S2. 水相的制备:取柠檬酸和苯甲酸钠溶于纯水,水相中柠檬酸的浓度为0.05%,苯甲酸钠的浓度为0.08%;S2中水相的将柠檬酸和苯甲酸钠添加到水中,并充分搅拌溶解。
S3. 自乳化法制备谷维素鱼油纳米乳液:将有机相以1滴秒的速度滴入持续搅拌的水相中,搅拌转数为850rmin,温度为28±2℃;有机相滴加完毕后搅拌均匀得到谷维素鱼油纳米乳液;
谷维素鱼油纳米乳液中表面活性剂的含量为10%,油相的含量为10%。
检测谷维素鱼油纳米乳液的外观、浊度、粒径、物理稳定性。实验结果如表2所示。
表2
外观及稳定性:实施例1~3制备的谷维素鱼油纳米乳液在7天后无分层现象,无乳析现象。对比例1~11制备的谷维素鱼油纳米乳液放置3天内出现明显的絮凝、乳析现象、分层。
对比例9采用直接混合的方式,制得乳液粒径较大,相应的浊度也较大、乳白色、不透明,物理稳定性较差,3天内出现明显分层。
对比例10没有使用中链甘油三酯,制得乳液为乳黄色,不透明,浊度大,15min内出现分层现象,乳液极其不稳定。
Claims (7)
1.一种谷维素鱼油纳米乳液,其特征在于,由以下质量百分数的物质组成:
表面活性剂的含量为10%~12%,油相的含量为8%~11%,谷维素为油相质量的0.1%~1.8%,其余为水相;
其中,所述油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的20%~40%;
所述表面活性剂由吐温与司班20组成,表面活性剂的HLB值为13.4~15.0;
所述水相中酸度调节剂的浓度为0.01%~1%,防腐剂的浓度为0.01%~0.1%;
所述谷维素鱼油纳米乳液的制备方法包括以下步骤:
S1. 有机相的制备:取谷维素置于含有油相、表面活性剂的容器中,搅拌至谷维素完全溶解;其中,谷维素为油相质量的0.1%~1.8%;所述油相由中链甘油三酯和鱼油组成,其中鱼油的质量为油相的20%~40%;所述表面活性剂由吐温与司班20组成,表面活性剂的HLB值为13.4~15.0;
S2. 水相的制备:取酸度调节剂和防腐剂溶于纯水,水相中酸度调节剂的浓度为0.01%~1%,防腐剂的浓度为0.01%~0.1%;
S3. 自乳化法制备谷维素鱼油纳米乳液:将有机相以0.5~1.2滴秒的速度滴入持续搅拌的水相中,搅拌转数为700~1200rmin,温度为28±2℃;有机相滴加完毕后搅拌均匀得到谷维素鱼油纳米乳液。
2.根据权利要求1所述谷维素鱼油纳米乳液,其特征在于,所述谷维素为油相质量的1%;所述鱼油的质量为油相的30%;所述表面活性剂的HLB值为13.4。
3.根据权利要求1所述谷维素鱼油纳米乳液,其特征在于,所述谷维素鱼油纳米乳液中表面活性剂的含量为10%,油相的含量为10%。
4.根据权利要求1所述谷维素鱼油纳米乳液,其特征在于,所述鱼油为甘油酯型鱼油、乙酯型鱼油。
5.根据权利要求1所述谷维素鱼油纳米乳液,其特征在于,所述谷维素鱼油纳米乳液粒径为5 nm ~160nm。
6.根据权利要求1所述谷维素鱼油纳米乳液,其特征在于, S2中将 水相的酸度调节剂和防腐剂添加到水中,并充分搅拌溶解。
7.根据权利要求1~6任意一项所述谷维素鱼油纳米乳液在制备乳制品或功能饮料方面的应用。
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