CN111228126B - 一种食品级聚甘油单月桂酸酯可稀释微乳液及制备方法 - Google Patents
一种食品级聚甘油单月桂酸酯可稀释微乳液及制备方法 Download PDFInfo
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Abstract
本发明公开了一种食品级可稀释的聚甘油单月桂酸酯微乳液及其制备方法,本发明的目的在于针对现有微乳液技术存在的缺陷,提供一种可广泛应用于食品、药品领域的微乳液制备配方。其特征在于通过控制表面活性剂(六聚甘油单月桂酸酯、十聚甘油单月桂酸酯)、助表面活性剂(乙醇)、油(油酸)的比例,得到稳定的可稀释微乳液。通过调节不同的稀释程度,可得到不同结构(W/O或O/W型)的微乳液。所制备微乳液具有无毒无害、可生物降解、生物相容性好等优点。可负载生物活性成分、食品营养素或食品色素,增强生物利用率,克服活性成分、食品营养素或色素溶解度差的缺点。所使用表面活性剂安全稳定,价格低廉,应用潜力巨大。同时生产工艺简单,节能环保,无需复杂生产设备。
Description
技术领域
本发明涉及一种食品级可稀释的微乳液,具体是涉及聚甘油单月桂酸酯微乳的制备方法,属微乳液的生产制备及应用领域。
背景技术
微乳液是油相、水相、表面活性剂、助表面活性剂在一定比例下自发形成的各向同性、外观透明或半透明的热力学稳定体系,与普通乳液相比,微乳液具有更小的粒径(1~100nm)及稳定性。因其具有极佳的稳定性,对水和油均具有良好的增溶能力,可作为食品功能成分的载体而受到广泛关注。但是,与微乳液的工业应用相比,食品体系更为复杂,安全性要求更高,制备微乳液所使用表面活性剂和助表面活性剂不仅要求无毒无害,而且使用量要在相关规定的限制范围内,因此利用一些安全无毒可食用的表面活性剂或者对已有表面活性剂进行复配来制备微乳具有重要的意义。
聚甘油单月桂酸酯是由聚甘油与单月桂酸形成的酯,作为一类新型非离子型表面活性剂,聚甘油单月桂酸酯不仅具有较强的乳化性能,而且具有较好的耐酸、耐热能力,安全无毒,被广泛应用于食品工业。月桂酸作为最不活泼的脂肪酸之一,其甘油酯在食品、化妆品领域有广泛的应用,具有良好的抗菌及防腐效果。但聚甘油单月桂酸酯流动性较差,不易溶于水,可考虑将不同聚合度的聚甘油单月桂酸酯复配为表面活性剂来制备微乳液,既能增强微乳液的稳定性、提升其安全性,又可克服聚甘油单月桂酸酯本身的缺点,从而进一步拓展聚甘油单月桂酸酯的应用。
微乳液的制备对各成分及其比例有苛刻的要求,选择和设计微乳液的组成时复杂、耗时、不可预知。在已有专利及文献中,不同类型(W/O或O/W型)微乳液通常需要采用不同的配方,并未有能够普遍应用的配方及比例。同时制备可稀释型微乳液通常需要大量的表面活性剂,如何制备较低表面活性剂含量的微乳液也是亟待解决的问题。
发明内容
为了解决现有微乳液技术中存在的稀释性差、表面活性剂含量高、安全性差等问题,本发明提供一种可转变结构(W/O或O/W型)的聚甘油单月桂酸酯微乳液及制备方法。
为实现上述技术效果,所采用具体步骤如下:
(1)按质量比为2:1称取一定量的六聚甘油单月桂酸酯和十聚甘油单月桂酸酯,室温下混合,搅拌,得到复配表面活性剂;
(2)向步骤(1)中所得复配表面活性剂加入质量为复配表面活性剂1/7.33~1/9的油酸,混合并搅拌;
(3)向步骤(2)中所得混合物加入1~3倍的乙醇,200~500r/min搅拌,混合;
(4)保持200~500r/min搅拌,向步骤(3)中所得样品中缓慢滴加一定量的蒸馏水,得到均一、透明的微乳液。
(5)当加水量小于45%时,微乳液为W/O结构;当加水量45%~65%时,微乳液为双连续结构;当加水量大于65%时,微乳液为O/W结构。
(6)为制备载姜黄素微乳液,可将一定质量的姜黄素添加至步骤(3)所得混合物中,避光条件下200~500r/min搅拌12h,直至姜黄素完全溶解,并按照步骤(4)(5)制备载姜黄素微乳液。
本发明的有益效果:
与现有微乳液相比,采用本发明制备的微乳液,可以达到以下技术效果:
1.安全无毒,排除了现有技术中不安全成分,可食用。
2.制备技术简单,具有可广泛应用的配方,仅通过调节不同的稀释程度,既可得到不同结构(W/O或O/W型)的微乳液。
3.与现有可稀释微乳液相比,具有更低的表面活性剂及助表面活性剂含量。
4.具有较高的载姜黄素能力,姜黄素在微乳液中的溶解度可达4.87 mg/mL。
附图说明
图1是微乳的制备流程图。
图2是不同复配比例表面活性剂制备微乳液的拟三元相图。
HGM六聚甘油单月桂酸酯、DGM十聚甘油单月桂酸酯;S为微乳区域面积占比;DR为最小可稀释比,N/A表示不存在。
图3不同表面活性剂与油质量比制备的微乳液的粒径及状态。
照片为不同SOR制备微乳液的状态,从左到右SOR依次降低。
图4微乳液状态及微乳液增溶效果。
从左到右依次为O/W型微乳液、载姜黄素微乳液、姜黄素水溶液。
图5负载不同色素的微乳液状态。
具体实施方式:
下面结合具体实施例对本发明作进一步说明,但不作为对本发明保护范围的限定。
实施例1
W/O型聚甘油单月桂酸酯微乳液的制备方法,包括如下步骤:
准确称取4g六聚甘油单月桂酸酯和2g十聚甘油单月桂酸酯,均匀混合在100mL烧杯里,向烧杯中加入0.75g油酸并搅拌均匀,然后加入12g无水乙醇并置于25℃的恒温磁力搅拌器上搅拌,在300r/min搅拌状态下向烧杯缓慢滴加8g蒸馏水,继续搅拌,得到均一透明的W/O型微乳液。
实施例2
双连续型聚甘油单月桂酸酯微乳液的制备方法,包括如下步骤:
准确称取4g六聚甘油单月桂酸酯和2g十聚甘油单月桂酸酯,均匀混合在100mL烧杯里,向烧杯中加入0.75g油酸并搅拌均匀,然后加入12g无水乙醇并置于35℃的恒温磁力搅拌器上搅拌,在300r/min搅拌状态下向烧杯缓慢滴加20g蒸馏水,继续搅拌,得到均一透明的双连续型微乳液。
实施例3
O/W型聚甘油单月桂酸酯微乳液的制备方法,包括如下步骤:
准确称取4g六聚甘油单月桂酸酯和2g十聚甘油单月桂酸酯,均匀混合在100mL烧杯里,向烧杯中加入0.75g油酸并搅拌均匀,然后加入12g无水乙醇并置于25℃的恒温磁力搅拌器上搅拌,在300r/min搅拌状态下向烧杯缓慢滴加35g0.2mol/LNaCl水溶液,继续搅拌,得到均一透明的O/W型微乳液。
实施例4
负载姜黄素的聚甘油单月桂酸酯微乳液的制备方法,包括如下步骤:
准确称取4g六聚甘油单月桂酸酯和2g十聚甘油单月桂酸酯,均匀混合在100mL烧杯里,向烧杯中加入0.75g油酸并搅拌均匀,然后加入12g无水乙醇并置于25℃的恒温磁力搅拌器上搅拌,向烧杯中加入2mg姜黄素继续搅拌直至完全溶解,在500r/min搅拌状态下向烧杯缓慢滴加35g蒸馏水,继续搅拌,得到均一透明的载姜黄素微乳液。
实施例5
(1)微乳液类型鉴别:取不同含水量的微乳于烧杯中,采用电导率仪分别测定其电导率,若电导率随水分含量的增加而上升,则为W/O型微乳;若电导率随水分增加无明显变化,则为双连续型微乳;若电导率随水分含量的增加而下降,则为O/W型微乳。
(2)微乳液粒径测定:用移液枪吸取一定量的微乳液置于样品池中,随后用激光粒度仪测定粒径分布。测试条件:温度25℃,平衡时间120s,每个样重复测试3次,测得的平均粒径范围为20~80nm。
Claims (8)
1.一种食品级聚甘油单月桂酸酯可稀释微乳液的制备方法,其特征在于,包括以下步骤:
(1)按质量比为1∶7.33~1∶9,将油酸与表面活性剂混合,再加入表面活性剂质量1~3倍的乙醇,在室温下,以200~500r/min速率搅拌10min,得到均一的混合溶液;
(2)保持200~500r/min的搅拌速率,向混合溶液中逐滴加入蒸馏水,得到均一、透明的微乳液;
所述表面活性剂为六聚甘油单月桂酸酯和十聚甘油单月桂酸酯的组合,质量比为2:1。
2.根据权利要求1所述的制备方法,其特征在于:步骤(2)中加入的水还可含有0~0.6mol/L的NaCl,pH=6.5~7.5。
3.根据权利要求1所述的制备方法,其特征在于:制备温度为15~35℃,无需均质化处理即得到均一、透明的微乳液。
4.根据权利要求1所述的制备方法,其特征在于:当微乳液为W/O型时,步骤(2)中加入的蒸馏水的量为微乳液总体积的1%~45%。
5.根据权利要求1所述的制备方法,其特征在于:当微乳液为双连续型时,步骤(2)中加入的蒸馏水的量为微乳液总体积的45%~65%。
6.根据权利要求1所述的制备方法,其特征在于:当微乳液为O/W型时,步骤(2)中加入的蒸馏水的量为微乳液总体积的65%~99.9%。
7.权利要求1~6任一项制得的微乳液,其特征在于:平均粒径范围为20~80nm。
8.权利要求7所述的微乳液,其特征在于:具有较高的载姜黄素能力,姜黄素在微乳液中的溶解度可达4.87mg/mL。
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