CN113397156A - 一种双重Pickering乳液及其制备方法 - Google Patents
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Abstract
本发明公开了一种双重Pickering乳液及其制备方法。该方法采用超纯水将大豆水不溶性聚集体配成肽分散液,超声得到大豆水不溶性聚集体溶液;采用醋酸水溶液将壳聚糖配成溶液,获得壳聚糖溶液;将壳聚糖溶液缓慢滴于不断搅拌的大豆水不溶性聚集体溶液当中,并进行剪切均质获得复合胶体体系;调节包含复合胶体颗粒体系的pH为3~5,再与油脂混合,剪切乳化,得产物。本发明的双重乳液具有较高的稳定性,能够储藏长达四个月以上的时间不发生破乳漏油现象,乳液的双重结构能够保持一个月以上的时间,且流变和消化性能良好,有效的提高大豆蛋白酶解产物的绿色可持续化应用。
Description
技术领域
本发明涉及一种双重Pickering乳液,具体涉及一种大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定的双重Pickering乳液及其制备方法。
背景技术
双重乳液是乳液体系中一种较为复杂的乳液***,能够同时存在W/O与O/W两种乳液类型,凭借其自身独特的内部结构广泛应用于食品工业、药品及化妆品等多个领域。双重乳液的两种主要类型是水包油包水型(W/O/W)和油包水包油型(O/W/O)。
传统方式中对于双重乳液体系的稳定,通常需要两种或多种表面活性剂通过两步乳化法来实现。但这一方式在程序上更加复杂,且需要增加额外步骤或离子浓度来提高内水相渗透压防止内水相的外渗。为了克服这些弊端,利用一步乳化法途径稳定双重乳液受到了广泛的关注。一步乳化法稳定双重乳液的途径主要有微流控法、嵌段共聚物法以及Pickering乳液法。其中,Pickering乳液法利用胶体粒子能够吸附至油水界面形成坚固的屏障,抑制内部液滴发生聚集从而减少内水相损失,能够改善双重乳液体系的整体稳定性,且相对表面活性剂更加无毒、对环境友好。到目前为止,已经研究了由二氧化硅颗粒、氧化石墨烯颗粒和聚合物颗粒结合表面活性剂通过两步法制备稳定的双重Pickering乳液。然而,在这些胶体粒子中,使用可食用的胶体颗粒来一步法稳定双重乳液却很少被报道。显然,利用单一高剪切/高压作用下的完全可食用胶体颗粒进行乳化是一种很有前途的高效、安全的双重Pickering乳液生产方法,其潜在应用优势一直是食品工业中的研究热点。
中国发明专利申请2019106160134公开了一种利用改性高岭石作为乳化剂制备W/O/W双重Pickering乳液并实现对儿茶素和姜黄素的协同包封的方法。把溶有姜黄素的中链甘油三酯的作为乳化的油相(O),把溶有儿茶素的去离子水作为乳化的水相(W1),用接触角为130°的卵磷脂改性高岭石作为乳化剂,在剪切乳化条件下获得W1/O乳液。向获得的W1/O乳液加入分散有接触角为88°的卵磷脂改性高岭石的去离子水为W2相,在剪切乳化条件下获得同时将儿茶素和姜黄素包封在的O相和W1相中的W1/O/W2双重Pickering乳液。双重乳液对油溶性姜黄素和水溶性儿茶素的协同包封效率达到98%。但是该技术中的颗粒乳化剂为改性高岭土石,非食品级颗粒乳化剂,在食品领域应用受到限制;而且该技术采用两步法制备W1/O/W2双重Pickering乳液,制备方法复杂,成本高。
发明内容
本发明针对现有技术难以开发食品级双重Pickering乳液及复杂的两步制备工艺缺点,提供一种可用于食品领域的,制备成本低,不含表面活性剂的大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定的双重Pickering乳液及其制备方法,本发明不存在任何表面活性剂以及较复杂的程序即能得到稳定性高的双重Pickering乳液,并能储藏较长的时间。
本发明相对现有技术主要解决的问题是只使用食品级颗粒乳化剂,不同于常规两步乳化法方式,通过一步乳化法制备双重Pickering乳液,原料天然安全、制备方式简易。而且本发明中所用的颗粒乳化剂为可食用的大豆水不溶性聚集体-壳聚糖复合胶体颗粒,便于在食品中应用。
对于食品级双重Pickering乳液的制备,主要的障碍在于寻找功能性的,且食品工业允许的颗粒体系,且现有技术均为两步法制备繁琐。大豆蛋白广泛应用于食品工业中,通过将其酶解得到的产物也具备着于人体有益的功能保健特性。同时,大豆蛋白在酶解过程中产生的不溶性聚集体SWIA(Soy water-insoluble aggregates)也含有大量且成分均匀的必需氨基酸组成,且具备优异的荷载能力,能够作为一种潜在的功能性食品配料广泛应用于食品工业中。因此,利用大豆蛋白酶解后的水不溶性聚集体作为基料稳定双重Pickering乳液能够进一步提高大豆蛋白酶解产物的绿色可持续化应用。壳聚糖CS是一种碱性阳离子多糖,由甲壳素通过碱性脱乙酰作用得到。其来源丰富,具有良好的生物相容性、生物可降解性、抑菌性等特点被广泛应用在各个领域。
本发明开发出食品级的复合胶体颗粒,进而实现一步法制备双重Pickering乳液。现有技术中使用非食品级无机或聚合物颗粒结合表面活性剂作为双重Pickering乳液的乳化剂,且为两步制备方法,制备工艺繁琐;本发明利用大豆蛋白酶解副产物即大豆水不溶性聚集体与壳聚糖形成复合胶体颗粒,由此制备的复合胶体颗粒通过一步乳化法即可得到稳定双重Pickering乳液,有效的提高大豆蛋白酶解产物的绿色可持续化应用,在化妆品、药品、食品及保健品包括其他的领域具有良好的应用前景。目前国内关于利用食品级胶体颗粒一步乳化法制备双重Pickering乳液的方法尚未见报道。
本发明将大豆水不溶性聚集体SWIA与壳聚糖CS复合制备出结构稳定的复合胶体颗粒,以此作为乳化剂利用一步均质法制备稳定的双重Pickering乳液。在本发明中,不存在任何表面活性剂以及较复杂的程序即能得到稳定性高的双重Pickering乳液,并能储藏较长的时间,有效的提高大豆蛋白酶解产物的绿色可持续化应用,并为制备多重乳液提供一条便利途径。
本发明目的通过如下技术方案实现:
大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定双重Pickering乳液的制备方法,其特征在于:
采用超纯水将大豆水不溶性聚集体配制成肽分散液,超声得到大豆水不溶性聚集体溶液;采用醋酸水溶液将壳聚糖配成溶液,获得壳聚糖溶液:
将壳聚糖溶液滴于不断搅拌的大豆水不溶性聚集体溶液当中,并进行剪切均质获得包含复合胶体颗粒的体系;
调节复合胶体颗粒体系的pH为3~5,再与油脂混合,剪切乳化,得到大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定的双重Pickering乳液。
为进一步实现本发明目的,优选地,所述的大豆水不溶性聚集体SWIA为大豆分离蛋白用Protamex酶解12~24h后,将酶解液离心后的沉淀进行冷冻干燥所得到的粉末;Protamex的酶解条件设为pH5.0~8.0,温度50℃,按照底物重量计,每克底物的加酶量为000.5~0.01毫升。该方法在现有技术中常用。实施例中选择酶解20h,酶解条件设为pH6.0,温度50℃,按照底物重量计,每克底物的加酶量为000.8毫升,上述界定范围内所得其他工艺条件所得大豆水不溶性聚集体SWIA并无实质区别。
优选地,所述的醋酸水溶液的质量浓度为1%~3%。
优选地,所述的采用醋酸水溶液将壳聚糖配成溶液中壳聚糖的用量为醋酸溶液质量的0.5%~1%;
所述的采用超纯水将大豆水不溶性聚集体配制成肽分散液中大豆水不溶性聚集体的用量为水质量的0.2~0.5%;
所述的将壳聚糖溶液滴于不断搅拌的大豆水不溶性聚集体溶液当中大豆水不溶性聚集体溶液与壳聚糖溶液的体积比为1:1~2.5:1。
优选地,所述的超声功率为180W~200W,间歇时间为1~3s,总时间为5~10min。实施例的超声选择超声功率为200W,间歇时间为2s,总时间为8min,上述超声工艺条件下处理均可实现本发明目的。
优选地,所述的剪切均质的转速为15000rpm~20000rpm,剪切均质的时间为1~2min。
优选地,所述的油脂为玉米油。
优选地,调节pH为3~5后,复合胶体颗粒体系与油脂的体积比为1:1~3:1。
优选地,所述的剪切乳化的转速为8000rpm~12000rpm,剪切乳化的时间为30s~80s。
一种大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定双重Pickering乳液,由上述的制备方法制得。
与现有技术相比,本发明具有以下优点和有益效果:
(1)本发明首次利用大豆水不溶性聚集体-壳聚糖复合胶体颗粒通过一步法稳定双重Pickering乳液,不需要较为复杂的程序,不添加任何的表面活性剂。
(2)本发明的大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定的双重Pickering乳液具备较高的乳化效果与乳化稳定性,且储藏长达四个月以上不会出现破乳漏油的情况。
(3)本发明中用于稳定双重Pickering乳液的大豆水不溶性聚集体-壳聚糖复合胶体颗粒均为天然物质,且有效的提高大豆蛋白酶解产物的绿色可持续化应用,健康、无毒。
(4)本发明的大豆水不溶性聚集体复合胶体颗粒稳定的双重Pickering乳液具有良好的流变与消化性能,在化妆品、药品、食品及保健品包括其他的领域具有良好的应用前景。
附图说明
图1为实施例中新制SWIA-CS复合胶体颗粒稳定的双重Pickering乳液外观图;从左往右依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液;
图2为实施例1中放置四个月的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液外观图;从左往右依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液;
图3为对比例1制备的0.125%、0.25%与0.5%的CS稳定的Pickering乳液外观图;
图4为对比例1中放置24小时后0.125%、0.25%与0.5%的CS稳定的Pickering乳液外观图;
图5为实施例中新制和放置15天的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液的显微镜图;从上到下依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液;
图6为对比例1中新制0.125%、0.25%与0.5%的CS稳定的Pickering乳液显微镜观察图;
图7为实施例2中不同CS质量浓度的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液的激光共聚焦图;从左往右依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS复合胶体颗粒稳定的双重Pickering乳液;
图8~10分别为实施例1中0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定双重Pickering乳液应力扫描图;G'表示弹性模量,G"表示粘性模量;
图11和图12分别为实施例中0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定双重Pickering乳液在胃肠消化过程中的显微镜观察变化图。
具体实施方式
为更好地理解本发明,下面结合附图和实施例对本发明做进一步的说明,但本发明的实施方式不限于此。
对比例1
壳聚糖稳定双重Pickering乳液的制备方法,包括以下步骤:
(1)准确称取0.0125g、0.025g与0.05g壳聚糖CS溶解于10mL质量浓度为1%的醋酸溶液,得到质量浓度分别为0.125%、0.25%与0.5%的CS溶液;
(2)取3mL步骤(1)中所得溶液与3mL玉米油混合,剪切乳化转速为15000rpm/min,时间为2min,得到壳聚糖稳定的Pickering乳液。
实施例1-3
一种大豆水不溶性聚集体-壳聚糖一步法稳定双重Pickering乳液的制备方法,包括以下步骤:
(1)准确称取0.05g由大豆酶解过程产生的大豆水不溶性聚集体SWIA(酶解大豆蛋白获得)溶于10mL超纯水中,过夜水化之后进行超声,得到质量浓度为0.5%的SWIA溶液;
(2)准确称取0.1g壳聚糖CS溶解于10mL质量浓度为1%的醋酸溶液中,得到质量浓度为1%的CS溶液;
(3)将步骤(2)中所得CS溶液缓慢滴入步骤(1)所得的SWIA溶液中,并进行剪切均质得到质量浓度为0.25%SWIA-0.5%CS的复合胶体颗粒;
(4)取3mL步骤(3)中所得溶液和3mL玉米油混合,剪切乳化转速为15000rpm/min,时间为2min,得到大豆水不溶性聚集体-壳聚糖稳定的双重Pickering乳液。
本实施例对步骤(2)中CS的质量浓度进行了梯度试验,配制CS的质量浓度分别为0.125%、0.25%、0.5%,得到不同CS质量浓度的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液,具体分别得到0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS和0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液。
从实施例可见,本发明得到的产物与现有技术一般的双重Pickering乳液相比,颗粒乳化剂均为天然安全的食品原料,且一步乳化法制备得到。
通过显微镜观察证明得到的双重乳液结构;通过储存过程中显微观察双重乳液结构不变,结合外观稳定性,表征该大豆水不溶性聚集体-壳聚糖稳定的双重Pickering乳液产物;通过对颗粒和油脂进行荧光染色,激光共聚焦显微镜检测结果证明本发明的双重Pickering乳液为W/O/W型。
观察双重Pickering乳液放置不同时间的状态来表征其储藏稳定性。图1为实施例中新制SWIA-CS复合胶体颗粒稳定的双重Pickering乳液外观图;从左往右依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液;图2为实施例1中放置四个月的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液外观图;从左往右依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液;图5为实施例中新制和放置15天的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液的显微镜图;从上到下依次分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液。由图1和图2可知,分别由0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS、0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液放置储存长达4个月都很稳定,没有出现破乳情况。由图5可知,该乳液在放置15天后,其双重乳液结构仍然存在,较为稳定。
图3为对比例1制备的0.125%、0.25%与0.5%的CS稳定的Pickering乳液外观图;图4为对比例1中放置24小时后0.125%、0.25%与0.5%的CS稳定的Pickering乳液外观图;图6为对比例1中新制0.125%、0.25%与0.5%的CS稳定的Pickering乳液显微镜观察图。从图3、图4可见,对比例中新制0.125%、0.25%与0.5%的CS稳定的Pickering乳液在放置24小时后,油层完全析出,看见明显的破乳状态,且其新制乳液的显微图证明无双重乳液结构。由0.125%、0.25%与0.5%的CS稳定的Pickering乳液并不稳定,也无法制备成双重乳液。由图3和4可知,对比例1中不同壳聚糖浓度制备的Pickering乳液并不稳定,在放置24小时后完全破乳,再结合图6也能够清晰的看出单独的壳聚糖溶液也无法制备出双重乳液。由此可以看出,单独使用质量浓度为0.125%、0.25%与0.5%的CS不能够一步法制备稳定的双重Pickering乳液,而利用CS与SWIA形成的复合胶体颗粒可一步法制备稳定的双重Pickering乳液。
在新鲜乳液样品中加入尼罗红、尼罗蓝及荧光增白剂分别对油脂、蛋白与壳聚糖进行染色,进行激光共聚焦显微镜观察。尼罗蓝的激发波长为633nm,尼罗红的激发波长为488nm,荧光白额激发波长为405nm。图7是不同CS质量浓度的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液的激光共聚焦图。从图7中可以清晰的看到,所有大豆水不溶性聚集体-壳聚糖稳定的双重Pickering乳液中O/W乳滴内包含有大量的W/O小乳滴,表明大豆水不溶性聚集体-壳聚糖复合胶体颗粒能够通过简单的一步法均质形成W/O/W双重Pickering乳液。图中蓝色与红色即是大豆水不溶性聚集体与壳聚糖在双重乳液中的分布,可看出复合颗粒均匀的吸附在油脂界面上,进一步证实双重Pickering乳液的形成,并在界面形成坚固屏障使內相彼此独立且抑制聚并现象的出现。
对得到不同CS质量浓度的SWIA-CS复合胶体颗粒稳定的双重Pickering乳液,分别取1mL乳液进行流变学特性测试,温度为25℃,应力扫描频率设定为1Hz,得到应力扫描图。图8~10分别为0.25%SWIA-0.125%CS、0.25%SWIA-0.25%CS和0.25%SWIA-0.5%CS复合胶体颗粒稳定的双重Pickering乳液应力扫描图。由图可看出,弹性模量G′均大于粘性模量G″,表明此状态下的乳液呈现以粘弹性为主的凝胶性质。
图11、12分别为0.25%SWIA-0.25%CS和0.25%SWIA-0.5%CS复合胶体颗粒稳定Pickering双重乳液分别在肠消化与胃消化过程中乳液的定期显微镜观察图。油脂在食品中以很多种形式存在,它们的消化、吸收和代谢在指导食品配方中起着非常重要的作用。从图11、12中能够看出,在胃消化过程中,双重Pickering乳液的内水相因为消化液的高盐环境,促使部分内水相从低盐浓度的內相转移到相对高盐浓度的消化液环境中。但在胃消化结束之后乳滴还存在部分内水相,并且在整个胃消化过程中,油滴的尺寸基本没有出现显著的变化,初步说明复合胶体颗粒制备的双重Pickering乳液在胃消化过程中可以保持界面结构的完整性,有利于脂溶性活性物质输送至肠消化。
本发明大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定双重Pickering乳液在食品、药品领域和化妆品领域及其他领域中的应用中可作为疏水性及光敏、不耐受环境影响的活性成分输送载体,并可作为多孔微球制备的双重乳液模板;现有技术的双重Pickering乳液是由无机颗粒稳定,且分两步制备:先形成W1/O乳液后再制备W1/O/W2乳液(CN110302156A;佟永纯,王清云,白庆玲,李振,贾传明.双重Pickering乳液模板法制备无机-有机复合空心微球[J].高等学校化学学报,2018,39(07):1462-1466.);本发明所使用的颗粒乳化剂是绿色、天然的食品级大豆水不溶性聚集体-壳聚糖复合胶体颗粒,且本发明制备方式为一步法制备W1/O/W2双重Pickering乳液,本发明的双重Pickering乳液符合食品、药品等工业领域对原料天然、安全、无毒的要求,且制备工艺简易、高效。本发明大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定双重Pickering乳液在食品、药品领域和化妆品领域,可作为疏水性及光敏、不耐受环境影响的活性成分输送载体,并可作为多孔微球制备的双重乳液模板。
现有技术中使用非食品级无机或聚合物颗粒结合表面活性剂作为双重Pickering乳液的乳化剂,且为两步制备方法,制备工艺繁琐;本发明开发出食品级的复合胶体颗粒,并实现一步法制备双重Pickering乳液,为规模化生产提供了良好的技术支持。
本发明的实施方式并不受上述实施案例的限制,其他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。
Claims (10)
1.一种双重Pickering乳液的制备方法,其特征在于:
采用超纯水将大豆水不溶性聚集体配制成肽分散液,超声得到大豆水不溶性聚集体溶液;采用醋酸水溶液将壳聚糖配成溶液,获得壳聚糖溶液:
将壳聚糖溶液滴于不断搅拌的大豆水不溶性聚集体溶液当中,并进行剪切均质获得包含复合胶体颗粒的体系;
调节复合胶体颗粒体系的pH为3~5,再与油脂混合,剪切乳化,得到大豆水不溶性聚集体-壳聚糖复合胶体颗粒稳定的双重Pickering乳液。
2.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的大豆水不溶性聚集体为大豆分离蛋白用Protamex酶解12~24h后,将酶解液离心后的沉淀进行冷冻干燥所得到的粉末;Protamex的酶解条件设为pH5.0~8.0,温度50℃,按照底物重量计,每克底物的加酶量为000.5~0.01毫升。
3.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的醋酸水溶液的质量浓度为1%~3%。
4.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的采用醋酸水溶液将壳聚糖配成溶液中壳聚糖的用量为醋酸溶液质量的0.5%~1%;
所述的采用超纯水将大豆水不溶性聚集体配制成肽分散液中大豆水不溶性聚集体的用量为水质量的0.2~0.5%;
所述的将壳聚糖溶液滴于不断搅拌的大豆水不溶性聚集体溶液当中大豆水不溶性聚集体溶液与壳聚糖溶液的体积比为1:1~2.5:1。
5.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的超声功率为180W~200W,间歇时间为1~3s,总时间为5~10min。
6.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的剪切均质的转速为15000rpm~20000rpm,剪切均质的时间为1~2min。
7.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的油脂为玉米油。
8.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:调节pH为3~5后,复合胶体颗粒体系与油脂的体积比为1:1~3:1。
9.根据权利要求1中所述的双重Pickering乳液的制备方法,其特征在于:所述的剪切乳化的转速为8000rpm~12000rpm,剪切乳化的时间为30s~80s。
10.一种双重Pickering乳液,其特征在于:其由权利要求1-9所述的制备方法制得。
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