CN114569474A - 一种维生素e纳米乳及其制备方法 - Google Patents
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Abstract
本发明公开了一种维生素E纳米乳,包括以下重量分的原料,维生素E 10‑20份;辛烯基琥珀酸可得然胶酯5‑12.5份;表面活性剂0.2‑1份;水66.5‑84.8份。还公开了该维生素E纳米乳的制备方法。本发明采用纳米乳载体以及表面活性剂,都可生物降解,安全可靠。
Description
技术领域
本发明属于日化产品及其助剂领域,特别是涉及一种维生素E纳米乳及其制备方法。
背景技术
维生素E是一种脂溶性的抗氧化剂,能够在肌体内对抗自由基的破坏作用和清除自由基,抑制过氧化物的产生,参与机体多种代谢过程。维生素E能增强皮肤毛细血管的血流量,增加血管对寒冷的抵抗力,维持毛细血管的正常通透性,延缓皮肤和一些器官的萎缩和退化。
除了药用以外,近年来维生素E还被广泛用于保健品、营养剂、食品添加剂及化妆品中。在食品工业方面,维生素E又是一种良好的脱臭剂,如在口香糖中加入一定量的维生素E,可消除口腔臭味。在香波中,维生素E也具有脱臭效果。
在药学领域,维生素E的给药形式主要集中在胶丸剂、注射液,以及外用的霜剂、乳膏剂等。这些粒径较大的维生素E剂型,不同程度的存在生物利用度低、吸收差的不足;并且维生素E容易受环境中氧的影响被氧化形成生育醌,很容易受到紫外线的照射而分解。将维生素E制成O/W型纳米乳可以解决这些问题。
纳米技术是21世纪最具发展前景的领域之一,美国国家科学技术委员会在2000年指出:全世界在未来10年约有占市场销售额50%的药品将要运用纳米技术。随着科学研究地不断深入,新型化妆品不断涌现,纳米技术在日化领域中的应用逐渐增多。
目前,在纳米药物研究领域,药物载体的筛选以及制备工艺的优化已经成为研究重点。载体包括聚合物纳米粒,纳米乳液,脂质体,纳米悬浮液,固体脂质纳米粒,纳米结构脂质载体等。
传统工艺生产的维生素E乳液粒径大小在5-20微米,不同程度的存在生物利用度低、吸收差的不足。因此,研究制备粒径更小的维生素E乳液方法,提高产品渗透性,并将该制备方法应用于实际生产中是当前急需解决的问题。
发明内容
本发明提供一种维生素E纳米乳及其制备方法,目的在于解决如下技术问题:(1)采用聚合物作为载体,通过超高压均质制备维生素E纳米乳,设备投资少,工艺简便,可广泛应用于工业生产;(2)将维生素E纳米乳的粒径控制在较窄的范围,利于提高纳米乳的渗透性。
本发明针对现有技术的不足,提出了一种维生素E纳米乳及其制备方法,使用可生物降解的聚合物作为软质载体,制备维生素E纳米乳。该制备方法简单、易操作,制备的维生素E纳米乳粒径为200nm左右,具有优良的稳定性。
本发明使用过以下技术方案实现的:
一种维生素E纳米乳,包括以下重量分的原料,维生素E10-20份;辛烯基琥珀酸可得然胶酯5-12.5份;表面活性剂0.2-1份;水66.5-84.8份。
一种维生素E纳米乳,包括以下重量分的原料,维生素E15份;辛烯基琥珀酸可得然胶酯8.5份;表面活性剂0.7份;水75.8份。
所述表面活性剂为蔗糖脂肪酸酯。
所述辛烯基琥珀酸可得然胶酯通过以下方法制备:取可得然胶,放入双锥干燥混合机中,然后取占可得然胶干重7%的辛烯基琥珀酸酐用无水乙醇稀释后喷入可得然胶中,混合均匀,回收乙醇后,加入占可得然胶干重5%的无水碳酸钠,并调整可得然胶的含水量达到25%,加热至60℃至反应完成,反应产物用乙醇洗涤3次后50℃烘干,过80目筛。
一种维生素E纳米乳的制备方法,其特征在于,包括以下步骤:
步骤Ⅰ,在配料罐中加入水,边搅拌边依次加入维生素E、蔗糖脂肪酸酯、辛烯基琥珀酸可得然胶酯;
步骤Ⅱ,开启高剪切乳化机对物料进行剪切乳化;
步骤Ⅲ,将已经乳化的物料泵入超高压纳米均质机,进行循环均质;
步骤Ⅳ,将均质好的物料泵入成品暂存罐中,开启搅拌,灌装得到成品。
所述步骤Ⅱ中物料进行剪切分散乳化时,物料温度保持室温。
所述步骤Ⅲ中物料进行循环均质时,物料温度保持室温。
所述循环均质时,均质压力为120MPa。
所述剪切乳化和循环均质的时长均为1h。
本发明具有以下技术效果:
本发明采用辛烯基琥珀酸可得然胶酯作为维生素E纳米乳载体,蔗糖脂肪酸酯作为表面活性剂,两者都可生物降解,安全可靠。
本发明完全以水为介质,采用超高压均质的技术手段将维生素E制备成为维生素E纳米乳,粒径为200nm左右,远小于传统工艺生产的维生素E乳液的微米尺寸,提高了产品稳定性和渗透性。
具体实施方式
本发明提供的维生素E纳米乳,包括以下组分,按重量计维生素E10-20份;辛烯基琥珀酸可得然胶酯5-12.5份;表面活性剂0.2-1份;水66.5-84.8份。
利用以上原料制备维生素E纳米乳的方法包括以下步骤:
在室温下,首先10-20份维生素E加入66.5-84.8份水中;然后加入0.2-1份表面活性剂、5-12.5份纳米粒子载体,用高剪切分散乳化机在转速2900rpm下混合均匀,最后在保持室温的状态下通过超高压纳米均质机进行均质,均质完成后得到稳定性良好的维生素E纳米乳。
本发明中采用的纳米粒子载体是辛烯基琥珀酸可得然胶酯,该载体是用辛烯基琥珀酸酐修饰可得然胶制得。可得然胶是以β-1,3糖苷键构成的水不溶性葡聚糖,其悬浊液加热后既能形成硬而有弹性的热不可逆性凝胶又能形成热可逆性凝胶。可得然胶具有极强的包油性,将3%可得然胶与各种浓度的玉米油混合液均质并在95℃,10min加热后,随含油量的增加,形成不可逆性凝胶的凝胶强度和脱水率均降低。当含油量达到24%时,凝胶在生成过程和生成后仍不发生油分离,将含油凝胶夹在两板间压榨,仅能除去部分水分,油仍然残留在干燥物中,含量可达85%。可得然胶加热形成的凝胶无法稀释,这极大地限制了其应用范围。本发明中采用辛烯基琥珀酸酐修饰可得然胶(取代度为0.015左右)后,形成的辛烯基琥珀酸可得然胶酯在高温下不会形成凝胶,并且仍具有很强的包油性。以辛烯基琥珀酸可得然胶酯为载体,以维生素E为芯材,在一定条件下可以制备成维生素E纳米乳,粒径在200纳米左右,远小于传统工艺生产的维生素E乳液的微米尺寸,提高了产品稳定性和渗透性。
下面通过具体实施例对本发明的技术方案进行详细说明。
以下实施例中超高压纳米均质机型号为JZH2000-180,上海锦竹机械设备有限公司;蔗糖脂肪酸酯的HLB值为15;激光粒度分析仪购自英国马尔文仪器有限公司。
以下实施例中使用的辛烯基琥珀酸可得然胶酯的制备方法为:取100kg可得然胶,放入双锥干燥混合机中,取占可得然胶干重7%的辛烯基琥珀酸酐用10千克无水乙醇进行稀释后喷入可得然胶中;混合均匀,回收无水乙醇,待无水乙醇含量低于0.2%后,加入占可得然胶干重5%的无水碳酸钠,喷入适量的水使可得然胶的含水量达到25%,加热至60℃反应8h。反应产物用乙醇洗涤3次后50℃烘干,过80目筛得到辛烯基琥珀酸可得然胶酯,取代度为0.015左右。
实施例一,含10wt%维生素E纳米乳的制备
步骤Ⅰ,在配料罐中加入84.8份的纯净水,称取10份的维生素E投入配料罐中。
步骤Ⅱ,称取0.2份的蔗糖脂肪酸酯和5份的辛烯基琥珀酸可得然胶酯加入配料罐中,开启高剪切分散乳化机,转速为2900rpm;1h后停止高剪切分散乳化机,开启搅拌准备均质,期间控制物料温度为室温。
步骤Ⅲ,用变频螺杆泵将配料罐中已经乳化的物料泵入超高压纳米均质机,调节变频螺杆泵流量与均质机流量相匹配,均质压力控制在120MPa,均质后的物料回流至配料罐,并控制物料温度始终控制在室温,物料循环均质1h。
步骤Ⅳ,将均质好的物料泵入成品暂存罐中,开启搅拌,转速为120rpm,灌装得到成品。产品经激光粒度分析仪测定纳米粒子粒径为198nm。
实施例二,含15wt%维生素E纳米乳的制备
步骤Ⅰ,在配料罐中加入75.8份的纯净水,称取15份的维生素E投入配料罐中。
步骤Ⅱ,称取0.7份蔗糖脂肪酸酯和8.5份辛烯基琥珀酸可得然胶酯加入配料罐中,开启高剪切分散乳化机,转速为2900rpm;1h后停止高剪切分散乳化机,开启搅拌准备均质,期间控制物料温度为室温。
步骤Ⅲ,用变频螺杆泵将配料罐中已经乳化的物料泵入超高压纳米均质机,调节变频螺杆泵流量与均质机流量相匹配,均质压力控制在120MPa,均质后的物料回流至配料罐,并使物料温度始终控制在室温,物料循环均质1h。
步骤Ⅳ,将均质好的物料泵入成品暂存罐中,开启搅拌,转速为120rpm,灌装得到成品。产品经激光粒度分析仪测定纳米粒子粒径为211nm。
实施例三,含20wt%维生素E纳米乳的制备
步骤Ⅰ,在配料罐中加入66.5份的纯净水,称取20份的维生素E投入配料罐中。
步骤Ⅱ,称1份的取蔗糖脂肪酸酯和12.5份辛烯基琥珀酸可得然胶酯加入配料罐中,开启高剪切乳化机,转速为2900rpm;1h后停止高剪切乳化机,开启搅拌准备均质,期间控制物料温度为室温。
步骤Ⅲ,用变频螺杆泵将配料罐中已经乳化的物料泵入超高压纳米均质机,调节变频螺杆泵流量与均质机流量相匹配,均质压力控制在120MPa,均质后的物料回流至配料罐,并使物料温度始终控制在室温,物料循环均质1h。
步骤Ⅳ,将均质好的物料泵入成品暂存罐中,开启搅拌,转速为120rpm,灌装得到成品。产品经激光粒度分析仪测定纳米粒子粒径为219nm。
稳定性试验:
将含20wt%维生素E纳米乳产品在40℃下放置30天,分别测定第0、1、4、7、15、30天产品的粒径,数据如表1
表1放置不同时间后产品的粒径
放置时间/天 | 0 | 1 | 4 | 7 | 15 | 30 |
产品粒径/nm | 219 | 221 | 227 | 224 | 225 | 225 |
从表中数据可以看出:产品的粒径未发生大的变化,具有较强的稳定性。
Claims (9)
1.一种维生素E纳米乳,其特征在于:包括以下重量分的原料,维生素E 10-20份;辛烯基琥珀酸可得然胶酯5-12.5份;表面活性剂0.2-1份;水66.5-84.8份。
2.根据权利要求1所述的维生素E纳米乳,其特征在于:包括以下重量分的原料,维生素E 15份;辛烯基琥珀酸可得然胶酯8.5份;表面活性剂0.7份;水75.8份。
3.根据权利要求1或2所述的维生素E纳米乳,其特征在于:所述表面活性剂为蔗糖脂肪酸酯。
4.根据权利要求1或2所述的维生素E纳米乳,其特征在于,所述辛烯基琥珀酸可得然胶酯通过以下方法制备:取可得然胶,放入双锥干燥混合机中,然后取占可得然胶干重7%的辛烯基琥珀酸酐用无水乙醇稀释后喷入可得然胶中,混合均匀,回收乙醇后,加入占可得然胶干重5%的无水碳酸钠,并调整可得然胶的含水量达到25%,加热至60℃至反应完成,反应产物用乙醇洗涤3次后50℃烘干,过80目筛。
5.一种用于制备权利要求1至4任意一项所述的维生素E纳米乳的制备方法,其特征在于,包括以下步骤:
步骤Ⅰ,在配料罐中加入水,然后边搅拌边依次加入维生素E、蔗糖脂肪酸酯、辛烯基琥珀酸可得然胶酯;
步骤Ⅱ,开启高剪切乳化机对物料进行剪切乳化;
步骤Ⅲ,将已经乳化的物料泵入超高压纳米均质机,进行循环均质;
步骤Ⅳ,将均质好的物料泵入成品暂存罐中,开启搅拌,灌装得到成品。
6.根据权利要求5所述的维生素E纳米乳的制备方法,其特征在于:所述步骤Ⅱ中物料进行剪切分散乳化时,物料温度保持室温。
7.根据权利要求5所述的维生素E纳米乳的制备方法,其特征在于:所述步骤Ⅲ中物料进行均质时,物料温度保持室温。
8.根据权利要求5所述的维生素E纳米乳的制备方法,其特征在于:所述循环均质时,均质压力为120MPa。
9.根据权利要求5所述的维生素E纳米乳的制备方法,其特征在于:所述剪切乳化和循环均质的时长均为1h。
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