CN116531265A - 一种超分子微脂囊冻干球组合物及其制备方法和应用 - Google Patents
一种超分子微脂囊冻干球组合物及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种超分子微脂囊冻干球组合物及其制备方法和应用,包括超分子微脂囊冻干球组合物包括了油脂、活性物、超分子离子液体、磷脂、冻干保护剂、pH调节剂、去离子水的原辅料制备而来;利用超分子离子液体结合超分子微脂囊技术,将离子液体添加至油水两相及内外双层,冷冻干燥处理后制备得水油双相、微囊内外多重双保护的成型性强的超分子微脂囊冻干球;超分子微脂囊具备粒径小(0.01‑0.30μm),超分子微脂囊冻干球可与水任意比例快速混合均匀的优势,复溶效果好,透皮吸收强,应用便利,解决了冻干产品于化妆品领域中使用的局限性。
Description
技术领域
本发明涉及化妆品技术领域,特别涉及一种超分子微脂囊冻干球组合物及其制备方法和应用。
背景技术
现有的护肤品为了防止微生物滋生,合理地延长液体护肤品的保质期,通常在液体护肤品中添加防腐剂以确保液体护肤品在使用期间不会因各种污染而变质。但防腐剂具有一定的刺激性,长期使用含有防腐剂的液体护肤品,容易使皮肤老化、抗氧化能力降低,甚至出现过敏问题。研究表明,防腐剂是化妆品最主要的过敏原,减少防腐剂的使用可以大大提高产品的安全性。
冷冻干燥,全称真空冷冻干燥,简称冻干,是指把含有大量水分的物料预先进行降温,冻结成冰点以下的固体,在真空条件下使冰直接升华,从而去除水分得到干燥产品的一种技术。冷冻干燥在低温且真空下进行,一方面,对于许多热敏性或易氧化的物质特别适用,如活性蛋白、多肽和微生物制剂等,并且物质中的一些挥发性成分损失很小;另一方面,冷冻干燥过程中,微生物的生长和酶的作用无法进行,同时能排除95-99%以上的水份,干燥后活性物能长期保存不降解。再而,在冻结的状态下进行干燥,体积几乎不变,保持了原来的结构,不会发生浓缩现象。干燥后的物质疏松多孔,呈海绵状,加水后溶解迅速而完全,几乎立即恢复原来的性状。因此,冷冻干燥目前在医药工业、食品工业、科研和其他部门得到广泛的应用。
在护肤品领域,消费大众对冻干产品的外形有着较高的期待。目前市面上常见的冻干产品只能盛放在西林瓶中,包装材料单一,且冻干产品表面粗糙是一种碎渣碎粉状态,倒放和运输的过程中,由于西林瓶的滑动、滚动甚至碎裂,最终会使产品四散开来,不能满足消费者的对美观的追求;若盛放于常规包材,易因吸潮等原因而滋生微生物,无法长期保存;而常见的多肽类冻干球存在塑形差、易萎缩破碎的问题,常温下不稳定,不易保存;此外,部分冻干产品还存在复溶效果差、复溶不完全等问题,严重影响消费者体验。另外,冻干粉等产品形态单一,产品同质化严重,市场竞争非常激烈。
为了提高冻干球的结构稳定性,申请号为CN 110433086A的中国发明专利提出了以胶原蛋白复配甘露糖醇、普鲁兰多糖和透明质酸钠的冻干球骨架。以胶原蛋白为骨架主要成分,一方面确实大大提高了冻干球骨架的稳定性,但是另一方却引发了冻干球复溶性差的问题。申请号为CN 109350555A通过在重组胶原蛋白中加入透明质酸、海藻糖、甘露糖醇、出芽短梗霉多糖等材料提高重组胶原蛋白的成型性,但是海藻糖和甘露糖醇无法冻干成型,而单独使用透明质酸、海藻酸钠、出芽短梗霉多糖(普鲁兰糖)虽然能够冻干成球形,但是透明质酸、海藻酸钠冻干后的溶解性较差,容易形成凝胶状。
本发明意外发现,开创性地利用超分子离子液体结合超分子微脂囊技术将活性物进行包裹,利用超分子离子液体水油双亲的优势,将一部分离子液体添加至油相中,作为油相保护,同时将另一部分离子液体加入水相,结合微囊内外层保护,冷冻干燥处理后制备得水油双相、微囊内外多重双保护的成型性强的超分子微脂囊冻干球。所述制备方法适于规模化生产,所得冻干球以保持完整的球型结构,在25℃下存放和运输过程中不会坍塌,并且可以很好的保持活性物的结构和生物活性;所述超分子离子液体本身所具有的许多传统溶剂所无法比拟的优点及其作为绿色溶剂应用于有机及高分子物质的合成,离子液体无味、不燃,其蒸汽压极低,可减少因挥发而产生的环境污染问题;可操作温度范围宽,具有良好的冷热稳定性和化学稳定性,可以循环利用。另外,苦参碱类离子液体的苦参碱成分对真菌、球菌、杆菌有良好的抑制与杀灭作用。抑菌活性的研究表明,产品对多种真菌有显著的抑制作用,苦参生物碱除对许多病原真菌的菌丝生长和孢子萌发有抑制作用,不仅可抑制菌丝扩展,还可使病原菌碟上菌丝萎缩;还具有抗肿瘤、免疫调节、抗病毒、抗炎等药理作用。本发明提供了一种超分子微脂囊冻干球,使用的高压均质或微射流技术,制备过程即相当于灭菌过程,所得产品含菌量远远低于化妆品限度要求,结合抑菌超分子离子液体,可不添加防腐剂,实现了活性物的长期保鲜,绿色安全,超分子微脂囊具备粒径小,可与水任意比例快速混合均匀的优势,使得超分子微脂囊冻干球可在水中快速溶解,复溶效果好,透皮吸收效果强,使用方便。
发明内容
鉴于以上,本发明提供一种超分子微脂囊冻干球组合物的制备方法与应用,成功制备了一种超分子微脂囊冻干球,解决了冻干产品于化妆品领域中使用的局限性。
本发明提供了一种超分子微脂囊冻干球组合物的制备方法与应用,该超分子微脂囊冻干球组合物包括了油脂、活性物、超分子离子液体、磷脂、冻干保护剂、pH调节剂、去离子水的原辅料制备而来;
其中,所述的超分子微脂囊冻干球中的油脂含量为1.0-30.0%,所述油脂为灵芝孢子油、异十六烷、橄榄油、山茶油、霍霍巴籽油、葡萄籽油、白池花籽油、碳酸二辛酯、氢化聚异丁烯、山茶籽油、白芒花油、人参籽油、辛基十二烷醇、聚二甲基硅氧烷、角鲨烷、辛酸/癸酸甘油三酯、异壬酸异壬酯、肉豆蔻酸异丙酯、乳木果油、白池花籽油等任意一种及其组合。
其中,所述的超分子微脂囊冻干球中的活性物总含量为0.1-10.0%,所述的活性物为视黄醇及衍生物、茶多酚、胶原蛋白、弹性蛋白、泛醌、虾青素、苯乙基间苯二酚、维生素C、烟酰胺单核苷酸(NMN)、肌肽、棕榈酰多肽、乙酰基多肽、肉豆蔻多肽、胜肽、类蛇毒肽等任意一种及其组合。
其中,超分子微脂囊冻干球组合物中超分子离子液体含量为1.0-30.0%,所述超分子离子液体包括苦参碱己酸、苦参碱辛酸、苦参碱癸酸、苦参碱月桂酸、苦参碱肉豆蔻酸、苦参碱棕榈酸、甜菜碱甘油、甜菜碱丙二醇、甜菜碱丁二醇离子液体等任意一种及其组合,离子液体的加入可以降低传统冻干保护剂的使用用量,复溶后产品肤感更佳,消费者体验升级。
其中,所述的超分子微脂囊冻干球中的磷脂的含量为0.1-5.0%,所述磷脂为卵磷脂、氢化卵磷脂、大豆卵磷脂、蛋黄卵磷脂、合成磷脂、磷脂酰丝氨酸、磷脂酰肌醇、磷脂酰胆碱等任意一种及其组合。
其中,所述的超分子微脂囊冻干球中的传统冻干保护剂含量为0.1-20.0%,所述的冻干保护剂为多元醇、甘露糖醇、山梨糖醇、赤藓糖醇、肌醇、海藻酸钠、黄原胶、淀粉、纤维素、果胶、蔗糖、海藻糖、普鲁兰多糖、葡聚糖、壳聚糖、透明质酸钠、胶原蛋白、弹性蛋白、粘性蛋白、聚乙烯吡咯烷酮、聚乙二醇、羟丙基甲基纤维素及羟丙基环糊精等任意一种及其组合。
其中,所述的超分子微脂囊冻干球的pH调节剂为抗坏血酸、抗坏血酸葡糖苷、氢氧化钠、精氨酸、柠檬酸、盐酸中任意一种及其组合。
本发明提供了一种超分子组合物制备方法,请参阅图1,图1为本发明提供一种超分子微脂囊冻干球制备方法实施例的流程图,如图所示,其包括如下步骤:
(1)微脂囊油相:于惰性气体环境下,将配方量的脂溶性活性物、磷脂、油脂溶解于超分子离子液体中,加热至规定温度,搅拌使完全溶解且室温不析出;
(2)微脂囊水相(内层冻干保护):将配方量的水溶性活性物、超分子离子液体、传统冻干保护剂溶于去离子水中,配置成水相备用;
(3)微脂囊料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将(1)中油相加入到(2)当中,通过探头超声、高压均质或微射流处理后,得到超分子微脂囊;
(4)微脂囊外层冻干保护:将配方量的冻干保护剂溶于(3)中,并调至适宜pH,备用;
(5)冻干处理:将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
其中,作为优选方案,所述步骤(1)中活性物总含量与超分子离子液体的质量比为1:1~1:10,优选为1:10。
其中,步骤(1)、步骤(2)的温度条件为:40~80℃,优选为70~80℃。所述搅拌转速为100-1000rpm,优选500-800rpm,所述搅拌的时间为0.5~2h。
其中,探头超声优选条件为200-800W,3-5s开,3-5s关,超声10-30min,超声温度优选为40-60℃。
其中,高压均质机优选两步高压均质机,均质条件为:一级阀均质压力400-1500bar,优选600-1000bar;二级阀为0-200bar,优选50-150bar;均质次数2-15遍,优选6-10遍;均质温度0-80℃,优选为40-60℃。
其中,微射流的均质条件为压力400-1500bar,优选600-1000bar;均质次数2-15遍,优选6-10遍;均质温度0-80℃,优选为40-60℃。
其中,注入料液后的模具的冷冻定型温度为-20℃~-80℃,优选为-20~-30℃;时间为0.5h~24h,优选为10-12h。
其中,冻干的温度为-80℃~30℃;时间为10h~40h,优选为12h~24h。
本发明与现有技术相比,本发明公开了一种超分子微脂囊冻干球组合物的制备方法与应用,具有以下有益效果:
1、利用超分子离子液体结合超分子微脂囊技术,将离子液体添加至油水两相及内外双层,冷冻干燥处理后制备得水油双相、微囊内外多重双保护的成型性强的超分子微脂囊冻干球;
2、无防腐剂添加,制备过程即灭菌过程,协同超分子离子液体天然绿色抑菌,避免防腐剂刺激性;
3、显著提升冻干产品稳定性:稳定性强,储存方便,可任意包材,无需限定盛放于西林瓶也能长期保存;
4、超分子微脂囊具备粒径小(0.01-0.30μm),超分子微脂囊冻干球可与水任意比例快速混合均匀的优势,复溶效果好,透皮吸收强,应用便利;
本发明成功制备了一种超分子微脂囊冻干球,解决了冻干产品于化妆品领域中使用的局限性。
附图说明
图1为本发明的超分子微脂囊冻干球的制备方法较佳实施例的流程图;
图2为本发明的超分子微脂囊冻干球图;
图3为本发明的超分子微脂囊冻干球和现有售冻干球在水中复溶效果图;
图4为本发明的超分子微脂囊冻干球复溶后料液的粒径及PDI结果图;
图5为某品牌现有冻干球复溶后料液的粒径及PDI结果图;
图6为本发明的超分子微脂囊冻干球复溶后料液的透射电镜表征图;
图7为本发明的超分子微脂囊冻干球复溶后料液的粒径稳定性图;
图8为本发明的超分子微脂囊冻干球复溶后料液的含量稳定性图;
图9为本发明的超分子微脂囊冻干球复溶后料液与对比例1、2复溶后料体的4h时皮肤滞留总量对比结果图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。
应当理解,如图1至图9所示,此处所描述的具体实施例和对比例仅仅用以解释本发明,并不用于限定本发明。
一、实施例、对比例,下面通过实施例对本发明进一步说明。
实施例1
本实施例超分子HPR抗皱微脂囊冻干球的制备方法,包括以下步骤:
(1)微脂囊油相:于惰性气体环境下,将0.2%的羟基频哪酮视黄酸酯(HPR)、1%氢化大豆磷脂、2%辛酸/癸酸甘油三酯溶解于5%超分子离子液体苦参碱山茶油中,加热至规定温度60℃,搅拌使完全溶解且室温不析出;
(2)微脂囊水相:将0.1%的烟酰胺单核苷酸(NMN)、5%甘油、5%海藻糖、2%胶原蛋白、1%透明质酸、0.1%弹性蛋白、0.1%粘性蛋白、1%超分子离子液体苦参碱山茶油溶于去离子水中,配置成水相备用;
(3)微脂囊料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将(1)中油相加入到(2)当中,通过探头超声、高压均质或微射流处理后,得到超分子微脂囊;
(4)微脂囊外层冻干保护:将0.5%透明质酸钠溶于(3)中,并调至适宜pH,备用;
(5)将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
实施例2
本实施例超分子虾青素抗衰微脂囊冻干球组合物的制备方法,包括以下步骤:
(1)微脂囊油相:于惰性气体环境下,将0.5%的虾青素、2%大豆卵磷脂、5%角鲨烷溶解于5%超分子离子液体苦参碱己酸中,加热至规定温度60℃,搅拌使完全溶解且室温不析出;
(2)微脂囊水相:将5%丁二醇、5%甘露糖醇、2%胶原蛋白、1%透明质酸、1%超分子离子液体苦参碱己酸溶于去离子水中,配置成水相备用;
(3)微脂囊料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将(1)中油相加入到(2)当中,通过探头超声、高压均质或微射流处理后,得到超分子微脂囊;
(4)微脂囊外层冻干保护:将0.5%黄原胶溶于(3)中,并调至适宜pH,备用;
(5)将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
实施例3
本实施例超分子577美白微脂囊冻干球组合物的制备方法,包括以下步骤:
(1)微脂囊油相:于惰性气体环境下,将0.5%的4-丁基间苯二酚(577)、2%氢化卵磷脂、5%霍霍巴油溶解于5%超分子离子液体椰油苦参碱中,加热至规定温度60℃,搅拌使完全溶解且室温不析出;
(2)微脂囊水相:将0.5%的维生素C(VC)、0.5%a-熊果苷,5%丙二醇、5%山梨糖醇、2%胶原蛋白、1%透明质酸、1%超分子离子液体椰油苦参碱溶于去离子水中,配置成水相备用;
(3)微脂囊料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将(1)中油相加入到(2)当中,通过探头超声、高压均质或微射流处理后,得到超分子微脂囊;
(4)微脂囊外层冻干保护:将1%羟丙基甲基纤维素溶于(3)中,并调至适宜pH,备用;
(5)将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
实施例4
本实施例超分子多肽抗皱微脂囊冻干球组合物的制备方法,包括以下步骤:
(1)微脂囊油相:于惰性气体环境下,将0.1%的棕榈酰三肽-5、1%磷脂、5%白池花籽油溶解于5%超分子离子液体苦参碱月桂酸中,加热至规定温度60℃,搅拌使完全溶解且室温不析出;
(2)微脂囊水相:将0.1%的蓝铜肽、5%甘油、5%山梨糖醇、2%胶原蛋白、1%透明质酸、1%超分子离子液体苦参碱月桂酸溶于去离子水中,配置成水相备用;
(3)微脂囊料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将(1)中油相加入到(2)当中,通过探头超声、高压均质或微射流处理后,得到超分子微脂囊;
(4)微脂囊外层冻干保护:将1%壳聚糖溶于(3)中,并调至适宜pH,备用;
(5)将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
对比例1
将某品牌冻干球作为实施例1的对比示例:
对比例2未作超分子微脂囊处理的常规冻干球的制备
(1)油相:于惰性气体环境下,将0.2%的羟基频哪酮视黄酸酯(HPR)、1%氢化大豆磷脂、5%辛酸/癸酸甘油三酯,加热至规定温度60℃,搅拌使完全溶解且室温不析出;
(2)水相:将0.1%的烟酰胺单核苷酸(NMN)、5%甘油、5%海藻糖溶于去离子水中,配置成水相备用;
(3)料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将(1)中油相加入到(2)当中得到料液;
(4)料液外层冻干保护:将0.5%透明质酸钠溶于(3)中,并调至适宜pH,备用;
(5)将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
对比例3未作超分子微脂囊及冻干处理游离HPR溶液的制备
将0.2%的羟基频哪酮视黄酸酯(HPR)、5% CO 40、余量为94.8%的去离子水,搅拌使完全溶解且室温不析出,即得游离HPR溶液。
二、各实施例、对比例的外观、性能测试
1、产品复溶效果表征
分别用等量的去离子水对实施例1超分子HPR抗皱微脂囊冻干球及对比示例1某品牌现有冻干球进行复溶后,得到外观如图3所示,图中左为超分子微脂囊冻干球复溶后外观,即带淡蓝色乳光且均一透明的液体;图中右为某品牌现有冻干球复溶后外观效果,即使经搅拌仍见部分未完全溶解分散块状,且料体浑浊,室温放置4h后见分层。
图3备注:复溶后料液外观图可见因超分子微脂囊冻干球复溶后料体(左,实施例1)粒径为10-300nm范围内,复溶效果好,料液均一,呈现明显淡蓝色透明乳光;而某品牌现有冻干球(右,对比示例1)为微米级,且复溶效果差,且存在少量不溶物,呈现不透明浑浊料液。
以上表明,本发明超分子微脂囊冻干球具备与水任意比例快速混合均匀的优势,使得超分子微脂囊冻干球可在水中快速溶解,复溶效果好,应用便利;
2、产品表征
利用动态光散射法分别对实施例1制备得到的超分子HPR抗皱微脂囊冻干球、对比示例1某品牌现有冻干球用等量去离子水复溶后料液进行粒径及PDI检测。图4为实施例1的超分子HPR抗皱微脂囊冻干球复溶后料液的粒径及PDI检测结果图。图5为某品牌现有冻干球复溶后料液的粒径及PDI检测结果图。
利用透射电镜观察实施例1制备得到的超分子HPR抗皱微脂囊冻干球复溶后料体颗粒,图6为实施例1的超分子HPR抗皱微脂囊冻干球复溶后料体的透射电镜表征图。
表明,超分子微脂囊冻干球具备复溶前后颗粒粒径小(0.01-0.3μm),而某品牌现有冻干球复溶后粒径大于34μm,且见不溶物。显然地,超分子微脂囊冻干球可与水任意比例快速混合均匀的优势,复溶效果好,料体颗粒均一稳定,显著提升冻干产品稳定性,储存方便,可任意包材;
3、粒径稳定性检测
实施例1制备得到的超分子HPR抗皱微脂囊冻干球分别在-20℃、4℃、室温、45℃、光照条件下存放,检测其复溶后粒径稳定性,图7为实施例1的超分子HPR抗皱微脂囊冻干球的粒径稳定性检测图,从图7可知超分子微脂囊冻干球在不同温度条件下放置六个月,样品复溶后粒径稳定,说明超分子微脂囊技术可显著提高产品体系的稳定,并且不受储存条件的影响。
4、活性成份含量稳定性检测
实施例1制备得到的超分子HPR抗皱微脂囊冻干球分别在-20℃、4℃、室温、45℃、光照条件下存放,检测其HPR含量稳定性,图8为实施例1的超分子HPR抗皱微脂囊冻干球中HPR含量稳定性检测图,从图8可知超分子HPR抗皱微脂囊冻干球在不同温度条件下放置六个月,对比未进行包裹的游离的HPR,超分子微脂囊稳定性样品中HPR仅极少量降解,而未进行包裹的游离HPR,在45℃条件下放置六个月含量降解达50%以上,说明超分子微脂囊技术可显著提高活性物的稳定性,稳定性提高达6倍以上。
5、功效检测
图9为超分子微脂囊冻干球复溶后料液与对比例1、2复溶后料体的4h时皮肤滞留总量对比结果图,表明实施例1制备得到的超分子HPR抗皱微脂囊冻干球、对比例1某品牌现有冻干球、对比例2的未作超分子微脂囊技术处理的常规冻干球分别用等量去离子水复溶后,样品中HPR的体外皮肤滞留对比结果图;可见,超分子微脂囊冻干球可达3倍促渗效果,显著提升产品功效。
本发明与现有技术相比,本发明公开了一种超分子微脂囊冻干球组合物的制备方法与应用,具有以下有益效果:
1、开创性地利用超分子离子液体结合超分子微脂囊技术,将离子液体添加至油水两相及内外双层,冷冻干燥处理后制备得水油双相、微囊内外多重双保护的成型性强的超分子微脂囊冻干球;
2、无防腐剂添加,制备过程即灭菌过程,协同超分子离子液体天然绿色抑菌,避免防腐剂刺激性;
3、显著提升冻干产品稳定性:稳定性强,储存方便,可任意包材,无需限定盛放于西林瓶也能长期保存;
4、超分子微脂囊具备粒径小(0.01-0.30μm),超分子微脂囊冻干球可与水任意比例快速混合均匀的优势,复溶效果好,透皮吸收强,应用便利;
本发明成功制备了一种超分子微脂囊冻干球,解决了冻干产品于化妆品领域中使用的局限性。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解;其依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明实施例技术方案的范围,其均应涵盖在本发明的权利要求和说明书的范围当中。
Claims (10)
1.一种超分子微脂囊冻干球组合物,其特征在于,包括油脂、活性物、超分子离子液体、磷脂、冻干保护剂、pH调节剂、去离子水的原辅料制备而来,所述质量组分如下:所述油脂为1.0-30.0%,所述活性物总含量为0.1-10.0%,所述超分子离子液体含量为1.0-30.0%,所述油脂1.0-30.0%,所述磷脂为0.1-5.0%,所述冻干保护剂为0.1-20.0%,所述pH调节剂适量,余量为去离子水。
2.如权利要求1所述的超分子微脂囊冻干球组合物,其特征在于,所述活性物为视黄醇及衍生物、茶多酚、胶原蛋白、弹性蛋白、泛醌、虾青素、苯乙基间苯二酚、维生素C、烟酰胺单核苷酸(NMN)、肌肽、棕榈酰多肽、乙酰基多肽、肉豆蔻多肽、胜肽和类蛇毒肽中任意一种及其组合。
3.如权利要求1所述的超分子微脂囊冻干球组合物,其特征在于,所述超分子离子液体包括苦参碱己酸、苦参碱辛酸、苦参碱癸酸、苦参碱月桂酸、苦参碱肉豆蔻酸、苦参碱棕榈酸、甜菜碱甘油、甜菜碱丙二醇、甜菜碱丁二醇离子液体等任意一种及其组合。
4.如权利要求1所述的超分子微脂囊冻干球组合物,其特征在于,所述活性物与所述超分子离子液体的质量比为1:1~1:10。
5.如权利要求1所述的超分子微脂囊冻干球组合物,其特征在于,所述冻干保护剂为多元醇、甘露糖醇、山梨糖醇、赤藓糖醇、肌醇、海藻酸钠、黄原胶、淀粉、纤维素、果胶、蔗糖、海藻糖、普鲁兰多糖、葡聚糖、壳聚糖、透明质酸钠、胶原蛋白、弹性蛋白、粘性蛋白、聚乙烯吡咯烷酮、聚乙二醇、羟丙基甲基纤维素及羟丙基环糊精等任意一种及其组合。
6.如权利要求1所述的超分子微脂囊冻干球组合物,其特征在于,所述pH调节剂为抗坏血酸、抗坏血酸葡糖苷、氢氧化钠、精氨酸、柠檬酸、盐酸中任意一种及其组合。
7.如权利要求1所述的超分子微脂囊冻干球组合物,其特征在于,所述pH调节剂调节所述超分子微脂囊的pH范围为4.5~9.0。
8.一种超分子微脂囊冻干球组合物的制备方法,其特征在于,包括如下步骤:
(1)微脂囊油相:于惰性气体环境下,将配方量的脂溶性活性物、磷脂、油脂溶解于超分子离子液体中,所述活性物总含量与超分子离子液体的质量比为1:1~1:10,加热至规定温度,搅拌使完全溶解且室温不析出;
(2)微脂囊水相(内层冻干保护):将配方量的水溶性活性物、超分子离子液体、传统冻干保护剂溶于去离子水中,配置成水相备用;
(3)微脂囊料液制备:维持惰性气体氛围及温度,在剪切条件下缓慢将所述步骤(1)中的油相加入到所述步骤(2)中的水相当中,通过探头超声、高压均质或微射流处理后,得到超分子微脂囊;
(4)微脂囊外层冻干保护:将配方量的冻干保护剂溶于所述步骤(3)中的所述超分子微脂囊,并调至适宜pH,备用;
(5)冻干处理:将步骤(4)得到的料液过滤除菌后,注入模具内冷冻定型,脱模,冻干。
9.如权利要求8所述的超分子微脂囊冻干球组合物的制备方法,其特征在于,步骤(1)和步骤(2)的温度条件为:40~80℃,所述搅拌转速为100-1000rpm,所述搅拌的时间为0.5~2h;
所述探头超声条件为200-800W,3-5s开,3-5s关,超声10-30min,超声温度为40-60℃;
所述高压均质机均质条件为:一级阀均质压400-1500bar,二级阀为0-200bar,均质次数2-15遍,均质温度0-80℃;
所述微射流的均质条件为压力400-1500bar,均质次数2-15遍,均质温度0-80℃。
10.一种超分子微脂囊冻干球组合物的应用,其特征在于,应用于化妆品领域,所述超分子微脂囊冻干球可与水任意比例快速混合均匀的优势,复溶效果好,透皮吸收强,解决了冻干产品于化妆品领域中使用的局限性。
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