CN114939072B - 一种保湿修护冻干乳及其制备方法 - Google Patents
一种保湿修护冻干乳及其制备方法 Download PDFInfo
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- A—HUMAN NECESSITIES
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- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Public Health (AREA)
- Veterinary Medicine (AREA)
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
Abstract
本发明公开了一种保湿修护冻干乳及其制备方法,包括按重量份计的有效成分:润肤剂0.1‑10份;乳化剂0.1‑4份;赋形剂1‑8份;润肤剂包括异十六烷和番茄籽油;制备方法包括,水相混合步骤:将水相的有效成分混合,加热至80‑85℃并混匀,得到水相混合料;油相混合步骤:将油相的有效成分混合,加热至80‑85℃并混匀,得到油相混合料;冻干步骤:将油相混合料加入水相混合料中,均质然后在温度≤‑40℃条件下真空冷冻干燥处理,得到保湿修护冻干乳;保湿修护冻干乳以番茄籽油和异十六烷按照比例复配,能完全互溶,制得的油相粘度低,易于乳化,制备的乳化体稳定性好。
Description
技术领域
本发明涉及一种保湿修护冻干乳及其制备方法,属于皮肤产品技术领域。
背景技术
冻干技术是采用冷冻干燥机的真空冷冻干燥法,预先将液体里面的水分冻结,然后在真空无菌的环境下将液体里面被冻结的水分升华,冷冻干燥而成的无菌粉体。冻干粉可以很好地保存溶液中的活性成分,同时不含防腐剂,因此冻干粉类产品受到了众多消费者的喜爱。但是目前的冻干粉都是用水溶性原料制备而成,而将冻干技术用于护肤产品领域的话,由于皮肤具有疏水性屏障作用,水溶性原料制备的冻干粉透皮吸收有限,大部分功效成分会停留在皮肤表面,不能发挥最好的功效。
市面上的皮肤修护冻干粉中包括D-甘露糖醇、海藻糖、普鲁兰多糖、寡肽、丁公藤提取物、玄参提取物等都是水溶性成分,难以突破皮肤屏障,发挥最大的功效。
另外还有脂溶性维生素冻干乳剂,脂溶性维生素为油溶性,制备成注射用的冻干乳。该冻干乳添加的油溶性成分为维生素A、维生素D2、维生素E和维生素K1,粘度比较大,比较难乳化。因此该脂溶性维生素冻干乳剂的制备用到了能调节匀化压力的均质仪,普通的化妆品工厂不具备这种生产条件。
其他一些冻干乳制备用到超低温冰箱和真空冷冻干燥箱,生产效率低,难以大规模生产。
发明内容
为了克服现有技术的不足,本发明的第一个目的在于提供一种保湿修护冻干乳,以番茄籽油和异十六烷按照比例复配,能完全互溶,制得的油相粘度低,易于乳化,制备的乳化体稳定性好。
本发明的第二个目的在于提供一种上述保湿修护冻干乳的制备方法,其制备工序简单高效,冻干过程中成分之间能够很好地融合,并保留有良好的护肤效果。
实现本发明的第一个目的可以通过采取如下技术方案达到:一种保湿修护冻干乳,包括按重量份计的以下有效成分:
润肤剂 0.1-10份;
乳化剂 0.1-4份;
赋形剂 1-8份;
润肤剂包括异十六烷和番茄籽油。
进一步地,异十六烷和番茄籽油的重量份按保湿修护冻干乳重量份计为:
异十六烷 1-3份;
番茄籽油 0.1-2份。
进一步地,润肤剂还包括矿油、鲸蜡醇乙基己酸酯、植物甾醇油酸酯和霍霍巴籽油中的至少一种。
进一步地,乳化剂包括卵磷脂和氢化卵磷脂;卵磷脂和氢化卵磷脂的重量份按保湿修护冻干乳重量份计为:
卵磷脂 0.1-0.8份;
氢化卵磷脂 0.1-0.8份。
进一步地,赋形剂包括甘露聚糖。
进一步地,保湿修护冻干乳还包括按重量份计的皮肤调理剂0.1-10份。
进一步地,皮肤调理剂包括透明质酸钠和海藻糖;透明质酸钠和海藻糖的重量份按保湿修护冻干乳重量份计为:
透明质酸钠 0.01-0.1份;
海藻糖 0.1-2份。
进一步地,保湿修护冻干乳还包括按重量份计的pH调节剂0.1-0.8份。
进一步地,pH调节剂包括磷酸氢二钠和磷酸二氢钠;磷酸氢二钠和磷酸二氢钠的重量份按保湿修护冻干乳重量份计为:
磷酸氢二钠 0.1-0.15份;
磷酸二氢钠 0.1-0.2份。
实现本发明的第二个目的可以通过采取如下技术方案达到:一种如上所述的保湿修护冻干乳的制备方法,包括,
水相混合步骤:将水相的有效成分混合,加热至80-85℃并混匀,得到水相混合料;
油相混合步骤:将油相的有效成分混合,加热至80-85℃并混匀,得到油相混合料;
冻干步骤:将油相混合料加入水相混合料中,均质然后在温度≤-40℃条件下真空冷冻干燥处理,得到保湿修护冻干乳。
相比现有技术,本发明的有益效果在于:
1、本发明保湿修护冻干乳以番茄籽油和异十六烷按照比例复配,能完全互溶,制得的油相粘度低,易于乳化,制备的乳化体稳定性好;
2、本发明保湿修护冻干乳具有好的保湿修护功效的油溶性成分,保湿修护效果明显;
3、本发明制备方法以冻干的制备技术应用于护肤品制备领域,其成分以番茄籽油、异十六烷和乳化剂、赋形剂配合,其制备工序简单高效,冻干过程中成分之间能够很好地融合,并保留有良好的护肤效果。
具体实施方式
下面,结合具体实施方式,对本发明做进一步描述:
一种保湿修护冻干乳,包括如表格1所示按重量份计的以下有效成分:
表格1保湿修护冻干乳的有效成分
保湿修护冻干乳的制备方法包括,
水相混合步骤:将甘露聚糖、透明质酸钠、海藻糖、磷酸氢二钠、磷酸二氢钠和水83.95-97.75份加入真空乳化锅中,搅拌加热至80-85℃并混匀,保温得到水相混合料;
油相混合步骤:将异十六烷、番茄籽油、卵磷脂、氢化卵磷脂加入油相锅中混合,搅拌加热至80-85℃并混匀,保温得到油相混合料;
冻干步骤:将油相混合料加入水相混合料中,3000r/min均质6min,保温搅拌30min,冷却出料;分装在5mL西林瓶中,在温度≤-40℃条件下真空20Pa冷冻干燥处理40h,真空条件下压塞,得到保湿修护冻干乳。
异十六烷可以在皮肤上形成一层阻挡屏障以防止水分散失。异十六烷表面张力低,粘度低,极易铺展和被乳化,与常见油脂的相容性好,能增进不同体系间的相容性,提高乳化体的稳定性。
番茄(SOLANUM LYCOPERSICUM)籽油富含不饱和脂肪酸(尤其是亚油酸)、天然番茄红素、维生素E及β-胡萝卜素等成分,能滋润皮肤、促进表皮角质细胞增殖、活化组织蛋白酶,增强皮肤细胞新陈代谢,有很好的保湿修护功效。
但是番茄籽油比较粘稠,不易乳化。番茄籽油和异十六烷按照以上比例复配,能完全互溶,制得的油相粘度低,易于乳化,制备的乳化体稳定性好。
实施例1-3和对比例1-5:
实施例1-3和对比例1-5的成分和重量份如表格2所示:
表格2保湿修护冻干乳的成分(重量份)
保湿修护冻干乳的制备方法包括,
水相混合步骤:将甘露聚糖、透明质酸钠、海藻糖、磷酸氢二钠、磷酸二氢钠和水加入真空乳化锅中,搅拌加热至80-85℃并混匀,保温得到水相混合料;
油相混合步骤:将异十六烷/异十二烷、番茄籽油、卵磷脂、氢化卵磷脂、生育酚乙酸酯加入油相锅中混合,搅拌加热至80-85℃并混匀,保温得到油相混合料;
冻干步骤:将油相混合料加入水相混合料中,3000r/min均质6min,保温搅拌30min,冷却出料;分装在5mL西林瓶中,在温度≤-40℃条件下真空20Pa冷冻干燥处理40h,真空条件下压塞,得到保湿修护冻干乳。
对于对比例1、3以异十二烷代替异十六烷;对比例2、3省略番茄籽油,添加生育酚乙酸酯;对比例4为空白对照;对比例5省略异十六烷。
对于实施例1-3和对比例1-5的保湿修护冻干乳,加入5mL去离子水溶解后,根据GB/T29665-2013进行理化指标检测,结果如表格3所示:
表格3实施例1-3和对比例1-5的理化指标
耐热要求(40±1)℃保持24h,恢复至室温后与试验前无明显性状差异;
耐寒要求(﹣5±1)℃保持24h,恢复至室温后与试验前无明显性状差异;
离心要求2000r/min,30min不分层。
由表格3可以得知,本发明实施例1-3和对比例1-4制备的保湿修护冻干乳理化性质符合要求,对比例5单独添加番茄籽油制备的冻干乳耐寒和离心不合格。说明异十六烷能分散好番茄籽油,使油相更易乳化,制备的保湿修护冻干乳的理化性质符合要求。
检测:
一、产品安全性试验:
根据《化妆品安全技术规范2015》中描述的方法对实施例和对比例进行人体斑贴测试。
1、实验人群:共28人,女21人,男7人,年龄21-59,每组4人,符合受试者志愿入选标准;
2、测试方法:选择面积不超过50mm2,深度约为1mm的合适斑试器,以封闭式斑贴测试试验方法,将受试物约0.020-0.025mL加于斑试器内。将斑试器贴敷于受试者前臂曲侧,24h后去除受试物,分别于去除后0.5、24、48h观察皮肤反应,按《化妆品安全技术规范2015》中皮肤反应分级标准记录其结果。
3、试验结果:实施例1-3和对比例1-4受试者移除斑贴后3个观察时间点0.5h、24h、48h评分等级为0分(阴性反应)。
二、保湿功效测试:
1、实验人群:共7人,女5人,男2人,年龄21-59,符合受试者志愿入选标准;
2、测试方法:在温度为25℃,相对湿度50%的环境下,分布将实施例1-3和对比例1-4制备的保湿修护冻干乳均匀涂抹在4×4cm2方形无纺棉上,然后敷在脸上,分别测试在贴敷30min、1h、2h、3h敷贴区的皮肤水分含量,水分含量测试采用水分含量测试仪(Corneometer CM825),研究不同时间皮肤水分含量的增长率,皮肤水分含量的增长率=(测试值-空白值)/空白值×100%,结果如表格4所示。
表格4皮肤含水量的增长率
由表格4数据可知,本发明实施例1-3制备的保湿修护冻干乳保湿功效明显好于对比例1-4,说明番茄籽油和异十六烷按特定比例配合,能明显提升保湿修护冻干乳的保湿效果。
三、修护功效测试:
1、试验对象:选取70只雌性Wistar大鼠,体重为250g。
2、试验方法:将70只大鼠随机分为7组,分别为实施例1组、实施例2组、实施例3组、对比例1组、对比例2组、对比例3组、对比例4组,每组10只。
在大鼠背部脊柱两侧旁lcm,头尾两端平行于脊柱各标记一个半径1cm,面积3.14cm2的圆形切口线。经碘伏消毒皮肤后,用剪刀沿标记线剪除全层皮肤至深筋膜,形成圆形创伤面。左侧分别使用加入5mL去离子水溶解后的实施例1-3、对比例1-4冻干乳,右侧创伤不进行处理作为对照组,均用纱布覆盖包扎,连续观察9天。
3、试验结果:
在连续9天中,观察小鼠的平均创伤面积相对于第一天创伤面积的大小,具体结果如表格5所示。
表格5平均创伤面积(%)
如表格5所示:实施例1-3在异十六烷、番茄籽油复配的情况下,保湿和修护效果明显好于对比例1-3。其中,对比例1用异十二烷替代异十六烷,可以制备理化性质符合要求的保湿修护冻干乳,但是因为异十二烷分子量小,挥发性强于异十六烷,保湿修护效果弱于实施例。对比例2是用生育酚乙酸酯代替番茄籽油,可以制备理化性质符合要求的保湿修护冻干乳,但保湿修护效果弱于实施例。对比例4未添加油溶成分,保湿和修护效果更差。说明在本发明的比例下,异十六烷能分散好番茄籽油,降低油相粘度,使得油相易于乳化,能发生协同作用,制备的冻干保湿修护冻干乳理化性质符合要求,且具有良好的保湿和修护功效。
对于本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及变形,而所有的这些改变以及变形都应该属于本发明权利要求的保护范围之内。
Claims (3)
1. 一种保湿修护冻干乳,其特征在于包括按重量份计的以下有效成分:
异十六烷1-3份
番茄籽油0.1-2份
卵磷脂0.1-0.8份
氢化卵磷脂0.1-0.8份
甘露聚糖1-8份
透明质酸钠0.01-0.1份
海藻糖0.1-2份
磷酸氢二钠0.1-0.15份
磷酸二氢钠0.1-0.2份
保湿修护冻干乳不含防腐剂;
所述保湿修护冻干乳通过以下方法制备得到:水相混合步骤:将甘露聚糖、透明质酸钠、海藻糖、磷酸氢二钠、磷酸二氢钠和水83.95-97.75份加入真空乳化锅中,搅拌加热至80-85℃并混匀,保温得到水相混合料;
油相混合步骤:将异十六烷、番茄籽油、卵磷脂、氢化卵磷脂加入油相锅中混合,搅拌加热至80-85℃并混匀,保温得到油相混合料;
冻干步骤:将油相混合料加入水相混合料中,3000r/min均质6min,保温搅拌30min,冷却出料;分装在5mL西林瓶中,在温度≤-40℃条件下真空20Pa冷冻干燥处理40h,真空条件下压塞,得到保湿修护冻干乳。
2.如权利要求1所述的保湿修护冻干乳,其特征在于,所述保湿修护冻干乳还包括矿油、鲸蜡醇乙基己酸酯、植物甾醇油酸酯和霍霍巴籽油中的至少一种。
3.一种如权利要求1所述的保湿修护冻干乳的制备方法,其特征在于包括,
水相混合步骤:将甘露聚糖、透明质酸钠、海藻糖、磷酸氢二钠、磷酸二氢钠和水83.95-97.75份加入真空乳化锅中,搅拌加热至80-85℃并混匀,保温得到水相混合料;
油相混合步骤:将异十六烷、番茄籽油、卵磷脂、氢化卵磷脂加入油相锅中混合,搅拌加热至80-85℃并混匀,保温得到油相混合料;
冻干步骤:将油相混合料加入水相混合料中,3000r/min均质6min,保温搅拌30min,冷却出料;分装在5mL西林瓶中,在温度≤-40℃条件下真空20Pa冷冻干燥处理40h,真空条件下压塞,得到保湿修护冻干乳。
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