CN112168757B - 一种含有螺旋藻多糖提取物的组合物的制备方法 - Google Patents
一种含有螺旋藻多糖提取物的组合物的制备方法 Download PDFInfo
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- CN112168757B CN112168757B CN202011142910.5A CN202011142910A CN112168757B CN 112168757 B CN112168757 B CN 112168757B CN 202011142910 A CN202011142910 A CN 202011142910A CN 112168757 B CN112168757 B CN 112168757B
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Abstract
本发明公开了一种含有螺旋藻多糖提取物的组合物的制备方法，A相原料加热溶解，B相原料加热融化后加入A相中，边加边搅拌，均质，再在搅拌过程中依次加入C相原料，均质，搅拌，即得，A相包括：辛酸葵酸甘油三酯、CreamMaker‑Blead、GelmakerEMU、维E醋酸酯；或包括：荷荷巴油、CreamMaker‑Blead、鳄梨油、鲸蜡硬脂醇、维E醋酸酯、GelmakerEMU；B相包括：甘油、透明质酸钠、去离子水；或包括：甘油、透明质酸钠、吡咯烷酮羧酸钠、1，3‑丁二醇、去离子水；C相包括：螺旋藻提取物、密蒙花提取物、葡萄籽提取物、春榆提取物、积雪草苷提取物、苄醇‑DHA、香精。本发明产品具有较好的耐热、耐寒等稳定特性，对DPPH和·OH具有较好的清除功效，保湿性较好。
Description
技术领域
本发明涉及螺旋藻多糖提取物制品的制备方法，特别涉及一种含有螺旋藻多糖提取物的组合物的制备方法。
背景技术
随着科技的进步，越来越多的电子产品的问世，人们也过多的暴露在蓝光环境中。与紫外线相比，蓝光具有更强的穿透力，可直达人体皮肤真皮层，从而对皮肤造成损伤。比如氧化压力、色素沉着等，此外还会引起视网膜细胞的损伤，造成视力下降甚至丧失。蓝光造成的伤害也使得抗蓝光产品越来越受到人们的追捧。
螺旋藻中含有丰富的多糖、蛋白质、氨基酸、维生素、类胡萝卜素、γ-亚麻酸、无机元素Na、K、Ca、Mg以及微量元素Fe、Co、Mn、Ni、Cr、V、Zn、Se、Cu等。螺旋藻中的螺旋藻多糖具有抗辐射损伤和改善放、化疗引起的副作用，并通过增强机体免疫力，间接抑制癌细胞的增生。另外螺旋藻多糖能提高血浆中的SOD的活性，降低脂质过氧化，减少组织脂褐质的形成，有利于机体的延缓衰老作用。
护肤乳霜能给皮肤补充适当的油脂；有较好的保湿性能，防止皮肤开裂；对皮肤无刺激性，可安全使用；有较好的铺展性及渗透性；各种营养添加剂能有效的渗透于角质层，本发明中复配多种中药提取物，无毒无刺激，不会对肌肤造成伤害；产品在使用中和使用后具有悦人的肤感及香气。
发明内容
发明目的：本发明目的是提供具有保湿性能、清除DPPH、·OH等功效的含有螺旋藻多糖提取物的组合物的制备方法。
技术方案：本发明提供一种含有螺旋藻多糖提取物的组合物的制备方法，包括如下步骤：
A相原料加热溶解，B相原料加热融化后加入A相中，边加边搅拌，均质，再在搅拌过程中依次加入C相原料，均质，搅拌，即得，
所述A相原料包括：辛酸葵酸甘油三酯、CreamMaker-Blead、GelmakerEMU、维E 醋酸酯；或包括：荷荷巴油、CreamMaker-Blead、鳄梨油、鲸蜡硬脂醇、维E醋酸酯、GelmakerEMU；
所述B相原料包括：甘油、透明质酸钠、去离子水；或包括：甘油、透明质酸钠、吡咯烷酮羧酸钠、1，3-丁二醇、去离子水；
所述C相原料包括：螺旋藻提取物、密蒙花提取物、葡萄籽提取物、春榆提取物、积雪草苷提物、苄醇-DHA、香精。
进一步地，所述螺旋藻提取物是将螺旋藻粉末用超纯水配成水溶液制得。
进一步地，所述螺旋藻粉末的制备方法如下：
提取：取螺旋藻粉末加入去离子水溶解，冷冻、超声、恒温回流提取、离心、浓缩、醇沉、冷冻干燥，得粗多糖沉淀；
脱色：将粗多糖沉淀用超纯水溶解成溶液，加入双氧水，反应，醇沉，离心，将沉淀用有机溶剂洗涤，干燥。
进一步地，所述透明质酸钠是用酶切寡聚透明质酸配成的水溶液。
进一步地，得到的产品具有清除DPPH和·OH的功效。
进一步地，得到的产品具有保湿的功效。
上述技术方案中：
密蒙花提取物：密蒙花中含有黄酮类，挥发油，三萜类，环烯醚萜苷类等多种化学成分，具有抗氧化，抗炎，免疫调节等作用，能够强效应对紫外线，蓝光，红外所产生的红斑、氧化压力。将其应用于护肤品中，可作为护肤品中的抗氧化剂。
春榆提取物：提取自榆树的根皮部，富含天然来源的半乳糖、鼠李糖、葡萄糖、氨基葡萄糖、海藻糖等多糖，能抑制透明质酸酶的活性，减少经皮水分流失，可作为护肤品的强效保湿剂和抗衰老剂。同时能抑制IL-8/IL-6和PEG2的释放，具有良好的抗炎功效，有助于清洁皮肤，防止暗疮。此外，春榆提取物也能修复UVA照射引起的光损伤，提高细胞的存活能力。
葡萄籽提取物：主要是由原花青素＝儿茶素，表儿茶素，没食子酸，表儿茶素没食子酸酯等多份类物质组成。它是从葡萄籽中提取的纯天然物质，是迄今发现的植物来源最高效的抗氧化剂之一，其抗氧化效果是维生素C和维生素E的30-50倍，同时其含有的原花青素具有很强的自由基清除能力。
积雪草苷提取物：主要成分为积雪草苷，具有抗炎，滋润肌肤的作用，可以让肌肤变得更加光滑细腻，同时它还可以祛除肌肤废旧角质层，促进肌肤新陈代谢，增加肌肤弹性将其应用于护肤品中，能使皮肤柔润，舒缓，镇静。
有益效果：本发明制备的护肤品中以螺旋藻多糖为主要提取物同时复配多种中药提取物，无毒无刺激，不会对肌肤造成伤害，促进肌肤的新陈代谢，对皮肤有良好的保湿柔润性。本发明产品具有较好的耐热、耐寒等稳定特性，以不同的中药提取物复配，更大效果地发挥作用作用：通过清除自由基，降低脂质过氧化阻挡蓝光对皮肤的损伤，延缓由于皮肤氧化而导致的衰老。
附图说明
图1为本发明的乳霜产品，左图为乳霜*1、右图为乳霜*2；
图2依次为本发明乳霜产品离心、耐热、耐寒、冷热循环的实验结果图，其中左图为乳霜1的离心、耐热、耐寒、冷热循环实验结果，右图为乳霜2的离心、耐热、耐寒、冷热循环的实验结果；
图3为螺旋藻提取物对DPPH、·OH的清除实验结果图；
图4为春榆根提取物对DPPH、·OH的清除实验结果图；
图5为密蒙花提取物对DPPH、·OH的清除实验结果图；
图6为葡萄籽提取物对DPPH、·OH的清除实验结果图；
图7为本发明的乳霜产品保湿性能测试结果。
具体实施方式
实施例1：螺旋藻多糖粉末的制备：
提取：
1.称量：称取10.00g螺旋藻粉末于500ml烧杯中
2.溶解：按1∶25(g/ml)的料液比加入去离子水于烧杯中
3.冷冻，解冻处理：在-20℃冷冻4h，取出。然后在37℃水浴下解冻，如此重复3次
4.超声：解冻完成，在80Hz条件下超声15min
5.提取：超声结束后，再于90℃恒温回流提取提3h，
6.离心：提取液在3000r/min离心10min，取上清液
7.浓缩：提取液在70℃减压浓缩，得浓缩液
8.醇沉：然后用5倍浓缩液体积的95％乙醇醇沉过夜，3000r/min离心10min，取沉淀， -40℃真空冷冻干燥，即得粗多糖沉淀。
脱色：
9.将粗多糖沉淀用超纯水溶解成溶液，
10.按照6％的比例向其中加入浓度为30％的双氧水
11.调pH为4
12.于50℃的恒温水浴中反应7h，后静置，过滤
13.加入3倍体积的无水乙醇，醇沉36h，
14.后4000G离心10min后倒掉上层清液，取沉淀。
15.并将沉淀用无水乙醇，甲醇，丙酮各洗涤3次，挥发溶剂，在50℃烘箱干燥即可。
实施例2：乳霜的制备：
原料：
辛酸葵酸甘油三酯：购自Making Cosmetics网站(商品名为Triglyceride)
生育酚乙酸酯：购自Making Cosmetics网站(商品名为Vitamin E(dl-alphatocopheryl acetate)
硬脂酸甘油酯，聚乙二醇-100硬脂酸酯：购自Making Cosmetics网站(商品名为
BLEND)
丙烯酸钠/丙烯酰二甲酯牛磺酸钠共聚物、异十六烷、聚山梨醇酯80：购自MakingCosmetics网站(商品名为
EMU)
荷荷巴油：购自Making Cosmetics网站(商品名为Jojoba Oil，USDA CertifiedOrganic)
鳄梨油：购自Making Cosmetics网站(商品名为Avocado Butter)
甘油：购自Making Cosmetics网站(商品名为Glycerin)
鲸蜡硬脂醇：购自源叶生物
吡咯烷酮羧酸钠：购自源叶生物
酶切寡聚透明质酸钠：购自华熙福瑞达生物医药有限公司
1，3-丁二醇：购自麦克林
春榆根提取液：购自SK bioland(商品名为PF ULMUS EXTRACT)
葡萄籽提取液：购自广州佰宇生物科技有限公司
积雪草苷提取液：购自亚马逊网站GOTU KOLA
密蒙花提取物：购自上海百好博生物科技有限公司(商品名为SOLIBERINE)
苄醇、脱氢乙酸：购自Making Cosmetics网站(商品名为Benzylalcohol-DHA)
香精：购自芬豪香精香料有限公司
溶液的配制：将螺旋藻粉末用超纯水配成0.5％的水溶液，酶切寡聚透明质酸配成1％的水溶液，备用。
表1
制备：将A相原料加入消毒烧杯中，置于80-90℃水浴锅中搅拌直至原料溶解，将B相加热至80-90℃以融化成分，保温5-10min，将B相缓慢加入A中，边加边搅拌，然后立即在10000r/min下的均质机下均质3-5min，当温度低于54℃时，在搅拌过程中加入依次C相，再在均质机下均质1-2mim，然后转移到锡膏搅拌机下搅拌10min即得。产品见图1。
实施例3：稳定性试验，见图2
离心试验：
过程：将样品装入带有10ml刻度的离心管中约2/3的高度，并装实，用盖子塞好，然后放入预先调节到40℃的电热恒温培养箱内，保温1h后，两支离心管相对放入离心机中保持平衡，以转速2000r/min，离心30min，观察有无油水分层，颗粒的现象。
结果：无油水分层，无颗粒。
耐热试验：
过程：将样品装入封口的离心管中，在恒温箱中设定温度为40℃下放置24h，然后恢复室温观察液体变色、油水分层情况。
结果：无油水分层，无颗粒。
耐寒试验
过程：将样品装入封口的离心管中，放入-20℃以下的冰箱中放置24h，然后恢复室温观察液体有无变粗、变色、分层情况。。
结果：无油水分层，无变粗、变色。
冷热循环试验：
过程：将样品装入密闭的样品瓶中，在恒温箱(冰箱)内放置24h后取出恢复室温，再放入冰箱(恒温箱)24h。如此反复，直至所测样品出现油水分层、变化或渗油等现象，重复两次。
结果：无油水分层，无变粗、变色。
PH测定
直测法，设置三个重复组
表2
| 霜*1 | 霜*2 |
| 6.46 | 6.51 |
实施例4：功效性评价(单因素试验)，见图3-6
DPPH清除试验：DPPH无水乙醇溶液：0.05mg/mlDPPH无水乙醇溶液
不同浓度样品溶液：
螺旋藻提取物：0.25，0.50，0.75，1.00，1.25，，1.50(mg/ml)
春榆根提取物：1％，2％，3％、4％、5％、6％
密蒙花提取物：0.02％，0.04％、0.06％、0.08％、0.10％、0.12％
葡萄籽提取物：0.1％、0.2％、0.3％、0.4％、0.5％、0.6％
样品组：2ml样品溶液+2mlDPPH溶液，混匀，避光保存30min，517nm下测Aa
本底组：2ml超纯水+2ml样品溶液，混匀，避光保存30min，517nm下测Ab
空白组：2ml超纯水+2mlDPPH溶液，混匀，避光保存30min，517nm下测Ac IP＝[1-(Aa-Ab)/Ac]x100％
·OH清除试验：
(1)水杨酸溶液的配制：分析天平称取0.0622g水杨酸固体粉末，无水乙醇溶解定容至100mL容量瓶中备用；
(2)硫酸亚铁溶液的配制：分析天平称取0.1251g七水合硫酸亚铁固体粉末，用超纯水溶解定容至100mL容量瓶中备用；
(3)双氧水的配制：吸取0.17mL 30％的双氧水，超纯水定容于100mL容量瓶中备用。
(4)不同浓度样品溶液的配制：
螺旋藻提取物：0.50，1.00，1.50，2.00，2.50，3.00(mg/ml)
春榆根提取物：2％、4％，6％、8％、10％、12％
密蒙花提取物：1％，2％、3％、4％、5％、6％
葡萄籽提取物：2％，4％，6％、8％、10％、12％
水浴锅37℃下反应30min，在波长为510nm处测定混合液的吸光度，用超纯水做对比。
羟基自由基的清除率IP＝[1-(Aa-Ab)/Ac]x100％
式中：Aa-1.00mL水杨酸，1.00mL七水硫酸亚铁，1.00mL不同浓度的多糖提取液，1.00mL双氧水；
Ab-1.00mL水杨酸，1.00mL七水硫酸亚铁，1.00mL不同浓度的多糖提取液，1.00mL二次蒸馏水；
Ac-1.00mL水杨酸，1.00mL七水硫酸亚铁，1.00mL二次蒸馏水， 1.00mL双氧水。
保湿性能考察，见图7
方法：分别取200mg的样品 (霜1，霜2，1％甘油水溶液，1％透明质酸钠水溶液，去离子水)
均匀涂敷于培养皿中，上面封一层透气膜，置于37℃恒温干燥箱内，2、4、6、8h后称重，每组设置3个重复
保湿率(％)＝M1/M2×100％
M1--放置前水分质量(mg)M2--放置后水分质量(mg)。
Claims (6)
1.一种含有螺旋藻多糖提取物的组合物的制备方法，其特征在于：A相原料加热溶解，B相原料加热融化后加入A相中，边加边搅拌，均质，再在搅拌过程中依次加入C相原料，均质，搅拌，即得，
所述A相原料包括：辛酸癸酸甘油三酯、CreamMaker-Blead、GelmakerEMU、维E醋酸酯；或包括：荷荷巴油、CreamMaker-Blead、鳄梨油、鲸蜡硬脂醇、维E醋酸酯、GelmakerEMU；
所述CreamMaker-Blead为硬脂酸甘油酯和聚乙二醇-100硬脂酸酯；
所述GelmakerEMU为丙烯酸钠/丙烯酰二甲酯牛磺酸钠共聚物、异十六烷和聚山梨醇酯80；
所述B相原料包括：甘油、透明质酸钠 、去离子水；或包括：甘油、透明质酸钠、吡咯烷酮羧酸钠、1,3-丁二醇、去离子水；
所述C相原料包括：螺旋藻提取物、密蒙花提取物、葡萄籽提取物、春榆提取物、积雪草苷提取物、苄醇和脱氢乙酸、香精。
2.根据权利要求1所述的含有螺旋藻多糖提取物的组合物的制备方法，其特征在于：所述螺旋藻提取物是将螺旋藻粉末用超纯水配成水溶液制得。
3.根据权利要求2所述的含有螺旋藻多糖提取物的组合物的制备方法，其特征在于：所述螺旋藻粉末的制备方法如下：
提取：取螺旋藻粉末加入去离子水溶解，冷冻、超声、恒温回流提取、离心、浓缩、醇沉、冷冻干燥，得粗多糖沉淀；
脱色：将粗多糖沉淀用超纯水溶解成溶液，加入双氧水，反应，醇沉，离心，将沉淀用有机溶剂洗涤，干燥。
4.根据权利要求1所述的含有螺旋藻多糖提取物的组合物的制备方法，其特征在于：所述透明质酸钠是用酶切寡聚透明质酸配成的水溶液。
5.根据权利要求1所述的含有螺旋藻多糖提取物的组合物的制备方法，其特征在于：得到的产品具有清除DPPH和·OH的功效。
6.根据权利要求1所述的含有螺旋藻多糖提取物的组合物的制备方法，其特征在于：得到的产品具有保湿的功效。
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