CN114469816B - 抗氧化植物精华护肤乳液及其制备方法 - Google Patents
抗氧化植物精华护肤乳液及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗氧化植物精华护肤乳液，包括以下原料：霍霍巴油2～4％、角鲨烷1.5～2％、烟酰胺0.35～0.5％、聚甘油硬脂酸酯0.5～1％、生育酚乙酸酯1.5～2％、甘油10～12％、尼泊金甲酯0.05～0.1％、尿囊素0.2～0.3％、甘露聚糖0.2～0.5％、红麻叶提取物3～5％、余量为水。本发明制备得到的乳液美白紧致效果好且以纯天然的植物配方为主；本发明还使用了掺杂氧化锌纳米颗粒，通过掺杂后使其光学禁带宽度减小，活化能降低，更有利于反应的进行，大大提升了成品的抗氧化性能，有利于保存；本发明乳液质地均匀，稳定性较好；致敏性较低，受众范围较广。
Description
技术领域
本发明涉及日化产品技术领域，具体涉及抗氧化植物精华护肤乳液及其制备方法。
背景技术
植物中含有多种护肤营养成分，其中多糖除了具有抗氧化、抗肿瘤、抗衰老、抗炎等多种的药理作用外，其结构中的大量亲水性经基，使其外用时具有较好的吸水性、茹度性、乳化性和成膜性等，应用于化妆品可以产生保湿、修复受损皮肤、延缓衰老等功效。使用植物提取物制成的护肤乳液常伴有因光照、细菌导致的氧化变质，致使有效成分含量降低，影响了护肤乳液的各项功效。
专利CN 113908098 A公开了一种护肤乳液及其制备方法，使用紫茉莉籽粉和植物提取物，通过各功效成分之间的协同作用，解决了现有技术中乳液补水保湿不足、锁水效果差，不能同时保障良好保湿功效和肤感等问题。本发明护肤乳液肤感清爽、柔滑，具有深度补水保湿、长效锁水、降低肌肤油光度、调节肌肤水油平衡等功效。专利CN 104490637A提供了一种滋润保湿护肤乳液及其制备方法，采用聚甘油-10油酸酯作为主乳化剂，具有良好的乳化、润湿、分散、稳定等表面性质，且无臭无味，安全性高的特点，适合作为儿童及婴幼儿的护肤品。上述专利都没有对护肤乳液的抗氧化性进行优化，实际使用中可能会出现因氧化变质导致难以储存时间缩短的技术问题。
发明内容
为解决上述技术问题，本发明提供了一种抗氧化植物精华护肤乳液及其制备方法，技术方案如下：
一种抗氧化植物精华护肤乳液，包括以下原料：霍霍巴油2～4％、角鲨烷1.5～2％、烟酰胺0.35～0.5％、聚甘油硬脂酸酯0.5～1％、生育酚乙酸酯1.5～2％、甘油10～12％、尼泊金甲酯0.05～0.1％、尿囊素0.2～0.3％、甘露聚糖0.2～0.5％、余量为水。
烟酰胺，又名尼克酰胺、烟碱酰胺、3-吡啶甲酰胺，是烟酸的酰胺化合物，也是维生素B3的一种衍生物。为一种白色的结晶性粉末，微臭或几乎无臭，味苦，为维生素PP，属于氮杂环吡啶衍生物。其在水或乙醇中易溶，在甘油中溶解。烟酰胺的美白机制包含三个方面：(1)抑制黑色素颗粒的形成；(2)抑制黑色素向角质细胞传递；(3)加速角质细胞中黑色素向角质层转移并促进角质层脱落。
角鲨烷，又名深海鲨鱼肝油、鲨烷、异三十烷。最初，科学家从深海鲨鱼肝脏中提取的角鲨烯，经氢化制得到了角鲨烷。但近年发现，橄榄油、米糠油、麦胚油、酵母等中也可以提取少量的角鲨烷。角鲨烷是与人类皮脂最相近的一种油脂，有高效的携氧性，使用后可以与人体的皮脂融为一体，在皮肤表层形成一层渗透性良好的保护膜，让皮肤顺利代谢水与空气，不仅可以阻止水分流失，滋养皮肤，还不油腻。角鲨烷维持的是皮肤与皮脂间的平衡，在深层保湿的同时，还可以提高皮肤吸收水分和其他营养的能力，长期使用可以改善松弛、干燥、脱皮、粗糙、暗沉等皮肤问题，帮助皮肤恢复柔嫩。
烟酰胺、角鲨烷等物质已成为护肤品中的常规功能性成分，能起到基础美白保湿的功效，而消费者对市面上的护肤品的功能要求越来越高，与此同时还要保持护肤品成分的低敏性及纯天然性。因此，护肤品中除了基础配方外，通常会添加少量植物提取物以达到特定的功效。常规的植物提取物如玫瑰提取物、光果甘草提取物、金银花提取物以及黄芩提取物等，但现有技术中植物提取物的功能特性仍然较为单一且往往还需搭配使用。
马来西亚红麻，锦葵科木槿族植物(Hibiscus cannzzbinus L.)，正名大麻槿，一年生草本韧皮纤维作物，韧皮纤维柔软，纤维拉力强，对气候和环境的适应性强，具有耐旱、耐盐碱、耐贫瘠等强抗逆性和易栽培等特性。红麻是传统麻纺工业的重要原料，其纤维被开发为多种产品。长久以来，红麻的研发多集中在纤维上，育种目标也多集中在提高纤维产量和品质上。但红麻的其他部位也相应的具备不同的生物活性以及功能特性，如从红麻籽中提取得到红麻籽油，可通过进一步精深加工，得到生物柴油和生物润滑油，红麻籽油中主要含有油酸及亚油酸，具有抗癌抗氧化、降低血中胆固醇、预防高血压以及防止动脉粥样硬化等作用；从红麻的根部也可制备得到红麻根提取物，红麻根含有较多的强心甙，可用于心血管疾病方面的治疗；而酚类化合物含量最丰富的则是红麻叶，红麻的鲜叶和嫩茎叶具有较高总酚含量和的蛋白质含量，营养价值与苜蓿相当，并且富含多种维生素和氨基酸，是很好的植物性蛋白饲料原料，也常被用作饲料加工，但本发明人发现对红麻叶进行提取后其提取物中含有大量绿原酸、咖啡辅助剂、山奈酚和水合儿茶素等，且红麻叶提取物有较好的抗酪氨酸酶特性，还能起到紧致皮肤的作用。
进一步的，抗氧化植物精华护肤乳液，包括以下原料：霍霍巴油2～4％、角鲨烷1.5～2％、烟酰胺0.35～0.5％、聚甘油硬脂酸酯0.5～1％、生育酚乙酸酯1.5～2％、甘油10～12％、尼泊金甲酯0.05～0.1％、尿囊素0.2～0.3％、甘露聚糖0.2～0.5％、红麻叶提取物3～5％、余量为水。
优选的，所述红麻叶提取物采用如下方法制备得到：将红麻叶用水清洗后晾干，在﹣80～﹣60℃下保存10～12h；然后于﹣50～﹣40℃下冷冻干燥40～48h，取出研磨得到红麻叶粉；称取红麻叶粉3～5g，加入60～100mL氨性醇溶液于70～75℃下提取2～3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取2～3h后过滤，将两次滤液合并，于55～60℃下减压分馏，获得膏状提取物，即所述红麻叶提取物。
但在制备抗氧化植物精华护肤乳液的过程中，在加入红麻叶提取物后易导致乳液质地不稳定，难以形成均一的乳状液体，且产品贮存稳定性较差的问题。因此，在此基础上需要加入稳定剂和增稠剂等以改善乳液的状态。
细菌纤维素，在化学上与木材或植物纤维素相同，但在纯状态下通过发酵获得，由纳米级厚度(高长径比)的长纤维组成。细菌纤维素在生物医学方面的应用已经得到了显著的研究，在大多数领域的复合材料生产、乳剂和其他食品系统的生产和稳定、光电子和其他方面也得到了研究。近年来，细菌纤维素已被应用于化妆品面膜的开发中，作为用于皮肤护理的亲水化妆品化合物的基质，用于补水、恢复、延缓衰老和伤口治疗。本发明人发现将细菌纤维素与红麻叶提取物结合能有效提升红麻叶提取物的美白效果及其稳定性，红麻叶提取物中的酚类化合物作为植物次生代谢产物具有两亲结构，即既含有亲水性基团，又含有疏水性芳香基团。因此，这种结构可以通过非共价相互作用，如氢键和疏水力与细菌纤维素相互作用，而由于红麻叶提取物中含有较多的芳香基团，使得这种结合相比单一的酚类物质结合更加紧密，疏水相互作用更强。
最优选的，抗氧化植物精华护肤乳液，包括以下原料：霍霍巴油2～4％、角鲨烷1.5～2％、烟酰胺0.35～0.5％、聚甘油硬脂酸酯0.5～1％、生育酚乙酸酯1.5～2％、甘油10～12％、尼泊金甲酯0.05～0.1％、尿囊素0.2～0.3％、甘露聚糖0.2～0.5％、红麻叶提取物-细菌纤维素复合物3～5％、余量为水。
优选的，所述红麻叶提取物-细菌纤维素复合物采用如下方法制备得到：将红麻叶用水清洗后晾干，在﹣80～﹣60℃下保存10～12h；然后于﹣50～﹣40℃下冷冻干燥40～48h，取出研磨得到红麻叶粉；称取红麻叶粉3～5g，加入60～100mL氨性醇溶液于70～75℃下提取2～3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取2～3h后过滤，将两次滤液合并，于55～60℃下减压分馏，获得膏状提取物；再取0.5～1g细菌纤维素冻干粉加入到膏状提取物中搅拌混匀。
在长期的生产实践中发明人观察到，膏状提取物中由于富含有机物及水分，为物料的氧化及细菌的繁殖提供了有利条件。在膏状提取物的保存过程中时常出现因光照、细菌导致的氧化变质，致使膏状提取物有效成分含量降低，由此影响了护肤乳液的各项功效。为了提升膏状提取物的稳定性以，发明人在其制备过程中加入了氧化锌纳米颗粒；氧化锌纳米颗粒具有屏蔽紫外光照及抑菌效果，但是其参与反应的条件较高；为此，发明人进行掺杂后使其光学禁带宽度减小，活化能降低，更有利于反应的进行。
进一步优选的，所述红麻叶提取物-细菌纤维素复合物还可以采用如下方法制备得到：将红麻叶用水清洗后晾干，在﹣80～﹣60℃下保存10～12h；然后于﹣50～﹣40℃下冷冻干燥40～48h，取出研磨得到红麻叶粉；称取红麻叶粉3～5g，加入60～100mL氨性醇溶液于70～75℃下提取2～3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取2～3h后过滤，将两次滤液合并，于55～60℃下减压分馏，获得膏状提取物；再取0.5～1g细菌纤维素冻干粉及0.05～0.1g掺杂氧化锌纳米颗粒加入到膏状提取物中搅拌混匀。
优选的，所述掺杂氧化锌纳米颗粒的制备方法如下，以重量份计：
A1取3～6份红麻叶经干燥、研磨成红麻叶粉；将红麻叶粉与75～100份水混合，在65～80℃加热0.5～2h，冷却至常温后经过滤得滤液，得到红麻叶提取液；
A2将3.5～7份硝酸锌、0.06～0.12份硝酸铝、0.03～0.06份氯化锰溶解于所述红麻叶提取液中，首先在550～600℃煅烧15～30min，随后升温至650～750℃并煅烧2～3h，得到掺杂氧化锌纳米颗粒。
所述抗氧化植物精华护肤乳液采用如下方法制备，包括如下步骤：
S1按照配方量称取霍霍巴油、角鲨烷、烟酰胺、聚甘油硬脂酸酯、生育酚乙酸酯、甘油、尼泊金甲酯、尿囊素、甘露聚糖、水混匀再加热至75～80℃搅拌使固体完全溶解，再在20～30MPa下以2500～4500rpm的转速均质10～15min，得到均匀白色乳液；
S2将步骤S1得到的乳液冷却至40～45℃，加入红麻叶提取物或者红麻叶提取物-细菌纤维素复合物，以2000～3000rpm的转速搅拌10～15min再静置5～6h后得到所述抗氧化植物精华护肤乳液。
进一步的，所述氨性醇溶液中乙醇的体积分数为55～60％，氨气的体积分数为5～6％，余量为水。
相比现有技术，本发明具备如下有益效果：
1)美白紧致效果好且成分天然，以纯天然的植物配方为主；
2)乳液质地均匀，稳定性较好；
3)致敏性较低，受众范围较广；
4)抗氧化吸能好，能够长期储存。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述。以下实施例用于说明本发明，但不用来限制本发明的范围。实施例中涉及的操作如无特殊说明，均为本领域常规技术操作。
本发明对照例及实施例中部分原材料参数如下：
霍霍巴油，购于广州市嘉美化妆品有限公司；
聚甘油硬脂酸酯，CAS：105437-03-4，购于湖北汉达飞生物科技有限公司。
实施例1
一种抗氧化植物精华护肤乳液的制备方法，包括以下步骤：
S1制备红麻叶提取物：将红麻叶用水清洗后晾干，在﹣60℃下保存12h；然后于﹣40℃下冷冻干燥48h，取出研磨得到红麻叶粉；称取红麻叶粉5g，加入100mL氨性醇溶液于75℃下提取3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取3h后过滤，将两次滤液合并，于60℃下减压分馏，获得膏状提取物，即所述红麻叶提取物；
S2称取霍霍巴油4g、角鲨烷2g、烟酰胺0.5g、聚甘油硬脂酸酯1g、生育酚乙酸酯2g、甘油10g、尼泊金甲酯0.05g、尿囊素0.25g、甘露聚糖0.3g、76.9mL水混匀再加热至75℃搅拌使固体完全溶解，再在30MPa下以.3000rpm的转速均质12min，得到均匀白色乳液；
S3将步骤S2得到的乳液冷却至40℃，加入3g步骤S1制备得到的红麻叶提取物，以3000rpm的转速搅拌10min再静置5h后得到所述抗氧化植物精华护肤乳液。
所述氨性醇溶液中乙醇的体积分数为60％，氨气的体积分数为5％，水为35％。
对比例1
一种抗氧化植物精华护肤乳液的制备方法，包括以下步骤：
S1称取霍霍巴油4g、角鲨烷2g、烟酰胺0.5g、聚甘油硬脂酸酯1g、生育酚乙酸酯2g、甘油10g、尼泊金甲酯0.05g、尿囊素0.25g、甘露聚糖0.3g、水79.9mL混匀再加热至75℃搅拌使固体完全溶解，再在30MPa下以3000rpm的转速均质12min，得到均匀白色乳液；
S2将步骤S1得到的乳液冷却至40℃，再以3000rpm的转速搅拌10min再静置5h后得到所述抗氧化植物精华护肤乳液。
实施例2
一种抗氧化植物精华护肤乳液的制备方法，包括以下步骤：
S1制备红麻叶提取物-细菌纤维素复合物：将红麻叶用水清洗后晾干，在﹣60℃下保存12h，然后于﹣40℃下冷冻干燥48h，取出研磨得到红麻叶粉；称取红麻叶粉5g，加入100mL氨性醇溶液于75℃下提取3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取3h后过滤，将两次滤液合并，于60℃下减压分馏，获得红麻叶提取物；再取0.8g细菌纤维素冻干粉加入到红麻叶提取物中搅拌混匀即得红麻叶提取物-细菌纤维素复合物；
S2称取霍霍巴油4g、角鲨烷2g、烟酰胺0.5g、聚甘油硬脂酸酯1g、生育酚乙酸酯2g、甘油10g、尼泊金甲酯0.05g、尿囊素0.25g、甘露聚糖0.3g、水76.9mL混匀再加热至75℃搅拌使固体完全溶解，再在30MPa下以3000rpm的转速均质12min，得到均匀白色乳液；
S3将步骤S2得到的乳液冷却至40℃，加入3g步骤S1制备得到的红麻叶提取物-细菌纤维素复合物，以3000rpm的转速搅拌10min再静置5h后得到所述抗氧化植物精华护肤乳液。
所述氨性醇溶液中乙醇的体积分数为60％，氨气的体积分数为5％，水为35％。
细菌纤维素是以糖类为原料，经醋酸胶膜杆菌生物发酵得到的超高长径比的纤维状纳米材料，纤维直径在50～100nm，长度大于20um，吸水率约200倍左右，本发明中使用的是冻干细菌纤维素，粒径：50～100nm，购于桂林奇宏科技有限公司。
实施例3
一种抗氧化植物精华护肤乳液的制备方法，包括以下步骤：
S1制备红麻叶提取物-细菌纤维素复合物：将红麻叶用水清洗后晾干，在﹣60℃下保存12h；然后于﹣40℃下冷冻干燥48h，取出研磨得到红麻叶粉；称取红麻叶粉5g，加入100mL氨性醇溶液于75℃下提取3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取3h后过滤，将两次滤液合并，于60℃下减压分馏，获得红麻叶提取物；再取0.8g复合细菌纤维素加入到红麻叶提取物中搅拌混匀；
S2称取霍霍巴油4g、角鲨烷2g、烟酰胺0.5g、聚甘油硬脂酸酯1g、生育酚乙酸酯2g、甘油10g、尼泊金甲酯0.05g、尿囊素0.25g、甘露聚糖0.3g、水76.9mL混匀再加热至75℃搅拌使固体完全溶解，再在30MPa下以3000rpm的转速均质12min，得到均匀白色乳液；
S3将步骤S2得到的乳液冷却至40℃，加入3g步骤S1制备得到的红麻叶提取物-细菌纤维素复合物，以3000rpm的转速搅拌10min再静置5h后得到所述抗氧化植物精华护肤乳液。
所述氨性醇溶液中乙醇的体积分数为60％，氨气的体积分数为5％，水为35％。
所述复合细菌纤维素采用如下方法制备得到：将2g冻干细菌纤维素加入到10mL0.1mol/L的NaOH水溶液中浸泡12h，再用蒸馏水清洗4次，再向其中滴入3mL N-甲基吗啉-N-氧化物以9000rpm的速度湿磨，再称取吡啶硫酸盐0.65g继续搅拌，再缓慢加入5mL无水乙醇，用保鲜膜封住，静置8h后抽滤，得到滤液后再向其中加入0.5g的羧甲基纤维素钠，升温至80℃后于300rpm下搅拌12h，并在121℃下蒸压20分钟，取出冷却至室温后再于﹣40℃下冷冻干燥10h得到复合细菌纤维素。
本发明人发现将细菌纤维素与红麻叶提取物结合后能显著提升美白效果，且细菌纤维素是一种优良的载体基质，能有效保护红麻叶提取物的生物活性，但在添加进乳液中后，也容易发生小部分团聚的现象，因此本发明在此基础上进一步对细菌纤维素进行处理，通过少量的N-甲基吗啉-N-氧化物、吡啶硫酸盐、羧甲基纤维素与细菌纤维素进行结合，进一步提升乳液的稳定性。
实施例4
一种抗氧化植物精华护肤乳液的制备方法，包括以下步骤：
S1制备红麻叶提取物-细菌纤维素复合物：将红麻叶用水清洗后晾干，在﹣60℃下保存12h；然后于﹣40℃下冷冻干燥48h，取出研磨得到红麻叶粉；称取红麻叶粉5g，加入100mL氨性醇溶液于75℃下提取3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取3h后过滤，将两次滤液合并，于60℃下减压分馏，获得红麻叶提取物；再取0.8g复合细菌纤维素及0.06g掺杂氧化锌纳米颗粒加入到红麻叶提取物中搅拌混匀；
S2称取霍霍巴油4g、角鲨烷2g、烟酰胺0.5g、聚甘油硬脂酸酯1g、生育酚乙酸酯2g、甘油10g、尼泊金甲酯0.05g、尿囊素0.25g、甘露聚糖0.3g、水76.9mL混匀再加热至75℃搅拌使固体完全溶解，再在30MPa下以3000rpm的转速均质12min，得到均匀白色乳液；
S3将步骤S2得到的乳液冷却至40℃，加入3g步骤S1制备得到的红麻叶提取物-细菌纤维素复合物，以3000rpm的转速搅拌10min再静置5h后得到所述抗氧化植物精华护肤乳液。
所述氨性醇溶液中乙醇的体积分数为60％，氨气的体积分数为5％，水为35％。
所述复合细菌纤维素采用如下方法制备得到：将2g冻干细菌纤维素加入到10mL0.1mol/L的NaOH水溶液中浸泡12h，再用蒸馏水清洗4次，再向其中滴入3mL N-甲基吗啉-N-氧化物以9000rpm的速度湿磨，再称取吡啶硫酸盐0.65g继续搅拌，再缓慢加入5mL无水乙醇，用保鲜膜封住，静置8h后抽滤，得到滤液后再向其中加入0.5g的羧甲基纤维素钠，升温至80℃后于300rpm下搅拌12h，并在121℃下蒸压20分钟，取出冷却至室温后再于﹣40℃下冷冻干燥10h得到复合细菌纤维素。
所述掺杂氧化锌纳米颗粒的制备方法如下，以重量份计：
A1取5g红麻叶经干燥、研磨成红麻叶粉；将红麻叶粉与75g水混合，在75℃加热0.5h，冷却至常温后经过滤得滤液，得到红麻叶提取液；
A2将3.6g硝酸锌、0.06g硝酸铝、0.03g氯化锰溶解于所述红麻叶提取液中，首先在550℃煅烧15min，随后升温至750℃并煅烧2h，得到掺杂氧化锌纳米颗粒。
测试例1
对实施例1-4及对比例1的抗氧化植物精华护肤乳液进行美白评价测试，参考(上海日用化学品行业协会团体标准T/SHRH 015-2018)中的测试方法进行测试。具体步骤为：使用10mL试管设立样品管(T)、样品本底(T0)、酶反应管(C)和溶剂本底(C0)，每一样品的每个受试浓度的样品管(T)需设立3支平行管，同时酶反应管(C)也需设立3支平行管。在样品管(T)和样品本底(T0)中各加入1mL相同浓度的样品溶液，酶反应管(C)和溶剂本底(C0)则分别加入1mL磷酸氢二钠-柠檬酸缓冲液。在样品管(T)和酶反应管(C)中各加入0.5mL酪氨酸酶溶液，样品本底(T0)与溶剂本底(C0)以0.5mL磷酸氢二钠-柠檬酸缓冲液代替，将样品和酪氨酸酶充分混匀，置37℃水浴槽孵育10分钟。依次在各管中加入2mL的左旋多巴溶液，控制每管反应时间为5分钟，即刻将各管反应溶液移入比色皿中，在475nm处测定吸光值。计算公式如下：
表1酪氨酸酶活性抑制率测试结果表
| 抑制率/％ | |
| 对比例1 | 57.05％ |
| 实施例1 | 73.08％ |
| 实施例2 | 76.52％ |
| 实施例3 | 77.69％ |
| 实施例4 | 79.14％ |
由表1可知，加入了红麻叶提取物的美白乳液具有显著的美白功效，对酪氨酸酶活性的抑制作用越强，说明抑制黑色素生成的效果越好。而将细菌纤维素与红麻叶提取物结合后能进一步有效提升红麻叶提取物的美白效果，红麻叶提取物中的酚类化合物作为植物次生代谢产物具有两亲结构，即既含有亲水性基团，又含有疏水性芳香基团。因此，这种结构可以通过非共价相互作用，如氢键和疏水力与细菌纤维素相互作用，而由于红麻叶提取物中含有较多的芳香基团，使得这种结合相比单一的酚类物质结合更加紧密，疏水相互作用更强。细菌纤维素与红麻叶提取物结合后可以使得红麻叶提取物的渗透性更好，更能发挥其功能活性。
测试例2
对实施例1-4及对比例1的抗氧化植物精华护肤乳液进行稳定性测试，参考GB/T29665-2013对所配制乳液进行高温、低温和冷热交替贮存稳定性测试。3000rpm离心30min后观察乳液是否分层；48℃连续恒温20d，再恢复室温保持8h以上，观察乳液是否有分层、析出固体或其他不均一的现象；在﹣25℃连续冷冻20d，再恢复室温保持8h以上，观察乳液是否有分层、析出固体或其他不均一的现象；在48和﹣25℃条件下24h冷热交替循环20d，再恢复室温保持8h以上，观察乳液是否有分层、析出固体或其他不均一的现象。上述测试中，若乳液均无分层、析出固体或其他不均一现象，则稳定性测试通过，否则为稳定性测试未通过。测试结果见表2。
表2乳液稳定性测试结果
| 高温 | 低温 | 冷热交替 | |
| 实施例1 | 不通过 | 通过 | 不通过 |
| 实施例2 | 通过 | 通过 | 不通过 |
| 实施例3 | 通过 | 通过 | 通过 |
| 实施例4 | 通过 | 通过 | 通过 |
| 对比例1 | 不通过 | 通过 | 不通过 |
对乳液进行贮存稳定性测试，测试结果表明加入了细菌纤维素的乳液其高温贮存稳定性明显提高，但在冷热交替贮存中则出现了部分沉降的情况，而本发明对细菌纤维素进行进一步处理制备成复合细菌纤维素后整个乳液的稳定性得到了提升，复合细菌纤维素的加入在不添加大量化学成分的情况下又产生了表面活性剂的作用。
测试例3
对实施例1-4及对比例1的抗氧化植物精华护肤乳液进行抗氧化性测试，将实施例及对比例制备得到的乳液在贮存0天和25℃下密封贮存60天分别测定DPPH自由基清除率：取3mL等体积的待测液与2×10﹣4mol/L的DPPH溶液混匀(A1管)；取等体积的无水乙醇与2×10﹣4mol/L的DPPH溶液混匀(A2管)；取等体积的无水乙醇与待测液混匀(A3管)；30℃避光反应30min后，以蒸馏水为空白组，在517nm下测A1、A2、A3管的吸光度值，分别记作ODA1、ODA2和ODA3。DPPH自由基清除率根据如下公式进行计算，测试结果如表3：
表3 DPPH自由基清除率测试结果表
| 0天清除率％ | 60天清除率％ | |
| 对比例1 | 35.2 | 33.0 |
| 实施例1 | 63.0 | 61.8 |
| 实施例2 | 67.2 | 66.4 |
| 实施例3 | 67.5 | 67.2 |
| 实施例4 | 73.1 | 72.8 |
DPPH自由基清除率越高则代表样品的抗氧化性越强，由于红麻叶提取物中含有大量绿原酸、咖啡辅助剂、山奈酚和水合儿茶素等，因此具备较高的抗氧化性，而在乳液加工过程中，细菌纤维素的添加对红麻叶提取中的酚类成分起到了较好的作用，且在贮存期间其损失率相比不添加细菌纤维素要低，而对比实施例2和3可知，复合细菌纤维素进一步增强了美白乳液在长期贮存过程中的活性成分的有效性。实施例4具有最佳的抗氧化效果，其原因可能在于，氧化锌纳米颗粒具有屏蔽紫外光照及抑菌效果，进行掺杂后使其光学禁带宽度减小，活化能降低，更有利于反应的进行，能够降低紫外光照引起的氧化，使成品的有效成分含量更高、效果更好。
Claims (5)
1.一种抗氧化植物精华护肤乳液，其特征在于，包括以下质量比的原料：霍霍巴油2～4％、角鲨烷1.5～2％、烟酰胺0.35～0.5％、聚甘油硬脂酸酯0.5～1％、生育酚乙酸酯1.5～2％、甘油10～12％、尼泊金甲酯0.05～0.1％、尿囊素0.2～0.3％、甘露聚糖0.2～0.5％、红麻叶提取物-细菌纤维素复合物3～5％、余量为水；
所述红麻叶提取物-细菌纤维素复合物采用如下方法制备得到：将红麻叶用水清洗后晾干，在﹣80～﹣60℃下保存10～12h；然后于﹣50～﹣40℃下冷冻干燥40～48h，取出研磨得到红麻叶粉；称取红麻叶粉3～5g，加入60～100mL氨性醇溶液于70～75℃下提取2～3h后冷却过滤，保留上清液，取滤渣再加入等质量的氨性醇溶液提取2～3h后过滤，将两次滤液合并，于55～60℃下减压分馏，获得膏状提取物；再取0.5～1g复合细菌纤维素及0.05～0.1g掺杂氧化锌纳米颗粒加入到膏状提取物中搅拌混匀；
所述掺杂氧化锌纳米颗粒的制备方法如下，以重量份计：取3～6份红麻叶经干燥、研磨成红麻叶粉；将红麻叶粉与75～100份水混合，在65～80℃加热0.5～2h，冷却至常温后经过滤得滤液，得到红麻叶提取液；将3.5～7份硝酸锌、0.06～0.12份硝酸铝、0.03～0.06份氯化锰溶解于所述红麻叶提取液中，首先在550～600℃煅烧15～30min，随后升温至650～750℃并煅烧2～3h，得到掺杂氧化锌纳米颗粒；
所述复合细菌纤维素采用如下方法制备得到：将2g冻干细菌纤维素加入到10mL0.1mol/L的NaOH水溶液中浸泡12h，再用蒸馏水清洗4次，再向其中滴入3mL N-甲基吗啉-N-氧化物以9000rpm的速度湿磨，再称取吡啶硫酸盐0.65g继续搅拌，再缓慢加入5mL无水乙醇，用保鲜膜封住，静置8h后抽滤，得到滤液后再向其中加入0.5g的羧甲基纤维素钠，升温至80℃后于300rpm下搅拌12h，并在121℃下蒸压20分钟，取出冷却至室温后再于﹣40℃下冷冻干燥10h得到复合细菌纤维素。
2.如权利要求1所述的抗氧化植物精华护肤乳液的制备方法，其特征在于，制备步骤如下：
S1按照配方量称取霍霍巴油、角鲨烷、烟酰胺、聚甘油硬脂酸酯、生育酚乙酸酯、甘油、尼泊金甲酯、尿囊素、甘露聚糖、水混匀再加热至75～80℃搅拌使固体完全溶解，再均质得到均匀白色乳液；
S2将步骤S1得到的乳液冷却至40～45℃，加入红麻叶提取物或者红麻叶提取物-细菌纤维素复合物，搅拌均匀再静置5～6h后得到所述抗氧化植物精华护肤乳液。
3.如权利要求2所述的抗氧化植物精华护肤乳液的制备方法，其特征在于，所述步骤S1中的均质条件为：在20～30MPa下以2500～4500rpm的转速均质10～15min。
4.如权利要求2所述的抗氧化植物精华护肤乳液的制备方法，其特征在于，所述步骤S2中的搅拌条件为：以2000～3000rpm的转速搅拌10～15min。
5.如权利要求2所述的抗氧化植物精华护肤乳液，其特征在于，所述氨性醇溶液中乙醇的体积分数为55～60％，氨气的体积分数为5～6％，余量为水。
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