CN112641710A - 一种罗非鱼皮肽维生素e乳膏及其制备方法 - Google Patents
一种罗非鱼皮肽维生素e乳膏及其制备方法 Download PDFInfo
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- CN112641710A CN112641710A CN202011568507.9A CN202011568507A CN112641710A CN 112641710 A CN112641710 A CN 112641710A CN 202011568507 A CN202011568507 A CN 202011568507A CN 112641710 A CN112641710 A CN 112641710A
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- skin peptide
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Abstract
本发明提供了一种罗非鱼皮肽维生素E乳膏及其制备方法。本发明采用两步法添加罗非鱼皮肽水溶液来制备罗非鱼皮肽维生素E乳膏，具体步骤为：S1.将罗非鱼皮肽溶于纯化水中；S2.将硬脂酸、十八醇、单硬脂酸甘油酯混合，加热熔融，保温，得到油相；S3.将吐温‑80、三乙醇胺、甘油、尼泊金乙酯混合，加热熔融，保温，加入步骤S1的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；S4.将吐温‑80、维生素E混合，搅拌均匀，保温，得到备用液；S5.将油相加入到水相中混合均匀，然后添加备用液及剩余的2/5罗非鱼皮肽水溶液，快速搅拌成霜，冷却即得。该乳膏的稳定性和持久保湿性良好，能够养护肌肤，且制备工艺简单，适用于产业化生产。
Description
技术领域
本发明涉及日化用品领域，具体涉及一种罗非鱼皮肽维生素E乳膏及其制备方法。
背景技术
维生素E乳膏或者霜是临床上广为应用医用护肤品，它可以滋润皮肤，特别还可以抗氧化，抗老化，还有褪色素的作用，而且比较安全，特别适用一些敏感性的肌肤，比如脸上容易过敏，再就是一些皮炎、湿疹的患者。在治疗方面，维生素E霜可联合物理仪器使用，如配合空气波压力治疗仪配合维生素E霜外涂治疗老年患者输液外渗、红光照射与维生素E霜按摩联合治疗新生儿硬肿症等；也可联合其他药品使用，如复方刺梨合剂与维生素E霜联合、治疗黄褐斑；临床上也有联合2％的植物甾醇类、红松籽油、牡丹籽油、积雪草精油等，与维生素E霜一起使用，增强抗氧化功能。目前有相当部分维生素E霜添加药品制备复合维生素E霜，如添加有机锗配制成复方维E霜，可以用于治疗黄褐斑；黄芩维E防护乳膏可用于放疗患者的辅助治疗，且取得满意的疗效；添加芦荟凝胶干粉制备芦荟E乳膏，可保湿及消除面部青春痘甚至雀斑等，具有抗衰老、祛色斑、养颜护肤等功效；将维生素E、C制成霜剂，可用于治疗皮肤瘙痒及多形性日光疹；以维生素E、芦荟、珍珠粉为原料制备的维生素E芦荟珍珠霜对于日光性皮炎、皮肤色素沉积等有治疗作用；以尿素、维生素E、珍珠粉等为组方制备的水包油型尿素维E珍珠乳膏可用于改善皮肤干燥、瘙痒、皲裂、角质化及祛斑等，例如公布号为CN 105997989 A的中国专利公开了一种用于治疗手足皲裂和角化型手足癣引起皲裂的尿素维E乳膏，该乳膏包含尿素、维生素E、儿茶素和聚乙二醇-7-硬脂酸酯，膏状细腻、涂抹性好，能够有效改善皮肤皲裂的症状。虽然现有研究赋予了维E乳膏越来越多的作用和功效，但其持久保湿性能仍有待提高。
发明内容
本发明的目的在于克服现有技术中存在的上述缺陷和不足，提供一种罗非鱼皮肽维生素E乳膏。
本发明的另一目的在于提供一种罗非鱼皮肽维生素E乳膏的制备方法。
本发明的上述目的是通过以下技术方案给予实现的：
一种罗非鱼皮肽维生素E乳膏，包含以下重量份的各组分：硬脂酸、十八醇、单硬脂酸甘油酯、吐温-80、三乙醇胺、甘油、尼泊金乙酯、维生素E、罗非鱼皮肽、纯化水。
其中，硬脂酸是膏类和霜类护肤品中常用的一种乳化剂，用于配制雪花膏、冷霜、粉底霜，也可用于可用作油溶性颜料的溶剂、蜡笔调滑剂、蜡纸打光剂、以及用作橡胶合成与加工过程中的增塑剂和软化剂等。
硬脂醇在制药中用作分散剂，在化妆品中用作霜膏的乳化剂，还用作稻田的保温剂、水库覆盖剂以及合成橡胶和彩色胶片的成色剂等。
单硬脂酸甘油酯和吐温-80是表面活性剂，常用作食品和化妆品领域的乳化剂、助乳化剂、稳定剂和保鲜剂。
三乙醇胺在化妆品中用作乳化剂、保湿剂、增湿剂、增稠剂、pH平衡剂，用三乙醇胺乳化的乳膏产品具有膏体细腻，膏体亮白的特点。
甘油具有保湿、保润、抗氧化、促醇化等作用，已被广泛用于造纸、化妆品、印刷、金属加工、电工材料和橡胶等工业中。
尼泊金乙酯是一种用于食品、化妆品、医药的杀菌防腐剂。
罗非鱼皮肽通过对罗非鱼鱼皮进行酶解、离心、超滤分离、浓缩、喷雾干燥制备得到。本发明的罗非鱼皮肽以干基计蛋白含量约98％，灰分约0.50％，97％以上的分子量小于3000Da，70％以上的分子量小于1000Da；纯化水能够避免细菌、杂质影响乳膏的品质，包括去离子水、蒸馏水。罗非鱼皮肽在本发明中的作用是提高维生素E乳膏的持久保湿性能。
优选地，所述罗非鱼皮肽维生素E乳膏，包含以下重量份的各组分：硬脂酸6～8份、十八醇3～5.5份、单硬脂酸甘油酯4.5～5.5份、吐温-804～9份、三乙醇胺0.5～1.5份、甘油5～9份、尼泊金乙酯0.5～1.5份、维生素E0.5～1.5份、罗非鱼皮肽0.5～1.5份、纯化水60～70份。
优选地，所述罗非鱼皮肽维生素E乳膏，包含以下重量份的各组分：硬脂酸6.5～7.5份、十八醇3.5～4.5份、单硬脂酸甘油酯4.7～5.2份、吐温-80 5～9份、三乙醇胺0.5～1份、甘油6～9份、尼泊金乙酯0.5～1份、维生素0.5～1份、罗非鱼皮肽0.6～1份、纯化水60～65份。
优选地，所述罗非鱼皮肽维生素E乳膏，包含以下重量份的各组分：硬脂酸7份、十八醇4份、单硬脂酸甘油酯5份、吐温-80 9份、三乙醇胺1份、甘油9份、尼泊金乙酯1份、维生素E1份、罗非鱼皮肽1份、纯化水62份。
一种罗非鱼皮肽维生素E乳膏的制备方法，包含以下步骤：
S1.将罗非鱼皮肽溶于纯化水中；
S2.将硬脂酸、十八醇、单硬脂酸甘油酯混合，加热使其熔融，保温，得到油相；
S3.将吐温-80、三乙醇胺、甘油、尼泊金乙酯混合，加热使其熔融，保温，加入步骤S1的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；
S4.将吐温-80、维生素E混合，搅拌均匀，保温，得到备用液；
S5.将步骤S2的油相加入到步骤S3的水相中混合均匀，然后添加步骤S4的备用液及步骤S1剩余的2/5罗非鱼皮肽水溶液，快速搅拌均匀成霜，在室温下自然冷却呈乳膏状，即得。
本发明方法采用两步法添加罗非鱼皮肽水溶液替换传统的一步法来显著提高罗非鱼皮肽维生素E乳膏的稳定性。
优选地，所述步骤S2、S3的加热温度为70～80℃。
优选地，步骤S4所述搅拌温度为50～60℃。
优选地，步骤S5所述快速搅拌的速度为8000转/分～8500转/分。
优选地，步骤S5所述快速搅拌的时间为15s～25s。
作为一种优选地可实施方式，所述罗非鱼皮肽的制备方法，具体包括以下步骤：
(1)罗非鱼皮肽粉剂的制备：罗非鱼皮肽粉剂是依据优化的酶解工艺条件，对罗非鱼鱼皮进行酶解、离心、超滤分离、浓缩、喷雾干燥自制得到的。具体步骤如下：罗非鱼皮经解冻，剔干净残留的碎肉和鱼鳞后，按照重量比1：1加水经100℃煮沸10min，绞肉机打碎成匀浆液，再加水适量使最终料水比为1:3，一并放入酶解罐中，待匀浆液温度稳定为50℃，同时添加0.3％中性蛋白酶和0.05％木瓜蛋白酶，酶解3.5h后，升温100℃灭酶10min，待酶解液冷却至常温，离心(转速1500rpm，200目内衬滤袋)，去渣，上清液经200nm陶瓷膜微滤后再经1000Da超滤膜超滤，取超滤截留液旋转蒸发浓缩后喷雾干燥即得。
(2)罗非鱼皮肽维生素E乳膏的制备：将1份罗非鱼皮肽粉剂溶解在62份去离子水中；分别称取7份硬脂酸、4份十八醇、5份单硬脂酸甘油酯置于同一容器中水浴加热，温度70℃，保温备用，得到油相；分别称取4.5份吐温-80、1份三乙醇胺、9份甘油、1份尼泊金乙酯置于同一容器中水浴加热，温度75℃，保温备用，加入上述制备得到的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；分别称取4.5份吐温-80、1份维生素E置于同一容器中，在60℃搅拌均匀，保温备用，作为备用液；在75℃条件下，将制备好的油相加入到水相中搅拌均匀，然后添加备用液及剩余的2/5罗非鱼皮肽水溶液，在8500rpm转速下快速搅拌20s成霜，取出在室温自然冷却得到罗非鱼皮肽维生素E乳膏。
与现有技术相比，本发明具有以下有益效果：
本发明采用两步法添加罗非鱼皮肽水溶液制备罗非鱼皮肽维生素E乳膏，该乳膏稳定性和持久保湿性良好，能够深层快速地养护肌肤，且其制备工艺简单，适用于产业化生产。
附图说明
图1为罗非鱼皮肽维生素E乳膏图。
图2为不同制备方法得到的罗非鱼皮肽维生素E乳膏稳定性。
具体实施方式
以下结合说明书附图和具体实施例来进一步说明本发明，但实施例并不对本发明做任何形式的限定。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明，以下实施例所用试剂和材料均为市购。
实施例1罗非鱼皮肽维生素E乳膏的制备
(1)罗非鱼皮肽粉剂的制备：罗非鱼皮肽粉剂是依据优化的酶解工艺条件，对罗非鱼鱼皮进行酶解、离心、超滤分离、浓缩、喷雾干燥自制得到的。具体步骤如下：罗非鱼皮经解冻，剔干净残留的碎肉和鱼鳞后，按照重量比1：1加水经100℃煮沸10min，绞肉机打碎成匀浆液，再加水适量使最终料水比为1:3，一并放入酶解罐中，待匀浆液温度稳定为50℃，同时添加0.3％中性蛋白酶和0.05％木瓜蛋白酶，酶解3.5h后，升温100℃灭酶10min，待酶解液冷却至常温，离心(转速1500rpm，200目内衬滤袋)，去渣，上清液经200nm陶瓷膜微滤后再经1000Da超滤膜超滤，取超滤截留液旋转蒸发浓缩后喷雾干燥即得。
(2)罗非鱼皮肽维生素E乳膏的制备：将1.5份罗非鱼皮肽粉剂溶解在70份去离子水中；分别称取8份硬脂酸、3份十八醇、5.5份单硬脂酸甘油酯置于同一容器中水浴加热，温度75℃，保温备用，得到油相；分别称取2份吐温-80、0.5份三乙醇胺、5份甘油、1.5份尼泊金乙酯置于同一容器中水浴加热，温度80℃，保温备用，加入上述制备得到的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；分别称取2份吐温-80、0.5份维生素E置于同一容器中，在55℃搅拌均匀，保温备用，作为备用液；在75℃条件下，将制备好的油相加入到水相中混合搅拌均匀，然后添加备用液及剩余的2/5罗非鱼皮肽水溶液，在8000转/分下快速搅拌20s成霜，取出在室温自然冷却得到罗非鱼皮肽维生素E乳膏。
本发明制备的罗非鱼皮肽维生素E乳膏如图1所示。
实施例2罗非鱼皮肽维生素E乳膏的制备
罗非鱼皮肽粉剂的制备如实施例1所述。
将0.5份罗非鱼皮肽粉剂溶解在60份去离子水中；分别称取6份硬脂酸、5.5份十八醇、4.5份单硬脂酸甘油酯置于同一容器中水浴加热，温度70℃，保温备用，得到油相；分别称取4份吐温-80、1.5份三乙醇胺、7份甘油、0.5份尼泊金乙酯置于同一容器中水浴加热，温度75℃，保温备用，加入上述制备得到的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；分别称取3份吐温-80、1.5份维生素E置于同一容器中，在55℃搅拌均匀，保温备用，作为备用液；在75℃条件下，将制备好的油相加入到水相中混合搅拌均匀，然后添加备用液及剩余的2/5罗非鱼皮肽水溶液，在8300rpm转/分下快速搅拌15s成霜，取出在室温自然冷却得到罗非鱼皮肽维生素E乳膏。
实施例3罗非鱼皮肽维生素E乳膏的制备
罗非鱼皮肽粉剂的制备如实施例1所述。
将1份罗非鱼皮肽粉剂溶解在62份去离子水中；分别称取7份硬脂酸、4份十八醇、5份单硬脂酸甘油酯置于同一容器中水浴加热，温度70℃，保温备用，得到油相；分别称取4.5份吐温-80、1份三乙醇胺、9份甘油、1份尼泊金乙酯置于同一容器中水浴加热，温度75℃，保温备用，加入上述制备得到的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；分别称取4.5份吐温-80、1份维生素E置于同一容器中，在60℃搅拌均匀，保温备用，作为备用液；在75℃条件下，将制备好的油相加入到水相中混合搅拌均匀，然后添加备用液及剩余的2/5罗非鱼皮肽水溶液，在8500转/分下快速搅拌20s成霜，取出在室温自然冷却得到罗非鱼皮肽维生素E乳膏。
实施例4罗非鱼皮肽维生素E乳膏的制备
罗非鱼皮肽粉剂的制备如实施例1所述。
将0.8份罗非鱼皮肽粉剂溶解在65份去离子水中；分别称取7.5份硬脂酸、3.5份十八醇、5份单硬脂酸甘油酯置于同一容器中水浴加热，温度80℃，保温备用，得到油相；分别称取4份吐温-80、0.8份三乙醇胺、7份甘油、0.8份尼泊金乙酯置于同一容器中水浴加热，温度75℃，保温备用，加入上述制备得到的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；分别称取4份吐温-80、0.8份维生素E置于同一容器中，在60℃搅拌均匀，保温备用，作为备用液；在80℃条件下，将制备好的油相加入到水相中混合搅拌均匀，然后添加备用液及剩余的2/5罗非鱼皮肽水溶液，在8000rpm转/分下快速搅拌25s成霜，取出在室温自然冷却得到罗非鱼皮肽维生素E乳膏。
对比例1对比罗非鱼皮肽维生素E乳膏的制备
罗非鱼皮肽粉剂的制备如实施例1所述。
将1份罗非鱼皮肽粉剂溶解在62份去离子水中；分别称取7份硬脂酸、4份十八醇、5份单硬脂酸甘油酯置于同一容器中水浴加热，温度70℃，保温备用，得到油相；分别称取4.5份吐温-80、1份三乙醇胺、9份甘油、1份尼泊金乙酯置于同一容器中水浴加热，温度75℃，保温备用，加入上述制备得到的罗非鱼皮肽水溶液搅拌均匀，得到水相；分别称取4.5份吐温-80、1份维生素E置于同一容器中，在60℃搅拌均匀，保温备用，作为备用液；在75℃条件下，将制备好的油相加入到水相中混合搅拌均匀，然后添加备用液，在8500rpm转/分下快速搅拌20s成霜，取出在室温自然冷却即得。
对比例2维生素E乳膏的制备
称取7份硬脂酸、4份十八醇、5份单硬脂酸甘油酯置于同一容器中水浴加热，温度70℃，保温备用，得到油相；分别称取4.5份吐温-80、1份三乙醇胺、9份甘油、1份尼泊金乙酯置于同一容器中水浴加热，温度75℃，保温备用，得到水相；分别称取4.5份吐温-80、1份维生素E置于同一容器中，在60℃搅拌均匀，保温备用，作为备用液；在75℃条件下，将制备好的油相加入到水相中混合搅拌均匀，然后添加备用液和63份去离子水，在8500rpm转/分下快速搅拌20s成霜，取出在室温自然冷却得到维生素E乳膏。
测试例1罗非鱼皮肽维生素E乳膏的体表保湿性能
分别取实施例3与对比例2的乳膏样品直接少量涂抹在皮肤进行试验，并以1％的罗非鱼皮肽水溶液及现有的维E面霜作为对照组。随机挑选10位15～20年龄段的皮肤健康受试者，选取他们的左手前臂内侧相同区域2cm×2cm处为接受测试的部位，均匀涂抹少量试验品至相应待测区域，用皮肤水分测试仪分别测定10min、30min、60min后涂抹区域的皮肤含水率，在同一区域内选取3～4个不同的点进行检测，然后取平均值为测定值，将测定的皮肤含水率减去未涂抹样品前的皮肤含水率就得到该时段的测定值。
本实验要求受试部位实验前2～3天不能使用任何护肤品，另外，受试者需要提前进入测试环境，稍作休息后再开始进行实验。
体表保湿效果评价的评价公式：
相对保湿率(％)＝(P样t＝x﹣P空白)×100％
其中，P空白为未涂抹样品前皮肤的含水率，P样t＝x为涂抹样品一定时间后皮肤的含水率。
结果如表1所示：
表1罗非鱼皮肽维生素E乳膏的体表保湿性测试结果
| 名称 | 10min | 30min | 60min |
| 实施例3 | 19.7％ | 17.6％ | 17.2％ |
| 对比例2 | 17.3％ | 14.5％ | 10.7％ |
| 现有的维E面霜 | 16.2％ | 16.1％ | 15.4％ |
| 1％罗非鱼皮肽水溶液 | 3.6％ | 2.4％ | 2.3％ |
根据表1可知，1％罗非鱼皮肽水溶液的保湿性较差；相比于其他组，实施例3的罗非鱼皮肽维生素E乳膏的保湿性能较佳，能够保湿性更持久。
测试例2罗非鱼皮肽维生素E乳膏的稳定性
通过离心试验来评价不同制备方法制备得到的罗非鱼皮肽维生素E乳膏：分别称取实施例3与对比例1制备得到的10g样品于离心管中，于3000r/min离心30分钟，观察乳膏分层情况。
结果分析：如图2所示，对比例1制备得到的罗非鱼皮肽维生素E乳膏在离心之后出现了部分透明，分层，并可见白色絮状物分布；实施例3制备得到的罗非鱼皮肽维生素E乳膏在离心之后无絮状物分布，无分层，整体均匀度较好。
Claims (10)
1.一种罗非鱼皮肽维生素E乳膏，其特征在于，包含以下各组分：硬脂酸、十八醇、单硬脂酸甘油酯、吐温-80、三乙醇胺、甘油、尼泊金乙酯、维生素E、罗非鱼皮肽、纯化水。
2.根据权利要求1所述罗非鱼皮肽维生素E乳膏，其特征在于，包含以下重量份的各组分：硬脂酸6～8份、十八醇3～5.5份、单硬脂酸甘油酯4.5～5.5份、吐温-804～9份、三乙醇胺0.5～1.5份、甘油5～9份、尼泊金乙酯0.5～1.5份、维生素E0.5～1.5份、罗非鱼皮肽0.5～1.5份、纯化水60～70份。
3.根据权利要求2所述罗非鱼皮肽维生素E乳膏，其特征在于，包含以下重量份的各组分：硬脂酸6.5～7.5份、十八醇3.5～4.5份、单硬脂酸甘油酯4.7～5.2份、吐温-80 5～9份、三乙醇胺0.5～1份、甘油6～9份、尼泊金乙酯0.5～1份、维生素E 0.5～1份、罗非鱼皮肽0.6～1份、纯化水60～65份。
4.根据权利要求3所述罗非鱼皮肽维生素E乳膏，其特征在于，包含以下重量份的各组分：硬脂酸7份、十八醇4份、单硬脂酸甘油酯5份、吐温-80 9份、三乙醇胺1份、甘油9份、尼泊金乙酯1份、维生素E1份、罗非鱼皮肽1份、纯化水62份。
5.根据权利要求1～4任一所述罗非鱼皮肽维生素E乳膏，其特征在于，所述罗非鱼皮肽中97％以上的分子量小于3000Da，70％以上的分子量小于1000Da。
6.权利要求1～5任一所述罗非鱼皮肽维生素E乳膏的制备方法，其特征在于，包含以下步骤：
S1.将罗非鱼皮肽溶于纯化水中；
S2.将硬脂酸、十八醇、单硬脂酸甘油酯混合，加热使其熔融，保温，得到油相；
S3.将吐温-80、三乙醇胺、甘油、尼泊金乙酯混合，加热使其熔融，保温，加入步骤S1的3/5罗非鱼皮肽水溶液搅拌均匀，得到水相；
S4.将吐温-80、维生素E混合，搅拌均匀，保温，得到备用液；
S5.将步骤S2的油相加入到步骤S3的水相中混合均匀，然后添加步骤S4的备用液及步骤S1剩余的2/5罗非鱼皮肽水溶液，快速搅拌均匀成霜，在室温下自然冷却呈乳膏状，即得。
7.根据权利要求6所述制备方法，其特征在于，步骤S2、S3所述加热温度为70～80℃。
8.根据权利要求6所述制备方法，其特征在于，步骤S4所述搅拌温度为50～60℃。
9.根据权利要求6所述制备方法，其特征在于，步骤S5所述快速搅拌的速度为8000转/分～8500转/分。
10.根据权利要求6所述制备方法，其特征在于，步骤S5所述快速搅拌的时间为15s～25s。
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