CN112641682B - 一种玫瑰花液及其制备方法 - Google Patents
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Abstract
本发明涉及一种玫瑰花液及其制备方法,所述制备方法包括:新鲜保加利亚玫瑰花瓣去叶洗净、加入活化水浸泡、活化处理、水蒸气蒸馏提取、稳定化处理、过滤、辐照灭菌、检验灌装,不包括油水分离步骤。此提取方法完整保留玫瑰所蕴含的大量黄酮及其它有效活性成分,且采用特殊活化水蒸气蒸馏提取技术,不经过任何防腐处理、有机溶剂浸泡,无毒副作用,纯自然加工花瓣,保证玫瑰花液安全性。
Description
技术领域
本发明属于化妆品和保健品领域,特别涉及一种玫瑰花液及其制备方法。
背景技术
玫瑰的利用最早起源于中国。早在北宋时期就有记载,历代王宫一直都延续使用。据金代《后芳华苑》书中记载:“柏玉搔头绿云发,玫瑰面脂透骨滑”。到元代,人们将妙峰山玫瑰制成饮料送入宫庭,御医将之作为御药原料,在御膳太医所著《饮膳正要》中记载:"渴忒饼儿"的制作法功效为:生津止寒漱。玫瑰的芬芳来自它所含的约万分之三的挥发性成分,它丰富鲜艳的色彩来自所含的红色素、黄色素和β-胡萝卜素等天然色素。此外,尚含槲皮甙、脂肪油、有机酸等有益美容的物质。在每年的5-6月期间,当玫瑰花即将开时,分批摘取它的鲜嫩花蕾,再经严格的消毒、灭菌、风干,几乎完全保留了玫瑰花的色、香、味。取特殊加工过的花蕾3-5克,用沸水冲泡5分钟,可加糖或蜂蜜,或掺进自己喜欢的任何一种茶叶中一起冲泡,芳香怡人,有理气和血、舒肝解郁、降脂减肥、润肤养颜等作用。特别对妇女经痛、月经不调有神奇的功效。玫瑰不仅可供人观赏、美化环境,而且还具有神奇的疗效。《本草正文》中道:"玫瑰花,清而小浊,和而不猛,柔肝醒胃,疏气活血,宜通窒滞而绝无辛温刚燥之弊,断推气分药之中,最有捷效而最驯良,芳香诸品,殆无其匹"。玫瑰花中含有300多种化学成分,如芳香的醇、醛、脂肪酸、酚和含香精的油和脂,常食玫瑰制品可以柔肝醒胃、舒气活血、美容养颜、令人神爽。玫瑰初开的花朵及根可入药,有理气、活血、收敛等作用,主治月经不调、跌打损伤、肝气胃痛、乳臃肿痛等症。玫瑰果的果肉可制成果酱,具有特殊风味。果实含有丰富的VC及VP,可预防急、慢性传染病、冠心病、肝病和阻止产生致癌物质等,有些国家把果实用来做浓缩维生素制剂的原料。用玫瑰花瓣以蒸馏法提炼而得的玫瑰精油(古称玫瑰露),可活化男性荷尔蒙及精子,玫瑰露还可以改善皮肤质地,促进血液循环及新陈代谢。总之,玫瑰全身是宝,花、根、果均可入药。如花朵可作汤剂或丸剂,花霹调酒饮服,根主要作灼剂或汤剂,果实可作丸剂。
近年来由玫瑰提取的玫瑰纯露和精油产品在市场上深受各年龄层女性的喜爱,但现有市场上所售的玫瑰纯露或玫瑰水受蒸馏工艺限制所含玫瑰黄酮及其有效成分已微乎其微,并且在制作中通常会加入大量防腐剂以达到防腐效果,造成玫瑰水的刺激性增加,易引起过敏反应。
发明内容
针对上述问题,本发明提供了一种玫瑰花液及其制备方法,主要研究保加利亚玫瑰花瓣加工技术,应用于研制高浓度的玫瑰纯露。
一种玫瑰花液的制备方法,所述制备方法包括:
新鲜保加利亚玫瑰花瓣去叶洗净;
向洗净花瓣中加入活化水浸泡、活化处理,得到活化混合物;
水蒸气蒸馏提取所述活化混合物,得到蒸馏提取液;
稳定化处理所述蒸馏提取液,得到稳定液;
对所述稳定液进行过滤、辐照灭菌、检验灌装,得到玫瑰花液。
本申请采用珍贵的保加利亚玫瑰提取玫瑰花液,既保留了玫瑰精油的超强渗透性、抗皱效果及美白效果,又发挥了玫瑰纯露补水保湿的功效。且本申请玫瑰花瓣提取玫瑰花液技术,没有分离玫瑰精油这一步骤,含有大量玫瑰原液,和高浓度的玫瑰精油成分,完整的保留玫瑰所蕴含的大量有效成分(玫瑰精油及玫瑰黄酮等)。
进一步地,所述活化水的制造方式为:电解10-15%氯化钾水溶液得到所述活化水;
其中,电解条件为:电流强度为0.5-0.6A,电压为25—30v,氧化还原电位为-460到-400mV,阳极区和阴极区的流体流速为8-9cm3/h。
进一步地,所述活化水浸泡、活化处理包括:
所述洗净花瓣和所述活化水的料液比为1:2-1:7,pH=11-14;
混合后的所述洗净花瓣和所述活化水在45-50℃温度下,搅拌60-120分钟;
停止搅拌后在电场中进行倾析,所述电场提供0.5-0.6A的直流电和32—38v的电压进行活化13-25分钟。
水蒸气蒸馏提取中浸泡时间为0.5-2h,蒸馏时间为2-6小时,通过进一步试验确定最佳浸泡时间为1小时,蒸馏时间为5小时,在此条件下花液中精油的提取率最高。
为了实现蒸馏后水油成分很好的融合,蒸馏提取后,对于蒸馏提取液进行稳定处理,通过添加表面活性剂和超声波相结合的方式。
进一步地,所述稳定化处理具体为:在蒸馏提取液中添加0.3-0.5%的稳定成分;
所述稳定成分为非离子表面活性剂和聚乙二醇的混合液,或,
两性离子表面活性剂和PEG-40的混合液,或,
阴离子表面活性剂和非离子表面活性剂和氢化蓖麻油的混合液,或,
硅表面活性剂和辛甘醇的混合液;
所述稳定成分采用超声波分散技术进行分散。
进一步地,所述非离子表面活性剂和聚乙二醇的混合液中,所述非离子表面活性剂和所述聚乙二醇摩尔比为1:2-1:5。
进一步地,所述两性离子表面活性剂和PEG-40的混合液中,所述两性离子表面活性剂和所述PEG-40摩尔比为3:1-1.5:1。
进一步地,所述硅表面活性剂和辛甘醇的混合液中,所述硅表面活性剂和所述辛甘醇摩尔比为2:1。
进一步地,所述超声波分散频率为16KHZ-50KHZ,功率为30-80W。
本申请所选择的表面活性剂体系须具备以下基本的特点:(1)具有较好的水溶性;(2)与蒸馏液混合后,体系能较为容易、迅速地形成高含水量的精油包水型乳液;(3)同时粘度增加两倍以上。同时,由于本申请的稳定成分添加仅为极少量,在起到融合作用的同时最大限度的保留产品的天然性。
本发明还包括一种由上述制备方法获得的玫瑰花液。
本发明还包括一种通过上述制备方法获得的玫瑰花液在皮肤护理上的应用。
由上述方法制成的玫瑰花液在皮肤护理上效果明显。本申请获得的产品符合中华人民共和国轻工标准QB/T2660-2004《化妆水》标准要求。
(1)外观:均匀透明液体,不含杂质;
(2)香气:天然玫瑰花香气;
(3)色泽:透明无色或微黄色泽;
(4)耐热:(40±1)℃保持24h,恢复至室温后与试验前无明显性状差异;
(5)耐寒:(5±1)℃保持24h,恢复至室温后与试验前无明显性状差异;
(6)PH值(25度):4.0~8.5(直测法);
(7)细菌总数:≤1000CFU/g;
(8)霉菌和酵母菌总数:≤100CFU/g;
(9)粪大肠菌群:CFU/G未检出;
(10)金黄色葡萄球菌:CFU/g未检出;
(11)绿脓杆菌:CFU/G未检出;
(12)铅(以PB计):≤40mg/kg;
(13)汞(以HG计):≤1mg/kg;
(14)砷(以AS计):≤10mg/kg;
(15)铜绿假单胞菌:未检出;
(16)甲醇:≤2000mg/kg
本发明的玫瑰花液制备方法及所得玫瑰花液的有益效果在于:
(1)保持完整玫瑰花的有效成分
采用水蒸气蒸馏提取技术,蒸馏冷却后的玫瑰原液不进入油水分离器,直接进入蒸馏罐冷却,未提取精油的玫瑰原液保留了完整的玫瑰花有效成分:含挥发油(玫瑰油)、玫瑰黄酮、玫瑰醚及香茅醇、橙花醇、丁香油酚、苯乙醇、壬醇、苯甲醇、芳樟醇、乙酸苯乙酯,以及槲皮甙、苦味质、鞣质、没食子酸、胡萝卜素、红色素等成分。
(2)保持天然产品的活性成分技术
本发明的玫瑰花提取物在细胞培养中对干细胞的增殖作用,具有增强细胞活性的效果,具有活肤效果。能对尿酸酶抑制,具有减少体臭的性能,可用于抑汗类化妆品。对酪氨酸酶活性有一定的作用,有协助美白皮肤的作用。
(3)具有抗氧化作用
本发明的玫瑰花提取物除对羟基自由基和超氧自由基有消除外,在低剂量(0.2MG/ML)条件下,玫瑰花提取物即对DPPH(二苯基苦肼基自由基)有较强的清除能力,浓度越高效果越好,玫瑰花液可用作化妆品的抗氧剂;对脂肪氧合酶具有抑制效果。
(4)安全性高
采用特殊活化水蒸气蒸馏提取技术,原液不经油水分离环节,令提取的玫瑰花液精油浓度、纯度更高,药用价值更高,护肤效果更好。全部采用天然玫瑰花瓣,不经过任何防腐处理,在蒸馏水蒸馏之前采用活化处理从而不需要添加有机溶剂浸泡,无毒副作用,纯自然加工花瓣,保证玫瑰花液的安全性。
本发明的其它特征和优点将在随后的说明书中阐述,并且,部分地从说明书中变得显而易见,或者通过实施本发明而了解。本发明的目的和其他优点可通过在说明书、权利要求书以及附图中所指出的结构来实现和获得。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作一简单地介绍,显而易见地,下面描述中的附图是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1示出了根据本发明实施例浸泡时间对玫瑰花液中精油成分提取率的影响;
图2示出了根据本发明实施例蒸馏时间对玫瑰花液中精油成分提取率的影响;
图3示出了根据本发明实施例a、b、c、d组表面活性剂与助溶剂摩尔比对界面张力的影响。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地说明,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
新鲜保加利亚玫瑰花瓣1公斤去叶洗净。电解15%氯化钾水溶液得到的活化水,其中电流强度为0.6A,电压为30v,氧化还原电位为-460mV,阳极区和阴极区的流体流速为8cm3/h。
按照料液重量比1:4加入活化水浸泡0.5h,pH=12,然后搅拌,在45℃温度下保持60分钟,倾析在电场中进行,提供0.5A的直流电和32W的电压进行活化13分钟,停止活化后浸泡1h,水蒸气蒸馏2h提取玫瑰花液,得到玫瑰花蒸馏液。
实施例2
新鲜保加利亚玫瑰花瓣1公斤去叶洗净。电解13%氯化钾水溶液得到的活化水,其中电流强度为0.5A,电压为30W,氧化还原电位为-400mV,阳极区和阴极区的流体流速为9cm3/h。
按照料液重量比1:3加入活化水浸泡1h,pH=11,并搅拌,50℃温度下保持100分钟,倾析在电场中进行,提供0.5A的直流电和34W的电压进行活化15分钟,停止活化后浸泡0.5h,水蒸气蒸馏1.5h提取玫瑰花液,得到玫瑰花蒸馏液。
比较例1
新鲜保加利亚玫瑰花瓣1公斤去叶洗净。采用传统工艺制直接蒸馏:按照料液重量比1:3加入蒸馏水浸泡1h,pH=6.44±0.4,水蒸气蒸馏1.5h提取玫瑰花液。
对比过程:用GC-MS气质联用仪(型号:6890N,工作站:5973NETWORK,美国Agilent公司生产)对实施例1、2和比较例1提取的玫瑰花蒸馏液中有效成分、成分含量及理化指标进行测定及分析,具体测量结果见表1,表1数据为提取的玫瑰精油的色谱图像汇总。
表1实施例1、2和比较例中含玫瑰有效成分量
项目 | 实施例1 | 实施例2 | 比较例(蒸馏水) |
挥发油(玫瑰油)‰ | 2.93 | 2.85 | 1.81 |
玫瑰黄酮% | 2.6 | 1.8 | 1.5 |
玫瑰醚% | 0.8 | 1.2 | 0.9 |
香茅醇% | 36 | 38 | 30 |
对比结果:由表1可知实施例1和实施例2所制备的玫瑰花蒸馏液中,有效物质的含量全部明显高于采用传统蒸馏工艺制备的玫瑰花蒸馏液。说明采用本发明采用水蒸气蒸馏提取技术,蒸馏冷却后的玫瑰原液不进入油水分离器,直接进入蒸馏罐冷却,使得玫瑰原液保留了完整的玫瑰花有效成分:含挥发油(玫瑰油)、玫瑰黄酮、玫瑰醚及香茅醇、橙花醇、丁香油酚、苯乙醇、壬醇、苯甲醇、芳樟醇、乙酸苯乙酯,以及槲皮甙、苦味质、鞣质、没食子酸、胡萝卜素、红色素等成分。
蒸馏参数及稳定成分确定
申请人通过实验发现,对本发明的水蒸气蒸馏工艺进行试验研究,在工艺的影响因素中,料液比>浸泡时间>蒸馏时间。确定料液比为1:6后,在浸泡时间为0.5-2h,蒸馏时间为2-6小时的范围内,进一步试验确定最佳浸泡时间、蒸馏时间。
采用1:6的料液比和5h的蒸馏时间,研究不同浸泡时间对蒸馏得到的玫瑰花液中精油提取率的影响,选取浸泡0.25h、0.5h、1h以及2h的条件下进行提取率检测,绘制浸泡时间—精油提取率标准曲线,所得标准曲线如图1所示。
采用1:6的料液比和1.5h的浸泡时间,研究不同蒸馏时间对玫瑰花液中精油提取率的影响。选取蒸馏2h、3h、4h、5h以及6h的条件下进行提取率检测,绘制蒸馏时间—精油提取率标准曲线,所得标准曲线如图2所示。
通过图1和图2可知,料液比为1:6时,浸泡时间为1h,蒸馏时间为5h的水蒸气蒸馏工艺下玫瑰花液中精油提取率最高。
随后需要对玫瑰花蒸馏液进行稳定化处理,此时对于稳定助剂的选择尤为关键。须具备以下基本的特点:(1)具有较好的水溶性;(2)与原油混合后,体系能较为容易、迅速地形成高含水量的油包水型乳液;(3)同时体系的粘度较原油体系有较大幅度增加,至少粘度为原油体系的2倍以上。
发明人试验了大量不同乳化体系与蒸馏水的混合性能,以便寻找到符合上述要求的稳定剂体系。其中使用的表面活性剂浓度为0.3%(质量分数),助溶剂浓度为0.15%(质量分数),经测试获得表2结果。
测试大量不同乳化体系与蒸馏水的混合性能,以便寻找到符合上述要求的稳定剂体系。其中使用的表面活性剂浓度为0.3%(质量分数),助溶剂浓度为0.15%(质量分数),经测试获得表2结果。
表2不同乳化体系与蒸馏水混合性能
由表2可知,采用编号1、2、3、4体系的表面活性剂和助溶剂体系时无法同时实现水溶性、乳化性和增粘性三种性能的有益组合,而比较而言采用编号a、b、c、d体系的表面活性剂和助溶剂体系能够同时获得有益的三种性能。
随后,调整表面活性剂和助溶剂之间的比例关系,对于获得优异的水溶性、乳化性和增粘性的abcd四种体系的界面性能进行进一步测试。
表面活性剂和助溶剂总浓度为0.3%(w),按照相应比例的摩尔比混合。放置48h后,测定油水界面张力。表面张力采用滴体积法测定,表面张力曲线的转折点对应的浓度和表面张力分别为临界胶束浓度(cmc)和γcmc,饱和吸附量(Г∞)由Gibbs公式求得:
其中,γ是表面张力,c是表面活性剂浓度,对于阴阳离子表面活性剂体系,n=1,则表面活性剂分子最小吸附面积(Amin)为:
其中,NA为阿伏伽德罗常数。
将所使用的a、b、c、d组剂型分别加入到TX500C型旋滴法界面张力仪的样品管中,再注入对应的油相,恒温50℃待界面张力稳定后测定平衡界面张力,旋转角速度为5000r·s-1。
测试结果:编号为abcd的混合溶液中表面活性剂与助溶剂采用的不同摩尔比对界面张力的影响如图3所示。
由图3可知为保证稳定成分体系有更好的界面张力,在a组非离子表面活性剂季戊四醇和聚乙二醇的混合液中,季戊四醇和聚乙二醇的最佳摩尔比为1:2-1:5;
在b组两性离子表面活性剂脂肪醇聚氧乙烯醚硫酸钠/季戊四醇和PEG-40的混合液中,脂肪醇聚氧乙烯醚硫酸钠/季戊四醇和PEG-40最佳摩尔比为1.5:1-1:3;
在c组硅表面活性剂DC8500和辛甘醇的混合液中,DC8500和辛甘醇最佳摩尔比为2:1;
在d组两性离子璜基甜菜碱和PEG-40氢化蓖麻油,璜基甜菜碱和PEG-40氢化蓖麻油的最佳摩尔比为3:1-1.5:1。
实施例3
在实施例1的蒸馏提取液中添加0.3%的摩尔比为1:2的季戊四醇和聚乙二醇混合液,然后进行超声分散,超声波分散频率为50KHZ,功率为30w。声强为100w/cm2。
实施例4
在实施例2的蒸馏提取液中添加0.3%摩尔比为3:1的璜基甜菜碱:PEG-40,然后进行超声分散,超声波分散频率为40KHZ,功率为50w。声强为200w/cm2。
比较例2
对于比较例1获得的玫瑰花提取液进行油水分离,获得玫瑰花精油和纯露两种产品。
对比过程:通过电催化氧化法制的羟基自由基,将实施例3、4的玫瑰花液和比较例2制得的玫瑰花精油、玫瑰花纯露涂抹于面膜纸上然后浸入羟基自由基溶液,于10分钟左右注入石英毛细管中进行ESR检测(电子自旋共振)。同时还测试了超氧自由基以及DPPH(二苯基苦肼基自由基)清除率,结果如表3所示:
表3实施例3、4与比较例2中各自由基清除率值
项目 | 实施例3 | 实施例4 | 比较例2精油 | 比较例2纯露 |
羟基自由基清除率% | 93 | 95 | 92 | 80 |
超氧自由基清除率% | 76 | 78 | 75 | 42 |
DPPH清除率% | 60 | 58 | 57 | 38 |
由表3可知,本发明的制备方法可以实现和同等剂量下纯精油相近的抗氧化效果,但提取同样剂量的纯精油需要更多的玫瑰花,因此,本申请实际上成本更为低廉,同时本申请花液的抗氧化效果也要明显优于纯露。同时说明本申请的玫瑰花液除对羟基自由基和超氧自由基有消除外,在低剂量(0.2MG/ML)条件下,玫瑰花提取物对DPPH(二苯基苦肼基自由基)也有较强的清除能力,浓度越高效果越好,表明玫瑰花液是良好的化妆品抗氧成分,具有延缓衰老的作用。此外,本申请的玫瑰花液对脂肪氧合酶也有很好的抑制效果。
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:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分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各实施例技术方案的精神和范围。
Claims (6)
1.一种玫瑰花液的制备方法,其特征在于,所述制备方法包括:
新鲜保加利亚玫瑰花瓣去叶洗净;
向洗净花瓣中加入活化水浸泡、活化处理,得到活化混合物;
水蒸气蒸馏提取所述活化混合物,得到蒸馏提取液;
稳定化处理所述蒸馏提取液,得到稳定液;
对所述稳定液进行过滤、辐照灭菌、检验灌装,得到玫瑰花液;
所述稳定化处理具体为:在所述蒸馏提取液中添加0.3-0.5%的稳定成分;
所述稳定成分为季戊四醇和聚乙二醇的混合液,或,
磺基甜菜碱和PEG-40氢化蓖麻油的混合液,或,
脂肪醇聚氧乙烯醚硫酸钠/季戊四醇和PEG-40氢化蓖麻油的混合液,或,
DC8500和辛甘醇的混合液;
所述稳定成分在所述蒸馏提取液中采用超声波分散技术进行分散;
其中,所述季戊四醇和聚乙二醇的混合液中,所述季戊四醇和所述聚乙二醇摩尔比为1:2-1:5;
所述磺基甜菜碱和PEG-40氢化蓖麻油的混合液中,所述磺基甜菜碱和所述PEG-40氢化蓖麻油摩尔比为3:1-1.5:1;
所述脂肪醇聚氧乙烯醚硫酸钠/季戊四醇和PEG-40氢化蓖麻油的混合液中,所述脂肪醇聚氧乙烯醚硫酸钠/季戊四醇和所述PEG-40氢化蓖麻油摩尔比为1.5:1-1:3;
所述DC8500和辛甘醇的混合液中,所述DC8500和所述辛甘醇摩尔比为2:1。
2.如权利要求1所述的制备方法,其特征在于,所述活化水的制造方式为:电解10-15%氯化钾水溶液得到所述活化水;
其中,电解条件为:电流强度为0.5-0.6A,电压为25—30v,氧化还原电位为-460到-400mV,阳极区和阴极区的流体流速为8-9cm3/h。
3.如权利要求2所述的制备方法,其特征在于,所述活化水浸泡、活化处理包括:
所述洗净花瓣和所述活化水的料液比为1:2-1:7,pH=11-14;
混合后的所述洗净花瓣和所述活化水在45-50℃温度下,搅拌60-120分钟;
停止搅拌后在电场中进行倾析,所述电场提供0.5-0.6A的直流电和32—38v的电压进行活化13-25分钟。
4.如权利要求1所述的制备方法,其特征在于,所述超声波分散频率为16KHZ-50KHZ,功率为30-80W。
5.一种由权利要求1-4任一项所述制备方法获得的玫瑰花液。
6.一种由权利要求1所述制备方法获得的玫瑰花液在制备皮肤护理产品上的应用。
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