CN105708760A - 天女木兰提取液作为抑菌剂的用途 - Google Patents
天女木兰提取液作为抑菌剂的用途 Download PDFInfo
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Abstract
本发明公开了一种天女木兰提取液作为抑菌剂的用途;本发明采用水蒸气蒸馏、水提法或醇提法制备天女木兰提取液,均是一步法完成,工艺操作简单,制备得到的天女木兰提取液不含有机溶剂,无有害物质残留,刺激性小,符合绿色天然概念。本发明通过抑真菌测试、抑菌圈实验测试、防腐挑战实验测试天女木兰提取液的抑菌效果,证实天女木兰提取液可以显著起到抑制霉菌和酵母菌等真菌的抑菌作用,大大拓宽了天女木兰提取液在市场中的应用范围。将本发明的天女木兰提取液应用到化妆品、食品、保健品中作为抑菌剂,添加量少,且可以对化妆品、食品、保健品起到抑制霉菌和酵母菌等真菌的抑菌作用。
Description
技术领域
本发明涉及天女木兰提取液的新用途,特别涉及天女木兰提取液作为抑菌剂的用途。
背景技术
随着生活水平提高,越来越多人开始关注化妆品、食品、保健品中防腐剂安全问题,传统的防腐剂多为化学合成的,如苯甲酸钠、福尔马林、尼泊金酯、硝酸盐等,其在化妆品、食品、保健品中存在一些致癌、皮肤刺激等风险。
近年来,一方面,无尼泊金酯类的化妆品多了起来,多以苯氧乙醇或者二元醇系作为抗菌成分,但是其缺点在于连续使用多元醇防腐体系,皮肤接触多元醇过多,造成多元醇累加,皮肤会有发热感和刺激感,更甚者皮肤起红斑丘疹;另一方面,虽然人们也知道有很多种植物具有抗菌作用,但因其特有的抗菌特性,作为化妆品的防腐成分其防腐效果还是有很多不足,另外植物所特有的颜色以及气味对化妆品的品质有所影响,因此植物提取物作为防腐成分在化妆品中的使用只限于一部分化妆品。因此,研究开发一种新型高效安全天然的植物防腐剂,对于化妆品、食品、保健品等领域要重要意义。
天女木兰,属于木兰科木兰属植物,为落叶小乔木,分布在我国东北辽宁及朝鲜、日本。因花的花瓣洁白、雄蕊紫色、香气迷人、形似天女而得名天女木兰。天女木兰乃珍奇花木,系太古第四纪冰川期幸存的珍稀名贵花卉,被列入国家濒危植物名录,是我国重点保护的世界珍惜植物,叶如翠雕,花似玉琢,具有浓郁的芳香,可入药,叶含芳香油,含油量高达0.2%,是重要的园林绿化树种和提取香料的轻工业原料。中国专利CN1289835A公开了采用水蒸气蒸馏法从天女木兰叶中提取精天女木兰精油,油香气浓,留香持久,透发性好,略带醛味;对皮肤无刺激,无毒安全,无副作用,是优质的纯天然香料,可用于调配化妆品、洗涤品用的香精中,以及药用中。
目前,天女木兰精油被广泛应用为一种优质的纯天然香料,但是对在提取天女木兰精油过程中产生的废料天女木兰提取液作为抑菌剂的用途的文献未见报道。本发明制备的天女木兰提取液具有非常强的抑制霉菌和酵母菌能力,有望开发一款纯天然的植物防腐剂,用于护肤品、食品和保健品中。
发明内容
本发明旨在给出一种天女木兰提取液作为抑菌剂的用途。
优选地,本发明所述的天女木兰提取液作为在化妆品、食品、保健品中的抑菌剂的用途。
其中,所述抑菌剂的抑菌种类为抑制真菌,优选为抑制霉菌或抑制酵母菌。
其中,所述天女木兰提取液的加入量占化妆品总重量的0.1-1wt%;优选为0.3-0.8wt%。
当天女木兰提取液的加入量占化妆品总重量超过1wt%,会造成生产过高和浪费,另外也会对某些配方体系造成一定的风险,如料体变色或者沉淀等等。
其中,所述天女木兰提取液的加入量占食品总重量的0.1-1wt%;优选为0.3-0.8wt%。
当天女木兰提取液的加入量占食品总重量超过1wt%,会造成生产过高和浪费,还可能造成食品中营养成分活性下降,在安全方面也存在一定的风险。
其中,所述天女木兰提取液的加入量占保健品总重量的0.1-1wt%;优选为0.3-0.8wt%。
当天女木兰提取液的加入量占保健品总重量超过1wt%,会造成生产过高和浪费,还可能造成保健中活性成分活性下降,同时在安全方面也存在一定的风险。
本发明所述的天女木兰提取液可以采用水蒸气蒸馏法制备得到,包括如下步骤:取天女木兰叶粉碎至10-20目,装在3-5个串联水蒸气蒸馏反应釜中,分散均匀,加上网罩,通入水蒸气,打开冷凝器,反应1-2h,收集提取物,分离油和水,得到天女木兰提取液。
本发明所述的天女木兰提取液也可以采用水提法制备得到,包括如下步骤:取天女木兰叶粉碎至30-50目,按照质量体积料液比1:2-1:5加入蒸馏水,同时加入基于天女木兰叶总质量的1-3wt%的纤维素酶,在50-60℃条件下提取1-3h,过滤,加入基于滤液总质量的0.5wt%且质量复配比为1:1的活性炭和活性白土的复配脱色剂进行脱色,过陶瓷膜除掉脱色剂,得到天女木兰提取液。
本发明所述的天女木兰提取液也可以采用醇提法制备得到,包括如下步骤:取天女木兰叶粉碎至30-50目,按照质量体积料液比1:2-1:4加入体积分数为50-80%的乙醇;在60-80℃条件下,搅拌,冷凝回流,提取1-3h,过滤,得到滤液。用旋转蒸发仪脱掉滤液里面的乙醇,至溶液里面无醇味,加水补回蒸发掉的乙醇。加入基于滤液总质量的0.5wt%且质量复配比为1:1的活性炭和活性白土的复配脱色剂进行脱色,过陶瓷膜除掉脱色剂,得到天女木兰提取液。
本发明意外的发现,将天女木兰提取液作为抑菌剂添加到化妆品、食品、保健品中,天女木兰提取液可以显著起到抑制霉菌和酵母菌等真菌的抑菌作用,大大拓宽了天女木兰提取液在市场中的应用范围。
与现有技术相比,本发明具有如下有益效果:
1)本发明采用水蒸气蒸馏、水提法或醇提法制备天女木兰提取液,均是一步法完成,工艺操作简单,且天女木兰提取液的提取率较高。
2)本发明采用水蒸气蒸馏、水提法或醇提(后续脱醇)法制备天女木兰提取液,制备得到的天女木兰提取液不含有机溶剂,无有害物质残留,刺激性小,符合绿色天然概念。
3)本发明通过抑(霉)菌测试、抑菌圈实验测试、防腐挑战实验测试天女木兰提取液的抑菌效果,证实天女木兰提取液可以显著起到抑制霉菌和酵母菌等真菌的抑菌作用,大大拓宽了天女木兰提取液在市场中的应用范围。
4)将本发明的天女木兰提取液应用到化妆品、食品、保健品中作为抑菌剂,添加量少,且可以对化妆品、食品、保健品起到抑制霉菌和酵母菌等真菌的抑菌作用。
具体实施方式
下面通过具体实施方式来进一步说明本发明,以下实施例为本发明较佳的实施方式,但本发明的实施方式并不受下述实施例的限制。
实施例1:水蒸气蒸馏法制备天女木兰提取液
取50kg天女木兰叶,进行粉碎至20目,装在4个串联水蒸气蒸馏反应釜中,分散均匀,加上网罩,通入水蒸气,打开冷凝器,反应1h,收集提取物,分离油和水,得到天女木兰提取液12.8kg。再浓缩一定比例,得到本实验所用的天女木兰提取液。
实施例2:水提法制备天女木兰提取液
取1kg天女木兰叶粉碎至40目,按照质量体积料液比1:3加入蒸馏水,同时加入基于天女木兰叶总质量的2wt%的纤维素酶,在50-60℃条件下提取2h,过滤,得到滤液,加入基于滤液总质量的0.5wt%且质量复配比为1:1的活性炭和活性白土的复配脱色剂进行脱色,过陶瓷膜,得到天女木兰提取液2.4kg。
实施例3:醇提法制备天女木兰提取液
取1kg天女木兰叶粉碎至40目,按照质量体积料液比1:3加入体积分数75%乙醇,在70℃条件下,搅拌,冷凝回流,提取2h,过滤,得到滤液。用旋转蒸发仪脱掉滤液里面的乙醇,至溶液里面无醇味,加水补回蒸发掉的乙醇。加入基于滤液总质量的0.5wt%且质量复配比为1:1的活性炭和活性白土的复配脱色剂进行脱色,过陶瓷膜除掉脱色剂,得到天女木兰提取液1.1-3.3kg。
抑菌效果的测试
1.1抑(霉)菌测试
取2012年、2014年、2015年按照实施例1制备的天女木兰提取液,隔0天、7天、14天、21天和28天分别检测该三种天女木兰提取液里面微生物情况;实验结果如表1所示:
结论:通过一个月的微生物检测显示,每一个批次的天女木兰提取液霉菌指标均为检出,充分说明天女木兰提取液具有抑制霉菌效果;另外2012年批次天女木兰提取液放置三年,仍然澄清透明,霉菌检测均充分说明了天女木兰水具有持久性抑制霉菌效果。
抑菌圈实验测试
1.2.1抑菌片的制备
按照要求将抑菌剂(天女木兰提取液)配置成试验所需浓度。取干燥备用的滤纸片,置37℃温箱或室温干燥备用。(溶出性抗抑菌产品,可直接制成直径为8mm,厚度不超过4mm圆片)。
1.2.2阴性对照样片的制备
取干燥备用的滤纸片,每片滴加无菌蒸馏水或抑菌剂溶剂20ul,干燥备用。
1.2.3试验菌的接种
取0.5ml浓度为5×105cfu/ml~5×106cfu/ml试验菌悬液与无菌培养皿,倒入营养琼脂培养基于平板并摇匀;盖好平板,置室温干燥5min。
1.2.4抑菌剂样片贴放
用无菌镊子取样片贴放于平板表面,立即滴加20ul抑菌剂。每次试验贴放3个染菌平板,其中2个平板每个贴放1片试验样片,另外一个平板贴放1片阴性对照样片,贴放好后,盖好平皿,置37℃培养箱培养16~18h观察结果;用卡尺测量抑菌环的直径(包括贴片)并记录。(测量抑菌环时,应选均匀而完全无菌生长的抑菌环进行;测量其直径应以抑菌环外沿为界)实验结果表2所示:
表2天女木兰提取液的抑菌圈测试结果
结论:对于天女木兰提取液作为抑菌剂的抑菌圈测试结果可知,其抑菌环直径为14mm,与空白对照可知,天女木兰提取液具有很强的抑制霉菌或酵母菌的抑菌效果,对细菌的抑制效果不明显。
防腐挑战实验测试防腐挑战实验测试
参照美国药典USP30(51)对天女木兰提取液做了一个防腐挑战实验,测试结果如表3所示:
表3天女木兰提取液的防腐挑战测试结果
结论:经过天女木兰提取液的7天防腐挑战测试结果可知,霉菌和酵母菌的对数减少至为3.85(基本杀死一半),14天为4.64,21天霉菌和酵母菌全杀死,表现出非常显著的杀霉菌和酵母菌的能力;而细菌7天的对数减少值为2.83,后期对数减少基本稳定在3左右,说明对细菌具有一定的抑制能力,但不显著。
总结:天女木兰提取液具有非常强的抑制霉菌或酵母菌的抑菌效果,但是对抑制细菌效果一直较弱。
应用实施例1:天女木兰提取液应用于喷雾剂型化妆品
按以下组分及含量配料并制备喷雾剂型化妆品:
主要组分配比(%为质量百分数)
A1水82.00%~91.00%;
A2冰川水1.00%~5.00%;
A3丁二醇1.00%~3.00%;
A4β-葡聚糖0.05%~0.30%;
A5香橙果提取物0.05%~0.30%;
B1水解植物蛋白0.001%~0.003%;
B2卤虫提取物0.001%~0.003%;
C1甘草酸二钾0.001%~0.003%;
SP1天女木兰提取液0.8%。
将上述喷雾剂型化妆品进行28天防腐挑战实验,测试结果如表4所示:
表4喷雾剂型化妆品的防腐挑战测试结果
经过28天防腐挑战实验,上述喷雾剂型化妆品里面的霉菌和酵母菌对数减少值为4.26,总菌落总数<10cfu/g,说明天女木兰提取液能够有效地抑制喷雾剂型化妆品里面的霉菌和酵母菌的生长。另外,细菌经过21天的防腐,对数减少为2.70,后期细菌总数基本维持在2.70左右。说明天女木兰提取液对喷雾剂型化妆品里面的细菌也具有一定的抑制作用。
应用实施例2:天女木兰提取液应用于面霜剂型化妆品
按以下组分及含量配料并制备面霜剂型化妆品:
主要组分配比(%为质量百分数)
A1水50.00%~55.00%;
A2冰川水1.00%~5.00%;
A3丁二醇1.00%~3.00%;
A4甘草酸二钾0.001%~0.003%;
A51,3-丙二醇5.00%~8.00%;
A6甘油2.00%~4.00%;
A71,2-己二醇0.40%~0.60%;
A81,2-戊二醇1.00%~3.00%;
A9月桂酰胺谷氨酰胺0.40%~0.60%;
B1聚二甲基硅氧烷2.00%~4.00%;
B2鲸蜡醇乙基己酸酯1.00%~4.00%;
B3角鲨烷1.00%~1.50%;
B4山嵛醇1.00%~1.50%;
B5澳洲坚果1.00%~2.00%;
B6鲸蜡硬脂醇2.00%~3.00%;
C1卡波姆3.00%~4.00%;
C2蔗糖硬脂酸酯0.60%~0.80%;
D1银耳提取物0.0004%~0.0006%;
D2β-葡聚糖0.04%~0.06%;
ST1白藜芦醇0.0001%~0.0002%;
SP1天女木兰提取液0.8%。
将上述面霜剂型化妆品进行28天防腐挑战实验,测试结果如表5所示:
表5面霜剂型化妆品的防腐挑战测试结果
经过28天防腐挑战实验,上述面霜剂型化妆品里面的霉菌和酵母菌对数减少值为4.64,总菌落总数<10cfu/g,说明天女木兰提取液能够有效地抑制面霜剂型化妆品里面的霉菌和酵母菌的生长。另外,细菌经过28天的防腐,对数减少为5.85,菌落总数<10cfu/g。说明天女木兰提取液对面霜剂型化妆品里面的细菌也具有一定的抑制作用。
应用实施例3:天女木兰提取液应用于乳液剂型化妆品
按以下组分及含量配料并制备乳液剂型化妆品:
主要组分配比(%为质量百分数)
A1水54.00%~56.00%;
A2甘油5.00%~7.00%;
A3黄原胶0.10%~0.30%;
A4月桂酰胺谷氨酰胺0.08%~0.12%;
B1角鲨烷5.00%~8.00%;
B2聚二甲基硅氧烷5.00%~7.00%;
B3鲸蜡硬脂醇2.00%~3.00%;
B4红花籽油0.50%~1.50%;
B5苯基聚甲基硅氧烷1.00%~2.00%;
C1蔗糖硬脂酸酯0.50%~1.50%;
C2聚丙烯酸2.00%~3.00%;
D1欧洲山杨树皮提取物0.05%~0.15%;
E1茵陈蒿花提取物0.05%~0.15%;
E2丁香花提取物0.05%~0.15%;
F1β-葡聚糖1.50%~2.50%;
F3香橙果提取物0.05%~0.15%;
SP1天女木兰提取液0.8%。
将上述乳液剂型化妆品进行28天防腐挑战实验,测试结果如表6所示:
表6乳液剂型化妆品的防腐挑战测试结果
经过28天防腐挑战实验,上述乳液剂型化妆品里面的霉菌和酵母菌对数减少值为4.76,总菌落总数<10cfu/g,说明天女木兰提取液能够有效地抑制乳液剂型化妆品里面的霉菌和酵母菌的生长。另外,细菌经过28天的防腐,对数减少为4.45,说明天女木兰提取液对乳液剂型化妆品里面的细菌也具有一定的抑制作用。
Claims (9)
1.天女木兰提取液作为抑菌剂的用途。
2.根据权利要求1所述的天女木兰提取液作为抑菌剂的用途,所述天女木兰提取液作为在护肤品、食品、保健品中的抑菌剂的用途。
3.根据权利要求1或2所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述抑菌剂的抑菌种类为抑制真菌,优选为抑制霉菌或抑制酵母菌。
4.根据权利要求2所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述天女木兰提取液的加入量占化妆品总重量的0.1-1wt%;优选为0.3-0.8wt%。
5.根据权利要求2所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述天女木兰提取液的加入量占食品总重量的0.1-1wt%;优选为0.3-0.8wt%。
6.根据权利要求2所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述天女木兰提取液的加入量占保健品总重量的0.1-1wt%;优选为0.3-0.8wt%。
7.根据权利要求1-6任一项所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述天女木兰提取液的制备方法,包括如下步骤:取天女木兰叶粉碎至10-20目,装在3-5个串联水蒸气蒸馏反应釜中,分散均匀,加上网罩,通入水蒸气,打开冷凝器,反应1-2h,收集提取物,分离油和水,得到天女木兰提取液。
8.根据权利要求1-6任一项所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述天女木兰提取液的制备方法,包括如下步骤:取天女木兰叶粉碎至30-50目,按照质量体积料液比1:2-1:5加入蒸馏水,同时加入基于天女木兰叶总质量的1-3wt%的纤维素酶,在50-60℃条件下提取1-3h,过滤,加入基于滤液总质量的0.5wt%且质量复配比为1:1的活性炭和活性白土的复配脱色剂进行脱色,过陶瓷膜除掉脱色剂,得到天女木兰提取液。
9.根据权利要求1-6任一项所述的天女木兰提取液作为抑菌剂的用途,其特征在于,所述天女木兰提取液的制备方法,包括如下步骤:取天女木兰叶粉碎至30-50目,按照质量体积料液比1:2-1:4加入体积分数为50-80%的乙醇;在60-80℃条件下,搅拌,冷凝回流,提取1-3h,过滤,得到滤液;用旋转蒸发仪脱掉滤液里面的乙醇,至溶液里面无醇味,加水补回蒸发掉的乙醇;加入基于滤液总质量的0.5wt%且质量复配比为1:1的活性炭和活性白土的复配脱色剂进行脱色,过陶瓷膜除掉脱色剂,得到天女木兰提取液。
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CN113101316A (zh) * | 2021-04-23 | 2021-07-13 | 花安堂生物科技集团有限公司 | 天女木兰提取物在制备抗抑郁产品中的应用 |
CN113288834A (zh) * | 2021-04-23 | 2021-08-24 | 花安堂生物科技集团有限公司 | 天女木兰提取物的新应用 |
CN113694098A (zh) * | 2020-05-22 | 2021-11-26 | 广东省禾基生物科技有限公司 | 一种天女木兰细胞水的提取方法及其应用 |
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CN113101316B (zh) * | 2021-04-23 | 2022-11-25 | 花安堂生物科技集团有限公司 | 天女木兰提取物在制备抗抑郁产品中的应用 |
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