CN114787118A - 木糖醇羧酸酯及其酶促制备方法 - Google Patents
木糖醇羧酸酯及其酶促制备方法 Download PDFInfo
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- CN114787118A CN114787118A CN202080086956.1A CN202080086956A CN114787118A CN 114787118 A CN114787118 A CN 114787118A CN 202080086956 A CN202080086956 A CN 202080086956A CN 114787118 A CN114787118 A CN 114787118A
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- xylitol
- carboxylic acid
- evonik
- gmbh
- acid
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明的主题是木糖醇羧酸酯和酶促制备木糖醇羧酸酯的方法。
Description
发明领域
本发明的主题是木糖醇羧酸酯和酶促制备木糖醇羧酸酯的方法。
现有技术
木糖醇羧酸酯是食品和化妆品行业感兴趣的产品,一方面因为它们的表面活性剂性能,另一方面因为它们可以从天然和可再生原料中获得。
EP2902009A1描述了木糖醇与脂肪酸在不存在溶剂、在存在催化剂如对甲苯磺酸(pTSA)情况下在高达200℃的温度下历经8小时的经典化学酯化,以及使用由此获得的木糖醇羧酸酯作为化妆品配制剂中的活性成分。
经典化学酯化方法的缺点是,在这些条件下,木糖醇总是至少部分经历脱水或降解(Biotechnol. Bioeng. 1995, 48, 214-221)。在这样的条件下经常出现的木糖醇降解产物是脱水戊糖醇1,4-脱水木糖醇、1,4-脱水阿拉伯糖醇和1,4-脱水核糖醇(J.Carbohydr. Chem. 2004, 23, 4, 169-177和Adv. Carbohydr. Chem. Biochem., 1983,41, 27-66)。现有技术中描述的所述方法的另一个缺点是附加的方法步骤如活性炭和白土(硫酸钙)的使用和随后去除以改善所得产品的颜色和气味。
Pedersen等人(Enzyme Microb. Technol.2007, 41, 3, 346-352)描述了在45℃温度下使用溶剂如叔丁醇和吡啶来酶促合成木糖醇羧酸酯。现有技术中描述的此方法的缺点是溶剂的使用是食品或化妆品领域中使用的障碍,除此之外,必要的溶剂去除需要额外的方法步骤如结晶、过滤或蒸馏。
Basri等人(Carbohydr. Res. 2011, 346, 472-479)描述了使用来自南极假丝酵母的脂肪酶,在最高70℃和最佳60℃温度下,木糖醇与癸酸以及与己酸的无溶剂酯化。该方法产生产物混合物,其中酯化伯OH基团与酯化仲OH基团的比率总是大于80:20。现有技术中描述的该方法的缺点是使用分子筛,这使得在工业规模上实施困难。现有技术中描述的该方法的另一个缺点是使用溶剂或溶剂混合物来终止反应、去除酶和分子筛。此程序意味着额外的方法步骤来去除使用的溶剂,并消除了无溶剂工艺的优势。现有技术中描述的该方法的另一个缺点是在酯分布中以超过50%的相对比例获得木糖醇三羧酸酯作为主要组分。现有技术中描述的该方法的另一个缺点是酶负载不清楚。现有技术中描述的这种方法的另一个缺点是转化率低,只有约 70%,因此约15%的相对大量的脂肪酸残留在产物混合物中,这需要随后去除脂肪酸(任选预先中和)以避免不需要的副产物或者在例如己酸、辛酸和癸酸的情况下避免难闻的气味。现有技术中描述的该方法的另一个缺点是对长链脂肪酸的选择性。
Tan等人(J. Mol. Catal. B-Enzym 2013, 89, 61-66)描述了使用脂肪酶(假丝酵母属(Candida sp) 99-125)在最高50℃下,木糖醇与癸酸的无溶剂酯化。从给出的分析数据可以推断,酯化伯OH基团与酯化仲OH基团的比率总是大于80:20。现有技术中描述的该方法的一个缺点是使用非常精细研磨的木糖醇(粒度 < 0.2 mm),对于工业规模的实施,这意味着额外的工艺步骤和使用特殊设备(例如 Dispermat或特殊研磨机)。现有技术中描述的该方法的另一个缺点是长的反应时间(>100小时)。现有技术中描述的该方法的另一个缺点是在>140℃的温度下去除副产物,这对产品的颜色具有不利影响。现有技术中描述的该方法的另一个缺点是使用不可商购的酶。现有技术中描述的该方法的另一个缺点是该酶不是从野生型中分离的。
现有技术中描述的该方法的另一个缺点是使用非固定化酶,这使得从安全技术角度来看的操作以及产品分离困难。现有技术中描述的该方法的另一个缺点是所用脂肪酶的可回收性差。在现有技术中描述的该方法的另一个缺点是使用分批补料法来避免由过量的木糖醇或癸酸引起的高粘度。现有技术中描述的这种方法的另一个缺点是使用分批补料法,这需要特殊的测量和控制技术。现有技术中描述的该方法的另一个缺点是水的添加,在该方法结束时必须再次去除水。
KR101939851B1描述了脱水木糖醇的酯、由此用于制备木糖醇羧酸酯的经典化学酯化方法的上述副产物、以及这些脱水木糖醇的羧酸酯作为乳液中的流变添加剂/粘度调节剂的用途。现有技术中描述的脱水木糖醇羧酸酯的缺点是它们的亲水性降低。现有技术中描述的脱水木糖醇羧酸酯的另一个缺点是它们的颜色深。这样的脱水木糖醇羧酸酯的另一个缺点是在水性表面活性剂体系中的增稠性能不足。
本发明的目的是提供用于制备糖酯和/或糖醇酯的方法,该方法能够克服现有技术方法的至少一个缺点。
发明描述
令人惊讶地发现,下文所述的木糖醇羧酸酯和下文所述的方法能够实现本发明提出的目的。
本发明的优点在于,与现有技术相比,本发明的木糖醇羧酸酯是用于水性表面活性剂体系的优异增稠剂。
另一个优点是,与现有技术相比,本发明的木糖醇羧酸酯还具有优异的颜色和非常好的气味。本发明的优点是仅获得非常少量的木糖醇降解产物或降解产物的酯作为反应产物。本发明的优点是本发明的方法可以在不存在溶剂的情况下进行。本发明的另一个优点是木糖醇羧酸酯在均匀的反应混合物中获得,因此不需要额外的方法步骤,如萃取、结晶、过滤或蒸馏。本发明的优点是该方法可以在升高的温度下进行。这导致共反应物具有更好的混溶性,而所用酶的可回收性令人惊讶地高。本发明的另一个优点是所获得的木糖醇羧酸酯可以非常容易地掺入配制剂中,特别是掺入化妆品配制剂中。
因此,本发明的主题是
木糖醇羧酸酯,其包含
木糖醇的羧酸酯、1,4-脱水木糖醇的羧酸酯、1,4-脱水阿拉伯糖醇的羧酸酯和1,4-脱水核糖醇的羧酸酯,其中所述木糖醇羧酸酯中包含的木糖醇残基与所述木糖醇羧酸酯中包含的所有1,4-脱水木糖醇残基、1,4-脱水阿拉伯糖醇残基和1,4-脱水核糖醇残基的总和的重量比大于或等于96:4,优选大于97:3,更优选大于98:2,最优选大于99:1,
其特征在于:所述木糖醇的羧酸酯中的酯化伯羟基与酯化仲羟基的摩尔比为80:20至20:80,优选75:25至25:75,甚至更优选70:30至30:70,甚至更优选65:35至40:60。
本发明上下文中的术语“木糖醇羧酸酯”包括含有基于整个组合物计至少30重量%,优选至少40重量%,更优选至少50重量%,特别优选至少70重量%的木糖醇的羧酸酯的组合物。此外,还可以任选也包含来自各自制备过程的副产物,例如1,4-脱水木糖醇的羧酸酯、1,4-脱水阿拉伯糖醇的羧酸酯和1,4-脱水核糖醇的羧酸酯,以及未反应的反应物。
本发明上下文中的术语“木糖醇的羧酸酯”是指纯的木糖醇化合物。
本发明上下文中的术语“1,4-脱水木糖醇的羧酸酯”是指纯的1,4-脱水木糖醇化合物。
本发明上下文中的术语“1,4-脱水阿拉伯糖醇的羧酸酯”是指纯的1,4-脱水阿拉伯糖醇化合物。
本发明上下文中的术语“1,4-脱水核糖醇的羧酸酯”是指纯的1,4-脱水核糖醇化合物。
这种术语的使用是基于多元醇酯的习惯命名法;已知多元醇酯在其合成过程中容易脱水,因此产物是混合组合物。本领域技术人员因此将术语“脱水山梨糖醇酯”理解为表示混合物,其不仅包含1,4-脱水山梨糖醇(1,4-脱水山梨糖醇)的酯、1,5-脱水山梨糖醇(1,5-脱水山梨糖醇)的酯,而且包含异山梨醇的酯和山梨糖醇的酯,以及游离山梨糖醇,对此参见例如Food emulsifiers and their applications, 1997, 第26页。
由术语“木糖醇羧酸酯,其包含木糖醇的羧酸酯、1,4-脱水木糖醇的羧酸酯、1,4-脱水阿拉伯糖醇的羧酸酯和1,4-脱水核糖醇的羧酸酯,其中羧酸酯中包含的木糖醇残基与羧酸酯中包含的所有1,4-脱水木糖醇残基、1,4-脱水阿拉伯糖醇残基和1,4-脱水核糖醇残基的总和的重量比大于或等于96:4”清楚明确的是,在本发明的木糖醇羧酸酯中选自1,4-脱水木糖醇的羧酸酯、1,4-脱水阿拉伯糖醇的羧酸酯和1,4-脱水核糖醇的羧酸酯中的至少一种的含量必须不等于0(零),因为没有定义除数0。
除非另有说明,所有给出的百分比(%)是质量百分比。
本发明的木糖醇羧酸酯中包含的木糖醇残基与本发明的木糖醇羧酸酯中包含的所有1,4-脱水木糖醇残基、1,4-脱水阿拉伯糖醇残基和1,4-脱水核糖醇残基的总和的重量比通过高效液相色谱法(HPLC)测定。该方法包括进行受分析的木糖醇羧酸酯的碱性水解、羧酸的去除、和木糖醇及其降解产物1,4-脱水木糖醇、1,4-脱水阿拉伯糖醇和1,4-脱水核糖醇的分析。
为此,将150 mg受分析的木糖醇羧酸酯预先装载在2.00ml的1M KOH水溶液中并在搅拌下在95℃下水解30分钟。然后将反应溶液冷却至室温并用2M HCl水溶液调节至pH 2-3。结果沉淀出来的羧酸然后用二乙醚(3 × 3.00 ml)萃取,其中每次萃取后用移液管除去有机上清液。萃取后,将所述水溶液在搅拌下加热至50℃ 20分钟,由此除去剩余的醚(二乙醚的沸点:34.6℃)。
将上述得到的溶液用重蒸馏的H2O补至10.0 ml,然后1:10稀释,取一份溶液通过HPLC分析。在下列条件下进行分析:
柱: Aminex HPX-87C column 300 x 7.8 mm
洗脱液: H2O
注射体积: 10.0 µl
流速: 0.60 ml/min
柱温: 50℃
检测器: G1362A / 1260 RID (来自Agilent公司),35℃
测量时间: 30.0 min
木糖醇及其降解产物通过离子交换法分离。
为了评价,计算木糖醇的峰面积与1,4-脱水木糖醇、1,4-脱水阿拉伯糖醇和1,4-脱水核糖醇的峰面积总和的比率。
木糖醇降解产物的参比物质是可商购的,或可以替代地通过在酸性(>140℃)或碱性(>180℃)催化剂存在下加热纯木糖醇来获得。
所述木糖醇的羧酸酯中的酯化伯羟基与酯化仲羟基的摩尔比通过13C-NMR谱测定。将50-70 mg的物质溶解在1 ml已添加了弛豫促进剂(乙酰丙酮铬(III),1%)的氘代溶剂中,以制备样品。已发现DMSO-d6、CDCl3和甲醇-d4是合适的溶剂,取决于产物性能。如果样品不完全溶解在这些溶剂之一中,则必须找到溶剂混合物。将制备的样品溶液转移到5 mmNMR管中并引入NMR波谱仪中。
NMR谱研究原则上可以使用各种商购NMR仪器进行。对于目前的NMR谱研究,使用Bruker公司的Avance 400型号仪器。用以下参数记录波谱:
温度:T = 295 K,时间延迟:D1 = 2 s,扫描次数:NS = 2048,发射机频率偏移:O1P = 110 ppm,扫描宽度:SW = 300 ppm,探头:PA BBI 400 S1 H-BB-D-05-Z。
相对于作为内标的四甲基硅烷的化学位移(TMS = 0 ppm)记录共振信号。通过其它商购NMR仪器,在相同的运行参数下获得相当的结果。通过确定各自共振信号下的面积,即来自基线的信号所包围的面积来量化。在当前的NMR谱研究中,使用“TOPSPIN”软件(3.0版)进行积分。
为了准确识别酯化伯羟基和酯化仲羟基,主要记录DEPT谱。酯化伯羟基与酯化仲羟基的摩尔比通过从积分值C (酯羰基的信号组)中减去积分值P (酯化伯羟基的信号组)来确定。由此获得酯化仲羟基的信号组的积分值S,其由于与其它信号重叠而无法直接确定。
P = 酯化伯羟基[R-CH2-OC(O)R基团]的积分值
C = 酯羰基的积分值
S = C – P = 酯化仲羟基[R2-CH-OC(O)R基团]的积分值
P与S的所得比率对应于所述木糖醇的羧酸酯中的酯化伯羟基与酯化仲羟基的摩尔比。
根据本发明,优选木糖醇羧酸酯,其特征在于羧酸部分衍生自含有2至34,优选4至24,更优选6至22个碳原子的羧酸。
根据本发明,羧酸部分优选衍生自天然脂肪酸或其混合物。根据本发明,优选天然脂肪酸的混合物,特别是其中没有羧酸链长在整个链长分布中具有的比例超过95重量%,尤其是超过99重量%的混合物。
天然脂肪酸可以基于天然存在的植物油或动物油生产,并且优选具有6至30个碳原子,尤其是8至22个碳原子。天然脂肪酸通常是非支化的,大多由偶数个碳原子组成。可能的双键都具有顺式构型。实例是:己酸、辛酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、棕榈油酸、壬酸(例如可从油酸的臭氧分解或氧化裂解获得)、异硬脂酸、硬脂酸、12-羟基硬脂酸、二羟基硬脂酸、十一碳烯酸(可从蓖麻油酸的热解获得)、油酸、亚油酸、亚麻酸、岩芹酸、反油酸、花生酸、山嵛酸、芥酸、鳕油酸、亚麻酸、二十碳五烯酸、二十二碳六烯酸和花生四烯酸。
根据本发明,特别优选木糖醇羧酸酯,其特征在于:所述羧酸部分衍生自选自下组的至少两种的脂肪酸混合物:己酸、辛酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、棕榈油酸、壬酸(例如可从油酸的臭氧分解或氧化裂解获得)、异硬脂酸、硬脂酸、12-羟基硬脂酸、二羟基硬脂酸、十一碳烯酸(例如可从蓖麻油酸的热解获得)、油酸、亚油酸、亚麻酸、岩芹酸、反油酸、花生酸、山嵛酸、芥酸、鳕油酸、亚麻酸、二十碳五烯酸、二十二碳六烯酸和花生四烯酸。
根据本发明优选木糖醇羧酸酯,其特征在于:所包含的木糖醇的羧酸酯的平均酯化度为1.0至4.0,优选1.0至3.0,更优选1.1至2.7,特别优选1.3至2.6。根据本发明,替代地优选木糖醇羧酸酯,其特征在于:所包含的木糖醇的羧酸酯的平均酯化度为2.7至4.0。
本发明的木糖醇羧酸酯中包含的木糖醇的羧酸酯的平均酯化度例如通过首先经由GC或HPLC测定所涉木糖醇羧酸酯样品中的游离木糖醇及其降解产物1,4-脱水木糖醇、1,4-脱水阿拉伯糖醇和1,4-脱水核糖醇的含量来确定。必须另外确定游离和中和的脂肪酸的皂化值、酸值和含量(例如经由GC,如下文在“游离羧酸含量的测定”中所描述)。在碱性皂化后测定羧酸组成提供木糖醇羧酸酯中包含的羧酸残基的平均摩尔质量。然后可由其计算平均酯化度。
根据本发明优选木糖醇羧酸酯,其特征在于:所包含的木糖醇的羧酸酯包含木糖醇单酯、木糖醇二酯和木糖醇三酯,其中优选以基于所有包含的木糖醇的羧酸酯计10重量%至50重量%,优选15重量%至45重量%,更优选20重量%至40重量%的量包含木糖醇三酯。在此方面,进一步根据本发明优选,所包含的木糖醇的羧酸酯包含木糖醇单酯、木糖醇二酯、木糖醇三酯和木糖醇四酯。
根据本发明,优选木糖醇羧酸酯,其特征在于:其含有0.05重量%至40重量%,优选0.2重量%至25重量%,更优选0.5重量%至10重量%的游离木糖醇,其中所述重量百分比基于整个木糖醇羧酸酯计。
为了通过GC测定本发明的木糖醇羧酸酯中包含的木糖醇,将一部分样品溶解在吡啶:氯仿(4:1)中。向0.25 ml该溶液中加入0.5 ml MSTFA [N-甲基-N-(三甲基甲硅烷基)三氟乙酰胺]和0.5 ml N-三甲基甲硅烷基咪唑和吡啶(11:39)的混合物。
通过在80℃下反应(30分钟)将醇定量转化为它们的三甲基甲硅烷基醚,然后通过GC/FID进行检测。
这在配备有分流/无分流注射器、毛细管柱和火焰离子化检测器的气相色谱仪中在以下条件下进行:
注射器: 290℃,分流30ml
注射体积: 1 µl
柱: 50 m * 0.32 mm HP5 1.05 µm
载气: 氢气,恒流,2 ml/min
温度程序: 100℃至140℃以10℃/min,然后
140℃至300℃以5℃/min,然后
在300℃下调理5分钟。
检测器: FID,310℃
氢气 30 ml/min
空气 400 ml/min
补充气体 12 ml/min
分离出木糖醇并通过内标法测定其质量比例。为此,通过测量木糖醇和已知组成的内标的混合物来校准GC系统。
根据本发明,优选木糖醇羧酸酯,其特征在于:其含有小于25重量%,优选0.01重量%至20重量%,更优选0.05重量%至10重量%的至少一种游离羧酸,其中重量百分比基于整个木糖醇羧酸酯计。所述至少一种游离羧酸在此可以以质子化或中和的形式存在。
为了测定本发明的木糖醇羧酸酯中的游离羧酸的含量,首先确定酸值。由所涉脂肪酸的酸值和分子量,可以确定重量比例。
用于确定酸值的合适方法尤其是根据DGF C-V 2、DIN EN ISO 2114、Ph. Eur.2.5.1、ISO 3682和ASTM D 974的那些。
本领域技术人员已知,在其为羧酸混合物的情况下,还可以在木糖醇羧酸酯皂化之后补充进行GC分析,以由此确定所包含的羧酸混合物的平均分子量:
为此,将0.6g本发明的木糖醇羧酸酯在25ml的0.5M KOH乙醇溶液中在回流下煮沸4小时。然后用硫酸将pH调节至pH 2-3,并通过用各一个体积的石油醚萃取三次来分离出释放的羧酸。将合并的萃取物通过蒸发浓缩至约10ml。
用于确定脂肪酸分布的合适测定方法特别是根据 DGF C VI 11a、DGF C-VI 10 a和GAT- Ringtest 7/99的那些。
在自动进样器小瓶中向如上所述获得的石油醚萃取物的0.5 ml等分试样中加入0.5 ml MTBE和 1 ml三甲基苯胺氢氧化物(在甲醇中0.2 M),并通过GC分析。这在配备有分流/无分流注射器、毛细管柱和火焰离子化检测器的气相色谱仪中在以下条件下进行:
注射器: 290℃,分流30ml
注射体积: 1 µl
柱: 30 m * 0.32 mm HP1 0.25 µm
载气: 氦气,头部压力 70 kPa
温度程序: 80℃至300℃以8℃/min,然后
在300℃下调理20分钟。
检测器: FID,320℃
氢气 35 ml/min
空气 240 ml/min
补充气体 12 ml/min
所述羧酸根据其碳链长度以它们的甲酯形式分离。通过评估峰面积,可以确定这些羧酸甲酯彼此之间的质量比,并通过它们各自的分子量由此确定它们的摩尔量比,这对应于相关羧酸的摩尔量比。
此外可以确定该脂肪酸混合物的平均分子量:
其中ni = 100 g羧酸甲酯混合物中的羧酸甲酯i的摩尔量[mol];由此获得各个ni值彼此之间的比率,其对应于木糖醇羧酸酯中的相关羧酸的摩尔量比;因此,如从皂化值(见下文)获得的1 g木糖醇羧酸酯中的羧酸的总摩尔量ns[mol]可以根据所述比率分到其组分。Mi =对应于甲酯的羧酸i的分子量[g/mol]。
根据本发明,优选木糖醇羧酸酯,其特征在于:所述木糖醇的羧酸酯的整个单酯部分中含有5重量%至25重量%,优选7重量%至15重量%,更优选9重量%至13重量%的仲酯区域异构体。
根据本发明,优选木糖醇羧酸酯,其特征在于:所述木糖醇的羧酸酯的整个单酯部分中和所述木糖醇的羧酸酯的整个二酯部分中各自包含至少两种区域异构体。
根据本发明优选木糖醇羧酸酯,其特征在于:所述木糖醇的羧酸酯的整个二酯部分中含有25重量%至45重量%,优选28重量%至39重量%,更优选30重量%至37重量%的区域异构体,其中至少一种仲羟基被酯化。
本发明的木糖醇的羧酸酯的整个单酯部分中的仲酯区域异构体含量的测定,以及基于所有包含的木糖醇的羧酸酯的总和计的三酯物类含量的测定,以及其中至少一个仲羟基被酯化的整个二酯部分中的区域异构体含量的测定可通过气相色谱法(任选与质谱联用(GC-FID和GC-MS))进行:
首先将10 mg相应木糖醇羧酸酯样品溶解在1.5 ml三氯甲烷中,然后加入0.15 mlN-甲基-N-(三甲基甲硅烷基)三氟乙酰胺(MSTFA)。衍生化在80℃下进行30分钟。由此获得的澄清溶液的样品通过GC-FID和GC-MS分析。所述分析方法的参数如下:
气相色谱:Agilent MSD 7890
柱:Agilent HP-5 (50 m,0.32 mm,0.5 µm),
流速:用氢气恒定2 ml/min (GC-MS:氦气)
80℃调温,8℃/min;300℃,30分钟,注射器1 µl,分流 1:20,检测器310℃
检测器:FID,310℃/GC-MS scan 35-650 d。
在GC-FID分析中,样品中包含的酯根据它们的总链长进行分离。通过GC-FID峰的各自面积百分比来确定各个酯物类彼此之间的比率。所述峰通过GC-MS识别/分配给各个酯物类,任选还通过单独制备和分离的标准物(例如对于仅在伯羟基上酯化的单酯和二酯)的保留时间比较。
该方法同样可用于获取游离质子化和游离中和的羧酸的含量,因为它们同样是衍生化的。
本发明的另一主题是用于酶促制备木糖醇羧酸酯,优选本发明的木糖醇羧酸酯的方法,其包括以下方法步骤:
A) 提供木糖醇和至少一种酰基供体,优选脂肪酸酰基供体,特别选自脂肪酸酯和脂肪酸,特别优选脂肪酸,
B) 在75℃至110℃,优选77℃至100℃,甚至更优选80℃至95℃的温度下,在脂肪酶存在下使木糖醇与所述至少一种酰基供体反应,得到木糖醇羧酸酯,并任选地
C) 纯化所述木糖醇羧酸酯。
根据本发明,可以根据本发明使用所有酰基供体。这些是例如羧酸酯或羧酸本身,以及它们的混合物。
根据本发明优选用作酰基供体的羧酸酯选自基于具有最多6个碳原子,特别优选具有最多3个碳原子的烷醇和多元醇的酯,非常特别优选甘油酯。
根据本发明特别优选用作酰基供体的羧酸酯选自甘油三酯,尤其是天然脂肪和油,特别优选选自包含如下或由如下组成的组:椰子脂肪、棕榈仁油、橄榄油、棕榈油、摩洛哥坚果油、蓖麻油, 亚麻籽油、巴巴苏油、菜籽油、藻油、芝麻油、大豆油、鳄梨油、荷荷巴油、红花油、杏仁油、棉籽油、乳木果油、葵花籽油、古布阿苏果油和具有高比例的多不饱和脂肪酸(PUFA)的油。同样可以优选使用脱水山梨糖醇酯、甘油单酯和甘油二酯,特别是含有下文所述酰基的那些。
根据本发明,特别优选酰基供体选自脂肪酸酰基供体,其特别提供选自天然脂肪酸的酰基的酰基。在这方面,优选的脂肪酸是上述与本发明的木糖醇羧酸酯有关的那些,优选形成羧酸部分的脂肪酸,其具有相同的优选程度。
根据本发明,优选使用羧酸,尤其是脂肪酸作为酰基供体,其中上述具体提及的与本发明的木糖醇羧酸酯相关的脂肪酸优选以相同的优选程度使用。
替代地,根据本发明优选使用脂肪酸与甘油脂肪酸酯的混合物作为酰基供体,其中上述具体提及的与本发明的木糖醇羧酸酯相关的脂肪酸在脂肪酸和甘油脂肪酸酯组分中都以相同的优选程度优选使用。
所使用的脂肪酸与甘油脂肪酸酯的混合物优选具有的脂肪酸与甘油脂肪酸酯的重量比为80:20至99:1,优选90:10至99:1,更优选95:5至99:1。
根据本发明优选的方法的特征在于:所述木糖醇和所述至少一种酰基供体占基于方法步骤B)开始时整个反应混合物计至少80重量%,优选至少90重量%,更优选至少95重量%。
由于在此方面整个反应混合物主要由反应物,即木糖醇和酰基供体组成,在整个反应混合物中只能包含非常少的溶剂(如果有的话)。由于如上所述而显而易见,所述酰基供体在本发明方法中不被术语“溶剂”所涵盖。
可能的溶剂是例如酮,例如甲基异丁基酮或环己酮,位阻仲醇,如2-丁基-1-辛醇、甲基环己醇、1-甲氧基-2-丙醇、丁烷-2,3-二醇、2-辛醇、双丙酮醇、2-甲基-2-丁醇,和醚,如 1,4-二噁烷、四氢呋喃和Varonic APM。
基于整个反应混合物计,总共最多以小于20重量%,优选小于10重量%,尤其是小于5重量%包含溶剂。表述“最多以小于X重量%包含”可等同于“具有小于X重量%的含量”。
特别优选在不存在溶剂的情况下进行本发明的方法。
根据本发明优选的方法的特征在于:所提供的木糖醇与在所提供的所有酰基供体中包含的酰基的摩尔比为1.00:0.30至1.00:5.00,优选1.00:0.70至1.00:3.00,特别优选1.00:1.00至1.00:2.25,替代地特别优选1.00:2.3至1.00:4.50。
根据本发明优选的方法的特征在于:方法步骤A)包括
将木糖醇和所述至少一种酰基供体共混至少十分钟,优选30分钟,甚至更优选60分钟,
其中所述共混优选在80℃至120℃,优选90℃至120℃,甚至更优选95℃至120℃,甚至更优选100℃至120℃的温度范围内进行。
根据本发明在方法步骤B)中优选使用的脂肪酶以固定在固体载体上的形式存在。
在方法步骤B)中根据本发明优选使用的脂肪酶是选自包括如下的脂肪酶:来自绵毛嗜热丝菌(Thermomyces lanuginosus)的脂肪酶(登录号O59952)、来自南极假丝酵母(Candida antarctica)的脂肪酶A和B(登录号P41365)和来自米赫毛霉(Mucor miehei )的脂肪酶(登录号P19515)、来自腐质霉属(Humicola sp.)的脂肪酶(登录号 O59952)、来自爪哇根毛霉(Rhizomucor javanicus)的脂肪酶(登录号 S32492)、来自米根霉(Rhizopus oryzae)的脂肪酶(登录号 P61872)、来自皱褶假丝酵母(Candida rugosa)的脂肪酶(登录号 P20261、P32946、P32947、P3294和P32949)、来自雪白根霉(Rhizopus niveus)的脂肪酶(登录号P61871)、来自卡门培尔青霉(Penicillium camemberti)的脂肪酶(登录号P25234)、来自黑曲霉(Aspergillus niger)的脂肪酶(ABG73613、ABG73614和ABG37906)和来自圆弧青霉(Penicillium cyclopium)的脂肪酶(登录号 P61869),其中特别优选来自南极假丝酵母(Candida antarctica)的脂肪酶A和B(登录号P41365),以及各自它们在氨基酸水平上至少60%,优选至少80%,优选至少90%,尤其是优选至少95%、98%或99%的同源物。
本发明上下文中列出的登录号对应于日期为2017.01.01的NCBI ProteinBank数据库条目;在本上下文中条目的版本号通常由“.数字”,例如“.1”标识。
与参比序列相比,在氨基酸水平上同源的酶优选具有至少50%,尤其是至少90%的酶活性,其以在本发明的上下文中所定义的月桂酸丙酯单元(PLU)表示。
为了确定以PLU(月桂酸丙酯单元)表示的酶活性,将1-丙醇和月桂酸以等摩尔比在60℃下均匀混合。通过加入酶开始反应并测量反应时间。每隔一段时间从反应混合物中取出样品,并通过用氢氧化钾溶液滴定来确定转化的月桂酸的含量。以PLU表示的酶活性得自1 g相关酶在60℃下每分钟合成1 µmol月桂酸丙酯的速度;对此也参见US20070087418,特别是[0185]。
商业实例和同样优选用于根据本发明的方法的脂肪酶是商品Lipozyme TL IM、Novozym 435、Lipozyme IM 20、Lipase SP382、Lipase SP525、Lipase SP523(所有商品来自丹麦Bagsvaerd的Novozymes A/S公司)、Chirazyme L2、Chirazyme L5、Chirazyme L8、Chirazyme L9 (所有商品均来自德国曼海姆Roche Molecular Biochemicals公司),Purolite公司的CALB Immo Plus TM以及Lipase M “Amano”、LipaseF-AP 15 “Amano”、Lipase AY“Amano”、Lipase N“Amano”、LipaseR“Amano”、Lipase A“Amano”、Lipase D“Amano”、Lipase G“Amano”(所有商品均来自日本Amano公司)。
“氨基酸水平上的同源性”在本发明中应理解为是指“氨基酸同一性”,其可以借助已知方法确定。通常,使用特殊的计算机程序,其中算法考虑特定要求。确定同一性的优选方法首先在要比较的序列之间产生最大的相一致性。用于确定同一性的计算机程序包括但不限于GCG程序包,包括
- GAP (Deveroy, J.等人,Nucleic Acid Research 12 (1984), 第387页,Genetics Computer Group University of Wisconsin, Medicine (WI),和
- BLASTP、BLASTN和FASTA (Altschul, S.等人,Journal of Molecular Biology215 (1990),第403-410页。BLAST程序可从国家生物技术信息中心(NCBI)和其它来源(BLAST 手册,Altschul S.等人,NCBI NLM NIH Bethesda ND 22894;Altschul S.等人,如上)获得。
本领域技术人员知道,各种计算机程序可用于计算两个核苷酸序列或氨基酸序列之间的相似性或同一性。例如,两个氨基酸序列之间的同一性百分比可以通过例如由Needleman和Wunsch开发的算法(J. Mol. Biol. (48): 444-453 (1970))确定,该算法已整合到GCG软件包的GAP程序中(可从 http://www.gcg.com 获得),其中使用Blossom 62矩阵或PAM250矩阵,间隙权重为16、14、12、10、8、6或4以及长度权重为1、2、3、4、5或6。本领域技术人员认识到,使用不同参数将导致略微不同的结果,但两个氨基酸序列之间的同一性百分比总体上不会有显著差异。通常使用Blossom 62矩阵,其中使用默认设置(间隙权重:12,长度权重:1)。
在本发明的上下文中,根据上述算法60%的同一性意味着60%的同源性。这同样适用于更高的同一性。
在方法步骤B)中,根据本发明优选地,每克待转化的木糖醇使用500 PLU至2000PLU,优选200 PLU至1500 PLU,更优选25 PLU至1250 PLU的脂肪酶。
根据本发明的方法步骤B)优选在小于1bar,优选小于0.5bar,更优选小于0.1bar的压力下进行。
根据本发明,方法步骤B)替代地优选在鼓泡柱式反应器中进行,其中至少一种惰性气体通过反应混合物;该惰性气体优选地选自包含如下,优选由如下组成的组:氮气和氩气。在此方面,根据本发明优选,所述气体流量为1至60kg/h,优选5至25kg/h,甚至更优选10至14kg/h。
根据本发明,方法步骤B)的特征优选在于:所述方法步骤B)在添加脂肪酶后最迟180小时,优选120小时,更优选100小时后结束。
根据本发明优选的方法的特征在于:在方法步骤B)中去除形成的副产物,例如当使用的酰基供体为酸时的水和当使用的酰基供体为酯时的相应醇。这例如可以通过蒸馏。
本发明的方法的方法步骤C)包括纯化木糖醇羧酸酯。为此,可以采用所有允许以较高浓度获得木糖醇羧酸酯的方法。
根据本发明优选,本发明的方法包括在方法步骤C)中分离出本发明方法中使用的脂肪酶。
当脂肪酶以固定在载体上的形式存在时,根据本发明优选通过过滤器,尤其是袋式过滤器过滤而分离出脂肪酶,所述过滤器具有的细度为0.1μ至1250μ,优选0.5μ至100μ。
根据本发明优选,本发明的方法的特征在于:在其中不使用分子筛。
根据本发明优选,本发明的方法的特征在于:底物以没有固定在固体载体如二氧化硅上的形式使用。
本发明的另一主题是通过本发明的方法可得的木糖醇羧酸酯。
本发明的另一主题是本发明的木糖醇羧酸酯和/或通过本发明的方法可得的木糖醇羧酸酯的用途,其作为粘度调节剂、护理活性成分、泡沫促进剂或增溶剂、抗微生物剂、抗静电剂、粘合剂、腐蚀抑制剂、分散剂、乳化剂、成膜剂、保湿剂、遮光剂、口腔护理剂、防腐剂、护肤剂、亲水性润肤剂、泡沫稳定剂和非离子表面活性剂,优选作为粘度调节剂、乳化剂、抗微生物剂和亲水性润肤剂,特别优选作为粘度调节剂,尤其是作为增稠剂,尤其是在清洁或护理配制剂中。
下述实施例中举例描述了本发明,并不旨在将本发明限制于实施例中提及的实施方案,本发明的应用范围由整个说明书和权利要求书得出。
实施例:
如下文所述制备各种木糖醇羧酸酯。
确定色值的方法
在室温或90℃下在11 mm圆形比色皿中在Lico 690光谱色度计中测量等分试样(约10 g,使得比色皿充分填充),并记录每种情况下给出的色值。
实施例1:木糖醇与2.00当量辛酸的酶促酯化(本发明)
在搅拌和通导N2下将木糖醇(60.0 g,0.394 mol,1.00当量)和辛酸(酸值 = 389mg KOH/g,> 98%,113.70 g,0.788 mol,2.00当量)的混合物加热至80℃,1小时后加入固定化的南极假丝酵母脂肪酶B酶(5.21 g;Purolite D5619,对应于45110 PLU)。将混合物在80℃和15 mbar下搅拌24小时,在此期间连续蒸馏掉形成的水。然后将混合物在80℃下通过带有黑色带状过滤器的布氏漏斗过滤以去除酶。得到的产物是在熔体中均匀、无色的并且具有1.2mg KOH/g的酸值。基于所有包含的木糖醇的羧酸酯的总和计,三酯含量为27重量%,其通过GC-FID峰的面积%值确定。
实施例2:木糖醇与2.00当量辛酸/癸酸的酶促酯化(本发明)
在搅拌和通导N2下将木糖醇(70.8 g,0.465 mol,1.00当量)和辛酸/癸酸混合物(酸值 = 362 mg KOH/g,辛酸与癸酸的混合比60:40,146.0 g,0.930 mol,2.00当量)的混合物加热至90℃ 1小时,在冷却至85℃后加入固定化的南极假丝酵母脂肪酶B酶(6.50 g;Purolite D5619,对应于56280 PLU)。将混合物在85℃和50 mbar下搅拌24小时,在此期间连续蒸馏掉形成的水。然后将混合物在80℃下通过带有黑色带状过滤器的布氏漏斗过滤以去除酶。得到的产物是在熔体中均匀、无色的并且具有2.7 mg KOH/g的酸值。基于所有包含的木糖醇的羧酸酯的总和计,三酯含量为26重量%,其通过GC-FID峰的面积%值确定。
实施例3:木糖醇与1.80当量辛酸/癸酸的酶促酯化(本发明)
在搅拌和通导N2下将木糖醇(75.7 g,0.497 mol,1.00当量)和辛酸/癸酸混合物(酸值 = 362 mg KOH/g,辛酸与癸酸的混合比60:40,140.5 g,0.895 mol,1.80当量)的混合物加热至90℃ 1小时,在冷却至85℃后加入固定化的南极假丝酵母脂肪酶B酶(6.48 g;Purolite D5619,对应于56106 PLU)。将混合物在85℃和50 mbar下搅拌24小时,在此期间连续蒸馏掉形成的水。然后将混合物在80℃下通过带有黑色带状过滤器的布氏漏斗过滤以去除酶。得到的产物是在熔体中均匀、无色的并且具有1.5 mg KOH/g的酸值。基于所有包含的木糖醇的羧酸酯的总和计,三酯含量为25重量%,其通过GC-FID峰的面积%值确定。
实施例4:木糖醇与2.00当量硬脂酸的酶促酯化(本发明)
在搅拌和通导N2下将木糖醇(40.00 g,0.263 mol,1.00当量)和硬脂酸(酸值 =198 mg KOH/g,> 92%,148.18 g,0.526 mol,2.00当量)的混合物加热至90℃,1小时后加入固定化的南极假丝酵母脂肪酶B酶(5.65 g;Purolite D5619,对应于48919 PLU)。将混合物在90℃和15 mbar下搅拌24小时,在此期间连续蒸馏掉形成的水。然后将混合物在80℃下通过带有黑色带状过滤器的布氏漏斗过滤以去除酶。得到的产物是在熔体中均匀、无色、浅黄的并且具有1.3 mg KOH/g的酸值。基于所有包含的木糖醇的羧酸酯的总和计,三酯含量为35重量%,其通过GC-FID峰的面积%值确定。
实施例5:木糖醇与2.00当量油酸的酶促酯化(本发明)
在搅拌和通导N2下将木糖醇(40.00 g,0.263 mol,1.00当量)和油酸(酸值 = 200mg KOH/g,碘值= 92.3 g I2/100 g,147.5 g,0.526 mol,2.00当量)的混合物加热至90℃,1小时后加入固定化的南极假丝酵母脂肪酶B酶(5.65 g;Purolite D5619,对应于48919PLU)。将混合物在80℃和15 mbar下搅拌24小时,在此期间连续蒸馏掉形成的水。然后将混合物在80℃下通过带有黑色带状过滤器的布氏漏斗过滤以去除酶。得到的产物是在熔体中均匀、透明、淡黄色的并且具有1.1 mg KOH/g的酸值。基于所有包含的木糖醇的羧酸酯的总和计,三酯含量为34重量%,其通过GC-FID峰的面积%值确定。
实施例6:木糖醇癸酸/辛酸酯(非本发明)
来自 GiOrbis Laboratories的商品GiO™ -103,用作样品。
实施例7:根据KR101939851的木糖醇与2.00当量辛酸的酯化(非本发明)
例如在KR101939851或EP2902009A1中描述了在高温下在酸性催化剂存在下木糖醇与脂肪酸的酯化:
在加入对甲苯磺酸(0.29 g,基于辛酸计0.2%)后,在搅拌和通导N2下将木糖醇(76.1 g,0.500 mol,1.00当量)和辛酸(酸值 = 389 mg KOH/g,> 98%,144.2 g,1.00mol,2.00当量)的混合物加热至200℃。然后将混合物在该温度下搅拌8小时,在此期间连续蒸馏掉形成的水,直到达到0.7 mg KOH/g的酸值。所得产物为黄色至棕色,加德纳色值为6.4。
实施例8:木糖醇与2.00当量辛酸在低温下的酶促酯化(非本发明)
如在Basri等人(Carbohydr. Res. 2011, 346, 472-479)中所述,在搅拌和通导N2下将木糖醇(75.2 g,0.494 mol,1.00当量)、辛酸(酸值 = 389 mg KOH/g,> 98%,142.6g,0.989 mol,2.00当量)的混合物在60℃下酶促反应29小时。得到的产物是在熔体中非均匀的(即其形成两个相),具有约360 mg KOH/g的酸值。
表1比较了本发明实施例与非本发明实施例所确定的参数。
表1;本发明实施例标有*
实施例 | 木糖醇:降解产物比率 | NMR (伯:仲) | 经由GC的游离木糖醇[%] | 酸值 | 加德纳色值 |
1 * | > 99:1 | 51:49 | 1.9 | 1.2 | 0 |
2 * | > 99:1 | 53:47 | 1.6 | 2.7 | 0 |
3 * | > 99:1 | 54:46 | 4.4 | 1.5 | 0 |
4 * | > 99:1 | 57:43 | 0.9 | 1.3 | 0 |
5 * | > 99:1 | 55:45 | 1.3 | 1.1 | 1 |
6 | 95:5 | 67:33 | 10 | 3 | 7 |
7 | 1:99 | 方法不可用 | < 0,05 | 0.7 | 6.4 |
8 | > 99:1 | 81:19 | 0.3 | (360) | 0 |
实施例9:化妆品配制剂中的增稠性能
评价了本发明实施例1、2和3与非本发明增稠剂相比的增稠效果。为此,制备由9%SLES、3%椰油酰胺丙基甜菜碱和0.7% NaCl水溶液组成的化妆品配制剂。用柠檬酸将该配制剂的pH值调节至5.2。通过在60℃下搅拌30分钟,在每种情况下将1.1%的上述实施例物质掺入该配制剂中,并使用Brookfield粘度计(心轴62,30 rpm转数)在22℃下测量粘度。粘度测量结果示于表2中。
表 2:含有1.1%增稠剂的实施例配制剂的粘度
实施例 | 粘度 [mPa*s] | |
1 | 本发明 | 7733 |
2 | 本发明 | 7200 |
3 | 本发明 | 7776 |
6 | 非本发明 | 5995 |
7 | 非本发明 | 1313 |
8 | 非本发明 | 3968 |
表2的结果表明,在本发明实施例1、2和3中获得的配制剂比在非本发明实施例中具有更高的粘度。
配制剂实施例
配方1a、1b和1c:含有铝盐的止汗/除臭配制剂
配方 | 1a | 1b | 1c |
实施例4的组合物 | 3.2% | 3.2% | 3.2% |
C18-C22羟烷基羟丙基瓜尔胶(ESAFLOR HM 22, Lamberti S.p.A.) | 0.2% | ||
羟丙基瓜尔胶(ESAFLOR HDR,Lamberti S.p.A.) | 0.2% | 0.2% | |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 5.4% | 5.4% | 5.4% |
水 | 至100% | 至100% | 至100% |
氯化羟铝(50%水溶液;Locron LIC,Clariant AG) | 20.0% | 20.0% | 20.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | |
十一碳烯酰胺基丙基三甲基铵甲基硫酸盐;水;丙二醇(dermosoft® UTM,Evonik Dr.Straetmans GmbH) | 1.0% |
配方2a、2b和2c:不含止汗活性成分的无铝除臭配制剂
配方 | 2a | 2b | 2c |
实施例4的组合物 | 3.2% | 3.2% | 3.2% |
羟丙基瓜尔胶(ESAFLOR HDR,Lamberti S.p.A.) | 0.15% | ||
C18-C22羟烷基羟丙基瓜尔胶(ESAFLOR HM 22, Lamberti S.p.A.) | 0.15% | 0.15% | |
聚甘油-3辛酸酯(TEGO® Cosmo P 813,Evonik Operations GmbH) | 0.5% | 0.5% | 0.5% |
蓖麻酸锌(TEGODEO® PY 88 G,Evonik Operations GmbH) | 1.0% | 1.0% | 1.0% |
辛酸/癸酸甘油三酯(TEGOSOFT® CT,Evonik Operations GmbH) | 5.65% | 5.65% | 5.65% |
水 | 至100% | 至100% | 至100% |
甘油 | 3.0% | 3.0% | 3.0% |
苯甲醇、苯甲酸、山梨酸(Rokonsal BSB-N,Ashland Specialty Ingredients) | 1.0% | 1.0% | 1.0% |
柠檬酸(50%水溶液) | 适量 | 适量 | 适量 |
戊二醇(dermosoft® Pentiol eco,Evonik Dr. Straetmans GmbH) | 4.0 |
配方3a、3b和3c:含钾明矾的O/W除臭剂乳液
配方 | 3a | 3b | 3c |
实施例4的组合物 | 4.8% | 4.8% | 4.8% |
C18-C22羟烷基羟丙基瓜尔胶(ESAFLOR HM 22, Lamberti S.p.A.) | 0.25% | ||
羟丙基瓜尔胶(ESAFLOR HDR,Lamberti S.p.A.) | 0.25% | 0.25% | |
棕榈酸异丙酯(TEGOSOFT® P,Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
水 | 至100% | 至100% | 至100% |
甘油 | 3.0% | 3.0% | 3.0% |
钾明矾 | 5.0% | 5.0% | 5.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | |
戊二醇(dermosoft® Pentiol eco,Evonik Dr. Straetmans GmbH) | 3.5% |
配方4a和4b:止汗/除臭露
配方 | 4a | 4b |
实施例4的组合物 | 3.0% | 3.0% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 3.0% | 3.0% |
PPG-14丁基醚(TEGOSOFT® PBE,Evonik Operations GmbH) | 3.0% | 3.0% |
聚甘油-3辛酸酯(TEGO® Cosmo P813,Evonik Operations GmbH) | 0.5% | 0.5% |
去矿物质水 | 至100% | 至100% |
羟乙基纤维素(Natrosol 250 HHR,Ashland Specialty Chemicals) | 1.0% | 1.0% |
氯化羟铝(50%) (Reach 501L,Reheis) | 15.0% | 15.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 3.0% |
1,2-己二醇(dermosoft® Hexiol,Evonik Dr. Straetmans GmbH) | 2.8% |
配方5a、5b和5c:止汗/除臭霜
配方 | 5a | 5b | 5c |
实施例4的组合物 | 3.0% | 2.5% | 2.5% |
鲸蜡硬脂醇硫酸酯(Lanette E,BASF SE) | 0.5% | 0.5% | |
硬脂酸甘油酯 | 1.0% | 1.0% | 1.0% |
硬脂醇 | 1.0% | 1.0% | 1.0% |
PPG-15硬脂醚 | 5.0% | 5.0% | 5.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
<i>鳄梨(鳄梨)油</i> | 2.0% | 2.0% | 2.0% |
聚甘油-3辛酸酯(TEGO® Cosmo P813,Evonik Operations GmbH) | 0.5% | 0.5% | 0.5% |
蓖麻酸锌(TEGODEO® PY88 G,Evonik Operations GmbH) | 1.0% | 1.0% | 1.0% |
去矿物质水 | 至100% | 至100% | 至100% |
羟乙基纤维素(Natrosol 250 HHR (Ashland Specialty Chemicals) | 1.0% | 1.0% | 1.0% |
氯化羟铝(50%水溶液;Locron LIC,Clariant AG) | 15.0% | 15.0% | 15.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | |
甲基丙二醇;辛二醇;苯丙醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 3.5% |
配方6a和6b:防晒喷雾SPF 30
配方 | 6a | 6b |
实施例4的组合物 | 4.0% | 4.0% |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 3.2% | 3.2% |
棕榈酸异丙酯(TEGOSOFT® P,Evonik Operations GmbH) | 2.0% | 2.0% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 3.0% | 3.0% |
丁基甲氧基二苯甲酰基甲烷 | 2.0% | 2.0% |
EHC | 2.0% | 2.0% |
水杨酸乙基己酯 | 4.0% | 4.0% |
奥克立林 | 4.0% | 4.0% |
甘油 | 3.0% | 3.0% |
水 | 至100% | 至100% |
卡波姆混悬液1(丙烯酸酯/丙烯酸C10-30烷基酯交联聚合物,TEGO® Carbomer 341ER,EvonikOperations GmbH,辛酸苯氧基乙酯中20%) | 1.0% | 1.0% |
三(羟甲基)氨基甲烷(30%水溶液) | 0.6% | 0.6% |
紫外线滤光液(20%苯基苯并咪唑磺酸,8.8% 三(羟甲基)氨基甲烷,去矿物质水至100%) | 10.0% | 10.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | |
甲基丙二醇;辛二醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 4.0 |
配方7a、7b和7c:防晒喷雾
配方 | 7a | 7b | 7c |
实施例4的组合物 | 3.0% | 2.5% | 2.5% |
柠檬酸硬脂酸甘油酯(AXOL® C 62,Evonik Operations GmbH) | 0.5% | 0.5% | |
硬脂酸甘油酯 | 0.5% | 0.5% | 0.5% |
硬脂醇 | 0.5% | 0.5% | 0.5% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 3.0% | 3.0% | 3.0% |
丁基甲氧基二苯甲酰基甲烷 | 2.0% | 2.0% | 2.0% |
甲氧基肉桂酸乙基己酯 | 2.0% | 2.0% | 2.0% |
水杨酸乙基己酯 | 4.0% | 4.0% | 4.0% |
奥克立林 | 4.0% | 4.0% | 4.0% |
棕榈酸异丙酯 | 2.0% | 2.0% | 2.0% |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 3.2% | 3.2% | 3.2% |
甘油 | 3.0% | 3.0% | 3.0% |
去矿物质水 | 至100% | 至100% | 至100% |
卡波姆混悬液(丙烯酸酯/丙烯酸C10-30烷基酯交联聚合物,TEGO® Carbomer 341ER,辛酸苯氧基乙酯中20%) | 1.0% | 1.0% | 1.0% |
氨丁三醇 (30%) | 0.9% | 0.9% | 0.9% |
紫外线滤光液(20%苯基苯并咪唑磺酸,8.8% 三(羟甲基)氨基甲烷,去矿物质水至100%) | 10.0% | 10.0% | 10.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | |
甲基丙二醇;辛二醇;苯丙醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 3.0% |
配方8a、8b和8c:防晒露,SPF 30
配方 | 8a | 8b | 8c |
实施例4的组合物 | 3.00% | 2.00% | 2.00% |
鲸蜡硬脂基葡糖苷(TEGO® Care CG 90,Evonik Operations GmbH) | 0.50% | 0.50% | |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 8.00% | 8.00% | 8.00% |
二乙基氨基羟基苯甲酰基苯甲酸己酯(Uvinul A Plus,BASF SE) | 6.00% | 6.00% | 6.00% |
甲氧基肉桂酸乙基己酯 | 8.00% | 8.00% | 8.00% |
硬脂醇 | 1.00% | 1.00% | 1.00% |
硬脂酸甘油酯 | 1.00% | 1.00% | 1.00% |
生育酚乙酸酯 | 0.50% | 0.50% | 0.50% |
甘油 | 2.00% | 2.00% | 2.00% |
去矿物质水 | 至100% | 至100% | 至100% |
氨丁三醇 | 0.90% | 0.90% | 0.90% |
苯基苯并咪唑磺酸 | 2.00% | 2.00% | 2.00% |
丙烯酸酯/丙烯酸C10-30烷基酯交联聚合物(TEGO® Carbomer 341 ER,EvonikOperations GmbH) | 0.30% | 0.30% | 0.30% |
氢氧化钠(10%水溶液) | 适量 | 适量 | 适量 |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
辛二醇;甘油;辛酸甘油酯;苯丙醇;水(dermosoft® LP MB;Evonik Dr. StraetmansGmbH) | 1.0 |
配方9a、9b和9c:防晒露SPF 30,高UVA防护
配方 | 9a | 9b | 9c |
实施例4的组合物 | 3.00% | 2.50% | 2.50% |
鲸蜡硬脂醇硫酸酯钠(Lanette E,BASF SE) | 0.50% | 0.50% | |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 7.30% | 7.30% | 7.30% |
丁基甲氧基二苯甲酰基甲烷 | 5.00% | 5.00% | 5.00% |
二乙基己基丁酰胺基三嗪酮(UVAsorb HEB,3V Sigma) | 1.00% | 1.00% | 1.00% |
水杨酸乙基己酯 | 1.50% | 1.50% | 1.50% |
奥克立林 | 3.50% | 3.50% | 3.50% |
二氧化钛;碳酸二乙基己酯;聚甘油-6聚羟基硬脂酸酯(TEGO® Sun TDEC 45,EvonikOperations GmbH) | 2.20% | 2.20% | 2.20% |
硬脂醇 | 1.00% | 1.00% | 1.00% |
尼龙-10/10 (TEGOLON® ECO 10-10,Evonik Operations GmbH) | 0.50% | 0.50% | 0.50% |
硬脂酸甘油酯 | 1.00% | 1.00% | 1.00% |
生育酚乙酸酯 | 0.50% | 0.50% | 0.50% |
甘油 | 2.00% | 2.00% | 2.00% |
去矿物质水 | 至100% | 至100% | 至100% |
柠檬酸(50%水溶液) | 0.10% | 0.10% | 0.10% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 20.00% | 20.00% | 20.00% |
丙烯酸酯/丙烯酸C10-30烷基酯交联聚合物(TEGO® Carbomer 341 ER,Evonik OperationsGmbH) | 0.30% | 0.30% | 0.30% |
氢氧化钠(10%水溶液) | 0.90% | 0.90% | 0.90% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
柠檬酸三乙酯;辛二醇;苯甲酸(Verstatil® TBO;Evonik Dr. Straetmans GmbH) | 1.0% |
配方10a、10b和10c:防晒露,SPF 30
配方 | 10a | 10b | 10c |
实施例4的组合物 | 3.00% | 2.00% | 2.00% |
甲基葡萄糖倍半硬脂酸酯(TEGO® Care PS,Evonik Operations GmbH) | 1.00% | 1.00% | |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 1.50% | 1.50% | 1.50% |
奥克立林 | 10.00% | 10.00% | 10.00% |
丁基甲氧基二苯甲酰基甲烷 | 3.50% | 3.50% | 3.50% |
二氧化钛;碳酸二乙基己酯;聚甘油-6聚羟基硬脂酸酯(TEGO® Sun TDEC 45,EvonikOperations GmbH) | 14.50% | 14.50% | 14.50% |
硬脂醇 | 0.20% | 0.20% | 0.20% |
硬脂酸甘油酯 | 0.20% | 0.20% | 0.20% |
生育酚乙酸酯 | 0.50% | 0.50% | 0.50% |
甘油 | 2.00% | 2.00% | 2.00% |
去矿物质水 | 至100% | 至100% | 至100% |
丙烯酸酯/丙烯酸C10-30烷基酯交联聚合物(TEGO® Carbomer 341 ER,EvonikOperations GmbH) | 0.20% | 0.20% | 0.20% |
氢氧化钠(10%水溶液) | 0.60% | 0.60% | 0.60% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
甲基丙二醇;辛二醇;苯丙醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 3.0% |
配方11a、11b和11c:防晒露SPF 50,高UVA防护
配方 | 11a | 11b | 11c |
实施例4的组合物 | 3.00% | 2.50% | 2.50% |
聚甘油-3-甲基葡萄糖二硬脂酸酯(TEGO® Care 450,Evonik Operations GmbH) | 0.50% | 0.50% | |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 2.00% | 2.00% | 2.00% |
尼龙-10/10 (TEGOLON® ECO 10-10,Evonik Operations GmbH) | 0.50% | 0.50% | 0.50% |
丁基甲氧基二苯甲酰基甲烷 | 5.00% | 5.00% | 5.00% |
二乙基己基丁酰胺基三嗪酮(UVAsorb HEB,3V Sigma) | 1.00% | 1.00% | 1.00% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 3.00% | 3.00% | 3.00% |
水杨酸乙基己酯 | 1.00% | 1.00% | 1.00% |
奥克立林 | 8.00% | 8.00% | 8.00% |
硬脂醇 | 0.45% | 0.45% | 0.45% |
硬脂酸甘油酯 | 0.45% | 0.45% | 0.45% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.30% | 0.30% | 0.30% |
生育酚乙酸酯 | 0.50% | 0.50% | 0.50% |
羟乙基纤维素(Natrosol 250 HHR(Ashland Specialty Chemicals) | 0.50% | 0.50% | 0.50% |
去矿物质水 | 至100% | 至100% | 至100% |
氢氧化钠(10%水溶液,pH值调整至7.5) | 适量 | 适量 | 适量 |
苯基二苯并咪唑四磺酸酯二钠(Neoheliopan AP,Symrise) | 5.00% | 5.00% | 5.00% |
亚甲基双苯并三唑基四甲基丁基苯酚(Tinosorb M,BASF SE) | 8.00% | 8.00% | 8.00% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
甲基丙二醇;辛二醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 3.8% |
配方12a、12b和12c:防晒露,SPF 50
配方 | 12a | 12b | 12c |
实施例4的组合物 | 3.50% | 3.00% | 3.00% |
柠檬酸硬脂酸甘油酯(AXOL® C 62,Evonik Operations GmbH) | 1.00% | 1.00% | |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 2.50% | 2.50% | 2.50% |
二乙基氨基羟基苯甲酰基苯甲酸己酯 | 10.00% | 10.00% | 10.00% |
甲氧基肉桂酸乙基己酯 | 10.00% | 10.00% | 10.00% |
硬脂醇 | 1.00% | 1.00% | 1.00% |
硬脂酸甘油酯 | 1.00% | 1.00% | 1.00% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.50% | 0.50% | 0.50% |
生育酚乙酸酯 | 0.50% | 0.50% | 0.50% |
甘油 | 2.00% | 2.00% | 2.00% |
去矿物质水 | 至100% | 至100% | 至100% |
苯基苯并咪唑磺酸 | 4.00% | 4.00% | 4.00% |
氨丁三醇 | 1.80% | 1.80% | 1.80% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
柠檬酸三乙酯;辛酸甘油酯;苯甲酸(Verstatil® TBG MB,Evonik Dr. Straetmans GmbH) | 1.2% |
配方13a、13b和13c:防晒露SPF 50+
配方 | 13a | 13b | 13c |
实施例4的组合物 | 3.00% | 2.5% | 2.5% |
十六烷基磷酸钾 | 1.0% | 1.0% | |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 3.00% | 3.00% | 3.00% |
丁基甲氧基二苯甲酰基甲烷 | 5.00% | 5.00% | 5.00% |
奥克立林 | 4.90% | 4.90% | 4.90% |
甲氧基肉桂酸乙基己酯 | 0.10% | 0.10% | 0.10% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 4.70% | 4.70% | 4.70% |
二乙基己基丁酰胺基三嗪酮(UVAsorb HEB,3V Sigma) | 3.70% | 3.70% | 3.70% |
二氧化钛;碳酸二乙基己酯;聚甘油-6聚羟基硬脂酸酯(TEGO® Sun TDEC 45,EvonikOperations GmbH) | 11.00% | 11.00% | 11.00% |
硬脂醇 | 0.50% | 0.50% | 0.50% |
硬脂酸甘油酯 | 0.50% | 0.50% | 0.50% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.20% | 0.20% | 0.20% |
甘油 | 2.00% | 2.00% | 2.00% |
去矿物质水 | 至100% | 至100% | 至100% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
柠檬酸三乙酯;辛二醇;苯甲酸(Verstatil® TBO;Evonik Dr. Straetmans GmbH) | 0.9% |
配方14a和14b:身体露
配方 | 14a | 14b |
实施例4的组合物 | 4.0% | 4.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 2.5% | 2.5% |
辛酸/癸酸甘油三酯(TEGOSOFT® CT,Evonik Operations GmbH) | 3.5% | 3.5% |
水 | 至100% | 至100% |
肌酸(TEGO® Cosmo C 100,Evonik Operations GmbH) | 0.5% | 0.5% |
卡波姆混悬液2(Carbomer,TEGO® Carbomer 141,Evonik Operations GmbH,在硬脂酸乙基己酯中20%) | 1.0% | 1.0% |
氢氧化钠(10%水溶液) | 0.6% | 0.6% |
苯氧基乙醇、乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.7% | |
水;乙酰丙酸钠;苯甲酸钠(Verstatil® BL; Evonik Dr. Straetmans GmbH) | 1.5% | |
辛酸甘油酯(dermosoft® GMCY MB; Evonik Dr. Straetmans GmbH) | 0.3% |
配方15a和15b:天然护理霜
配方 | 15a | 15b |
实施例4的组合物 | 6.0% | 6.0% |
辛酸/癸酸甘油三酯(TEGOSOFT® CT,Evonik Operations GmbH) | 8.0% | 8.0% |
棕榈酸异丙酯(TEGOSOFT® P,Evonik Operations GmbH) | 11.0% | 11.0% |
甜扁桃(甜杏仁)油 | 10.0% | 10.0% |
水 | 至100% | 至100% |
甘油 | 3.0% | 3.0% |
氢氧化钠(10%水溶液) | 0.2% | 0.2% |
苯甲醇、苯甲酸、山梨酸(Rokonsal BSB-N,Ashland Specialty Ingredients) | 0.8% | |
甘油;水;乙酰丙酸钠;茴香酸钠(dermosoft® 1388 eco; Evonik Dr. Straetmans GmbH) | 3% | |
辛酸甘油酯(dermosoft® GMCY MB; Evonik Dr. Straetmans GmbH) | 0.2% |
配方16a和16b:抗老化霜
配方 | 16a | 16b |
实施例4的组合物 | 6.0% | 6.0% |
辛酸/癸酸甘油三酯(TEGOSOFT® CT,Evonik Operations GmbH) | 9.5% | 9.5% |
苯甲酸C12-15烷基酯(TEGOSOFT® TN, Evonik Operations GmbH) | 9.5% | 9.5% |
水 | 至100% | 至100% |
甘油 | 3.0% | 3.0% |
四肽-21;甘油;丁二醇;水(TEGO® Pep 4-17, Evonik Operations) | 4.0% | 4.0% |
透明质酸钠(HyaCare®, Evonik Operations GmbH) | 0.1% | 0.1% |
水解的透明质酸(HyaCare® 50, Evonik Operations GmbH) | 0.1% | 0.1% |
水;硬脂酸乙基己酯;透明质酸钠交联聚合物;聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯;异硬脂酸钠(HyaCare® Filler CL, Evonik Operations GmbH) | 5.0% | 5.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | |
水;乙酰丙酸钠;山梨酸钾(VERSTATIL SL non GMO;Evonik Dr. Straetmans GmbH) | 1.2% | |
辛二醇(dermosoft® Octiol; Evonik Dr. Straetmans GmbH) | 0.2% |
配方17a和17b:O/W 粉底
配方 | 17a | 17b |
实施例4的组合物 | 6.0% | 6.0% |
肉豆蔻酸肉豆蔻酯(TEGOSOFT® MM, Evonik Operations GmbH) | 2.0% | 2.0% |
肉豆蔻酸异丙酯(TEGOSOFT® M, Evonik Operations GmbH) | 6.0% | 6.0% |
椰油酸癸酯(TEGOSOFT® DC, Evonik Operations GmbH) | 6.0% | 6.0% |
蓖麻油酸十六烷基酯(TEGOSOFT® CR, Evonik Operations GmbH) | 1.0% | 1.0% |
水 | 至100% | 至100% |
甘油 | 1.0% | 1.0% |
二氧化钛(Hombitan AC 360, Sachtleben) | 8.0% | 8.0% |
氧化铁(Sicovit Yellow 72, Rockwood Pigments) | 0.9% | 0.9% |
氧化铁(Sicovit Red E 172, Rockwood Pigments) | 0.2% | 0.2% |
氧化铁(Sicovit Brown 172, Rockwood Pigments) | 0.4% | 0.4% |
氧化铁(Sicovit Black 80 E 172, Rockwood Pigments) | 0.1% | 0.1% |
纤维素(TEGO® Feel Green, Evonik Operations GmbH) | 2.0% | 2.0% |
氢氧化钠(10%水溶液) | 0.2% | 0.2% |
苯甲醇、苯甲酸、山梨酸(Rokonsal BSB-N,Ashland Specialty Ingredients) | 1.0% | |
甲基丙二醇;辛二醇;苯丙醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 3.2% |
配方18a、18b、18c和18d:含有化妆品活性成分的润肤露
配方 | 18a | 18b | 18c | 18d |
实施例4的组合物 | 3.5% | 3.5% | 3.0% | 3.0% |
硬脂酸 | 0.5% | 0.5% | ||
硬脂酸甘油酯 | 0.5% | 0.6% | 0.6% | 0.6% |
鲸蜡硬脂醇 | 0.5% | 0.6% | 0.6% | 0.6% |
辛酸/癸酸甘油三酯 | 8.5% | 8.5% | 8.5% | 8.5% |
棕榈酸乙基己酯(TEGOSOFT® OP, Evonik Operations GmbH) | 8.5% | 8.5% | 8.5% | 8.5% |
去矿物质水 | 至100% | 至100% | 至100% | 至100% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.8% | 0.8% | 0.8% | 0.8% |
榄仁树皮提取物;戊二醇(建议的;TEGO® Arjuna S, Evonik OperationsGmbH) | 2.0% | 2.0% | 2.0% | |
甜菜碱;脲;乳酸钾;聚谷氨酸钠(建议的);水解菌核胶(TEGO® Smooth;EvonikOperations GmbH) | 5.0% | |||
苯氧乙醇、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯 (PhenonipXB (Clariant International Ltd.) | 1.0% | |||
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(MicrocareMEM,Thor) | 0.8% | 0.8% | ||
辛二醇;辛酸甘油酯;二丙二醇(dermosoft® MCAV MB;Evonik Dr. StraetmansGmbH) | 1.0% |
配方19a、19b和19c:低油相含量的润肤露
配方 | 19a | 19b | 19c |
实施例4的组合物 | 3.0% | 2.0% | 2.0% |
聚甘油-3二柠檬酸酯/硬脂酸酯(TEGO® Care PSC 3 (Evonik Operations GmbH) | 1.0% | 1.0% | |
鲸蜡硬脂醇 | 0.5% | 0.5% | 0.5% |
辛酸/癸酸甘油三酯 | 6.5% | 6.5% | 6.5% |
去矿物质水 | 至100% | 至100% | 至100% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.5% | 0.5% | 0.5% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | |
甘油;水;乙酰丙酸钠;茴香酸钠(dermosoft® 1388;Evonik Dr. Straetmans GmbH) | 3.0% |
配方20a、20b、20c和20d:O/W精华液1
配方 | 20a | 20b | 20c | 20d |
实施例4的组合物 | 2.5% | 2.5% | 4.0% | 4.0% |
硬脂酰谷氨酸钠(Eumulgin SG, BASF SE) | 1.0% | |||
硬脂酸甘油酯 | 0.75% | 0.75% | ||
硬脂醇 | 0.75% | 0.75% | ||
辛酸/癸酸甘油三酯 | 2.0% | 2.0% | 2.0% | 2.0% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 2.0% | 2.0% | 2.0% | 2.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 3.0% | 3.0% | ||
鳄梨(鳄梨)油 | 1.0% | 1.0% | 1.0% | 1.0% |
水;硬脂酸乙基己酯;透明质酸钠交联聚合物;聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯;异硬脂酸钠(HyaCare® Filler CL, Evonik Operations) | 3.0% | 3.0% | ||
去矿物质水 | 至100% | 至100% | 至100% | 至100% |
丁二醇 | 5.0% | 5.0% | 5.0% | 5.0% |
四肽-21;甘油;丁二醇;水(TEGO® Pep 4-17, Evonik Operations) | 2.0% | 2.0% | 2.0% | 2.0% |
水解透明质酸(HyaCare® 50, Evonik Operations) | 0.1% | 0.1% | 0.1% | 0.1% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.5% | 0.5% | 0.5% | 0.5% |
氢氧化钠(10%水溶液) | 0.2% | 0.2% | 0.2% | 0.2% |
苯甲醇、苯甲酸、山梨酸(Rokonsal BSB-N,Ashland Specialty Ingredients) | 0.8% | 0.8% | 0.8% | |
聚谷氨酸;菌核葡聚糖;甜菜碱;脲;乳酸钾(TEGO® Smooth Complex, EvonikOperations) | 3.0% | 3.0% | 3.0% | 3.0% |
柠檬酸三乙酯;辛酸甘油酯;苯甲酸(Verstatil® TBG;Evonik Dr. StraetmansGmbH) | 1.2% |
配方20e、20f、20g和20h:O/W精华液2
配方 | 20e | 20f | 20g | 20h |
实施例4的组合物 | 3.0% | 3.0% | 2.0% | 2.0% |
鲸蜡硬脂基葡糖苷(TEGO® Care CG 90,Evonik Operations GmbH) | 0.5% | |||
聚甘油-3二柠檬酸酯/硬脂酸酯(TEGO® Care PSC 3,Evonik OperationsGmbH) | 1.5% | 1.5% | ||
硬脂酸甘油酯 | 0.75% | 0.5% | 0.5% | 0.5% |
硬脂醇 | 0.75% | 0.5% | 0.5% | 0.5% |
辛酸/癸酸甘油三酯 | 2.0% | 2.0% | 2.0% | 2.0% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 2.0% | 2.0% | 2.0% | 2.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 3.0% | |||
鳄梨(鳄梨)油 | 1.0% | 1.0% | 1.0% | 1.0% |
水;硬脂酸乙基己酯;透明质酸钠交联聚合物;聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯;异硬脂酸钠(HyaCare® Filler CL, Evonik Operations) | 3.0% | 3.0% | 3.0% | |
去矿物质水 | 至100% | 至100% | 至100% | 至100% |
丁二醇 | 5.0% | 5.0% | 5.0% | 5.0% |
四肽-21;甘油;丁二醇;水(TEGO® Pep 4-17, Evonik Operations) | 2.0% | 2.0% | 2.0% | 2.0% |
水解透明质酸(HyaCare® 50, Evonik Operations) | 0.1% | 0.1% | 0.1% | 0.1% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.5% | 0.5% | 0.5% | 0.5% |
氢氧化钠(10%水溶液) | 0.2% | 0.2% | 0.2% | 0.2% |
苯甲醇、苯甲酸、山梨酸(Rokonsal BSB-N,Ashland Specialty Ingredients) | 0.8% | 0.8% | 0.8% | |
聚谷氨酸;菌核葡聚糖;甜菜碱;脲;乳酸钾(TEGO® Smooth Complex, EvonikOperations) | 3.0% | 3.0% | ||
柠檬酸三乙酯;辛二醇;苯甲酸(Verstatil® TBO;Evonik Dr. StraetmansGmbH) | 1.0% |
配方21a、21b和21c:O/W 遮瑕露
配方 | 21a | 21b | 21c |
实施例4的组合物 | 4.00% | 3.00% | 3.00% |
聚甘油-3-甲基葡萄糖二硬脂酸酯(TEGO® Care 450,Evonik Operations GmbH) | 1.00% | 1.00% | |
硬脂酸甘油酯 | 0.75% | 0.75% | 0.75% |
硬脂醇 | 0.75% | 0.75% | 0.75% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 7.40% | 7.40% | 7.40% |
水;硬脂酸乙基己酯;透明质酸钠交联聚合物;聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯;异硬脂酸钠(HyaCare® Filler CL, Evonik Operations) | 2.00% | 2.00% | 2.00% |
甲氧基肉桂酸乙基己酯 | 5.00% | 5.00% | 5.00% |
二乙基氨基羟基苯甲酰基苯甲酸己酯(Uvinul A Plus,BASF SE) | 3.00% | 3.00% | 3.00% |
植物鞘氨醇 | 0.10% | 0.10% | 0.10% |
水解透明质酸(HyaCare® 50, Evonik Operations) | 0.10% | 0.10% | 0.10% |
四肽-21;甘油;丁二醇;水(TEGO® Pep 4-17, Evonik Operations) | 2.00% | 2.00% | 2.00% |
去矿物质水 | 至100% | 至100% | 至100% |
二氧化钛(Hombitan AC 360, Sachtleben) | 3.00% | 3.00% | 3.00% |
滑石 | 2.00% | 2.00% | 2.00% |
氧化铁(Unipure Yellow LC 182, Sensient Technologies) | 0.36% | 0.36% | 0.36% |
氧化铁(Unipure Red LC 381, Sensient Technologies) | 0.12% | 0.12% | 0.12% |
氧化铁(Unipure Black LC 989, Sensient Technologies) | 0.08% | 0.08% | 0.08% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 4.44% | 4.44% | 4.44% |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 4.00% | 4.00% | 4.00% |
尼龙-10/10 (TEGOLON® ECO 10-10,Evonik Operations GmbH) | 3.00% | 3.00% | 3.00% |
甘油 | 3.00% | 3.00% | 3.00% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.50% | 0.50% | 0.50% |
乙醇 | 3.00% | 3.00% | 3.00% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.80% | 0.80% | |
甲基丙二醇;辛二醇(dermosoft® OMP;Evonik Dr. Straetmans GmbH) | 4.0% |
配方22a、22b、22c和22d:敏感皮肤润肤露
配方 | 22a | 22b | 22c | 22d |
实施例4的组合物 | 3.0% | 3.0% | 3.0% | 3.0% |
硬脂酸甘油酯 | 0.5% | 1.0% | 0.5% | 0.5% |
鲸蜡硬脂醇 | 1.0% | 1.0% | 1.0% | 1.0% |
乳木果(乳木果)油 | 3.0% | 3.0% | 3.0% | 3.0% |
辛酸/癸酸甘油三酯 | 5.0% | 5.0% | 5.0% | 5.0% |
棕榈酸异丙酯(TEGOSOFT® P,Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% | 5.0% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.2% | 0.2% | 0.2% | 0.2% |
甘油 | 5.0% | 5.0% | 5.0% | 5.0% |
脲 | 10.0% | 15.0% | 20.0% | 20.0% |
去矿物质水 | 至100% | 至100% | 至100% | 至100% |
苯氧基乙醇、乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.7% | |||
氢氧化钠(10%水溶液)(pH调节至5.0) | 适量 | |||
苯甲酸钠、山梨酸钾(Euxyl K 712, Schülke & Mayr GmbH) | 1.2% | |||
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(MicrocareMEM,Thor) | 0.8% | |||
茴香酸钠(dermosoft® anisate; Evonik Dr. Straetmans GmbH) | 0.12% | |||
乙酰丙酸;乙酰丙酸钠;甘油;水(dermosoft® 700B; Evonik Dr. StraetmansGmbH) | 1.0% | |||
辛酸甘油酯(dermosoft® GMC MB; Evonik Dr. Straetmans GmbH) | 0.3% |
配方23a、23b、23c和23d:干性皮肤护肤露1
配方 | 23a | 23b | 23c | 23d |
实施例4的组合物 | 3.0% | 2.5% | 3.0% | 3.0% |
硬脂酰谷氨酸钠(Eumulgin SG, BASF SE) | 1.0% | |||
硬脂酸甘油酯 | 1.0% | 1.0% | 1.5% | 1.5% |
鲸蜡硬脂醇 | 1.0% | 1.0% | 1.5% | 1.5% |
蓖麻油酸十六烷基酯 | 2.0% | 2.0% | 2.0% | 2.0% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% | 5.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 8.0% | 8.0% | 8.0% | 8.0% |
椰油酸癸酯(TEGOSOFT® DC, Evonik Operations GmbH) | 3.0% | 3.0% | 3.0% | 3.0% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.2% | 0.2% | 0.2% | 0.2% |
甘油 | 5.0% | 5.0% | 5.0% | 5.0% |
脲 | 10.0% | 10.0% | 15.0% | 15.0% |
去矿物质水 | 至100% | 至100% | 至100% | 至100% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | 0.8% | |
苯乙醇(dermosoft® PEA; Evonik Dr. Straetmans GmbH) | 1.0% |
配方23e、23f、23g和23h:干性皮肤护肤露2
配方 | 23e | 23f | 23g | 23h |
实施例4的组合物 | 2.5% | 3.0% | 3.0% | 3.0% |
聚甘油-6二硬脂酸酯 | 0.5% | |||
硬脂酸 | 0.5% | 0.5% | ||
硬脂酸甘油酯 | 1.5% | 1.5% | 1.5% | 1.5% |
鲸蜡硬脂醇 | 1.5% | 1.5% | 1.5% | 1.5% |
蓖麻油酸十六烷基酯 | 2.0% | 2.0% | 2.0% | 2.0% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% | 5.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 8.0% | 8.0% | 8.0% | 8.0% |
椰油酸癸酯(TEGOSOFT® DC, Evonik Operations GmbH) | 3.0% | 3.0% | 3.0% | 3.0% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.2% | 0.2% | 0.2% | 0.2% |
甘油 | 5.0% | 5.0% | 5.0% | 5.0% |
脲 | 15.0% | 20.0% | 20.0% | 20.0% |
去矿物质水 | 至100% | 至100% | 至100% | 至100% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | 0.8% | 0.8% | |
苯丙醇(dermosoft® 250 eco; Evonik Dr. Straetmans GmbH) | 0.4% | |||
1,2-己二醇(dermosoft® Hexiol;Evonik Dr. Straetmans GmbH) | 3.0% |
配方24a、24b和24c:无防腐剂润肤露 1
配方 | 24a | 24b | 24c |
实施例4的组合物 | 3.0% | 2.0% | 3.0% |
(AXOL® C 62, Evonik Operations GmbH) | 1.0% | ||
硬脂酸甘油酯 | 0.2% | 0.2% | 0.5% |
硬脂醇 | 0.2% | 0.2% | 0.5% |
甜扁桃(甜杏仁)油 | 10.0% | 10.0% | 10.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 6.6% | 6.6% | 6.0% |
甘油 | 4.0% | 4.0% | 4.0% |
去矿物质水 | 至100.0% | 至100.0% | 至100.0% |
辛二醇、甘油、辛酸甘油酯、苯丙醇(Dermosoft® LP;Evonik Dr. StraetmansGmbH) | 1.0% | 1.0% | |
甲基丙二醇、辛二醇、苯丙醇(Dermosoft® OMP,Evonik Dr. Straetmans GmbH) | 4.0% | ||
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.5% | 0.5% | 0.5% |
配方24d、24e和24f:无防腐剂润肤露 2
配方 | 24d | 24e | 24f |
实施例4的组合物 | 3.0% | 3.0% | 1.5% |
硬脂酸甘油酯 SE | 0.5% | ||
聚甘油-3二柠檬酸酯/硬脂酸酯(TEGO® Care PSC 3,Evonik Operations GmbH) | 1.5% | ||
硬脂酸甘油酯 | 0.5% | 0.5% | 0.5% |
硬脂醇 | 0.5% | 0.5% | 0.5% |
甜扁桃(甜杏仁)油 | 10.0% | 10.0% | 10.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 6.0% | 6.0% | 6.0% |
甘油 | 4.0% | 4.0% | 4.0% |
去矿物质水 | 至100.0% | 至100.0% | 至100.0% |
甲基丙二醇、辛二醇、苯丙醇(Dermosoft® OMP,Evonik Dr. Straetmans GmbH) | 4.0% | ||
辛二醇(Dermosoft® Octiol,Evonik Dr. Straetmans GmbH) | 0.4% | 0.4% | |
对茴香酸10%溶液(将3.0g氢氧化钠溶解在56.5g去矿物质水中,加入 30.0g甘油和10.0g的dermosoft® Octiol[Evonik Dr. Straetmans GmbH]并搅拌至溶液澄清) | 2.0% | 2.0% | |
柠檬酸(10%水溶液)(pH调节至6.0) | 适量 | 适量 | |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.5% | 0.5% | 0.5% |
配方25a和25b:W/O润肤露
配方 | 25a | 25b |
实施例5的组合物 | 2.0% | 2.0% |
蜂蜡 | 0.5% | 0.5% |
蓖麻蜡 | 0.5% | 0.5% |
全液石蜡 | 10.5% | 10.5% |
椰油酸癸酯(TEGOSOFT® DC, Evonik Operations GmbH) | 8.0% | 8.0% |
生育酚乙酸酯 | 0.5% | 0.5% |
环戊硅氧烷 | 6.0% | 6.0% |
氯化钠 | 0.5% | 0.5% |
水 | 至100% | 至100% |
甘油 | 3.0% | 3.0% |
苯氧基乙醇、乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.7% | |
乙醇 | 5.0% | 5.0% |
辛酸甘油酯(dermosoft® GMC;Evonik Dr. Straetmans GmbH) | 0.4% | |
硫酸锌 | 1.0% |
配方26a和26b:W/O霜
配方 | 26a | 26b |
实施例5的组合物 | 2.0% | 2.0% |
矿物油 | 17.0% | 17.0% |
蓖麻蜡 | 0.4% | 0.4% |
微晶蜡 | 0.6% | 0.6% |
水 | 至100% | 至100% |
氯化钠 | 0.5% | 0.5% |
脲 | 10.0% | 10.0% |
苯氧基乙醇、乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.7% | |
辛酸甘油酯(dermosoft® GMC;Evonik Dr. Straetmans GmbH) | 0.35% | |
戊二醇(dermosoft® Pentiol eco;Evonik Dr. Straetmans GmbH) | 2.0% |
配方27a和27b:速溶霜
配方 | 27a | 27b |
实施例5的组合物 | 0.8% | 0.8% |
十六烷基聚二甲基硅氧烷(ABIL® Wax 9801, Evonik Operations GmbH) | 1.6% | 1.6% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 4.0% | 4.0% |
聚二甲基硅氧烷(ABIL® 350, Evonik Operations GmbH) | 1.0% | 1.0% |
环戊硅氧烷 | 4.0% | 4.0% |
硬脂酸镁 | 0.3% | 0.3% |
水 | 至100% | 至100% |
丙二醇 | 5.0% | 5.0% |
氯化钠 | 1.0% | 1.0% |
甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯;二丙二醇(Microcare MEM,Thor) | 0.8% | |
辛酸甘油酯(dermosoft® GMC;Evonik Dr. Straetmans GmbH) | 0.25% | |
苯丙醇(dermosoft® 250 eco; Evonik Dr. Straetmans GmbH) | 0.35% |
配方28a、28b和28c:清凉身体乳
配方 | 28a | 28b | 28c |
实施例5的组合物 | 2.0% | 1.5% | 1.5% |
聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯(ISOLAN® GPS, Evonik OperationsGmbH) | - | 0.5% | 0.5% |
蓖麻蜡 | 0.5% | 0.5% | 0.5% |
蜂蜡 | 0.5% | 0.5% | 0.5% |
硬脂酸乙基己酯(TEGOSOFT® OS, Evonik Operations GmbH) | 10.0% | 10.0% | 10.0% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 8.5% | 8.5% | 8.5% |
聚二甲基硅氧烷(Belsil DM 5, Wacker Chemical Corp.) | 6.0% | 6.0% | 6.0% |
生育酚乙酸酯 | 0.5% | 0.5% | 0.5% |
甘油 | 3.0% | 3.0% | 3.0% |
水 | 至100% | 至100% | 至100% |
氯化钠 | 1.0% | 1.0% | 1.0% |
乙醇 | 20.0% | 20.0% | 20.0% |
乙基己基甘油(dermosoft® EHG; Evonik Dr. Straetmans GmbH) | 0.5% |
配方29a、29b和29c:基于天然成分的W/O霜
配方 | 29a | 29b | 29c |
实施例5的组合物 | 3.0% | 2.5% | 2.5% |
二异硬脂酰聚甘油-3二聚体二亚油酸酯(ISOLAN® PDI, Evonik Operations GmbH) | - | 0.5% | 0.5% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 7.0% | 7.0% | 7.0% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 3.0% | 3.0% | 3.0% |
杏仁油 | 7.0% | 7.0% | 7.0% |
乳木果油 | 2.0% | 2.0% | 2.0% |
蓖麻油酸十六烷基酯(TEGOSOFT® CR, Evonik Operations GmbH) | 1.0% | 1.0% | 1.0% |
蜂蜡 | 0.6% | 0.6% | 0.6% |
蓖麻蜡 | 0.4% | 0.4% | 0.4% |
甘油 | 5.0% | 5.0% | 5.0% |
水 | 至100% | 至100% | 至100% |
七水合硫酸镁 | 1.5% | 1.5% | 1.5% |
苯甲酸钠、山梨酸钾(Euxyl K 712, Schülke & Mayr GmbH) | 0.5% | 0.5% | |
戊二醇(dermosoft® Pentiol eco;Evonik Dr. Straetmans GmbH) | 3.0% |
配方30a、30b和30c:冷调润肤露
配方 | 30a | 30b | 30c |
实施例5的组合物 | 3.0% | 2.5% | 2.5% |
聚甘油-3油酸酯(ISOLAN® GO 33, Evonik Operations GmbH) | - | 0.5% | 0.5% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 12.0% | 12.0% | 12.0% |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | 4.0% | 4.0% | 4.0% |
硬脂酸锌 | 0.5% | 0.5% | 0.5% |
水 | 至100% | 至100% | 至100% |
甘油 | 3.0% | 3.0% | 3.0% |
氯化钠 | 1.5% | 1.5% | 1.5% |
苯氧基乙醇、乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.7% | 0.7% | |
苯甲醇;辛二醇;苯甲酸(VERSTATIL® BOB; Evonik Dr. Straetmans GmbH) | 1.5% |
配方31a、31b和31c:含有脲的保湿露
配方 | 31a | 31b | 31c |
实施例5的组合物 | 2.0% | 1.5% | 1.5% |
十六烷基PEG/PPG-10/1聚二甲基硅氧烷(ABIL® EM 180, Evonik Operations GmbH) | - | 0.5% | 0.5% |
微晶蜡 | 0.5% | 0.5% | 0.5% |
蓖麻蜡 | 0.5% | 0.5% | 0.5% |
苯甲酸C12-15烷基酯 | 7.5% | 7.5% | 7.5% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
棕榈酸乙基己酯(TEGOSOFT® OP, Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
辛酸/癸酸甘油三酯 | 5.0% | 5.0% | 5.0% |
甘油 | 3.0% | 3.0% | 3.0% |
脲 | 20.0% | 20.0% | 20.0% |
七水合硫酸镁 | 1.0% | 1.0% | 1.0% |
水 | 至100% | 至100% | 至100% |
苯氧基乙醇、乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.70% | 0.70% | |
香水 | 0.10% | 0.10% | 0.10% |
甲基丙二醇;苯氧乙醇;辛二醇(VERSTATIL® MPC; Evonik Dr. Straetmans GmbH) | 1.5% |
配方32a、32b、32c和32d:具有如丝般轻盈肤感的W/O润肤露
配方 | 32a | 32b | 32c | 33d |
实施例5的组合物 | 2.5% | 2.0% | 2.0% | 2.0% |
十六烷基PEG/PPG-10/1聚二甲基硅氧烷(ABIL® EM 90, Evonik OperationsGmbH) | - | 0.5% | - | - |
双-PEG/PPG-14/14聚二甲基硅氧烷;聚二甲基硅氧烷(ABIL® EM 97 S, EvonikOperations GmbH) | - | - | 1.0% | 1.0% |
微晶蜡 | 0.1% | 0.1% | 0.1% | 0.1% |
蓖麻蜡 | 0.1% | 0.1% | 0.1% | 0.1% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 11.8% | 11.8% | 11.8% | 11.8% |
肉豆蔻酸肉豆蔻酯(TEGOSOFT® MM, Evonik Operations GmbH) | 1.0% | 1.0% | 1.0% | 1.0% |
聚二甲基硅氧烷(Belsil DM 5, Wacker Chemical Corp.) | 8.0% | 8.0% | 8.0% | 8.0% |
聚二甲基硅氧烷(ABIL® 350, Evonik Operations GmbH) | 0.5% | 0.5% | 0.5% | 0.5% |
甘油 | 3.0% | 3.0% | 3.0% | 3.0% |
七水合硫酸镁 | 1.5% | 1.5% | 1.5% | 1.5% |
水 | 至100% | 至100% | 至100% | 至100% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% | 0.7% | |
苯氧乙醇;乙基己基甘油(VERSTATIL® PE; Evonik Dr. Straetmans GmbH) | 1.0% |
配方33a、33b和33c:婴儿护理产品
配方 | 33a | 33b | 33c |
实施例5的组合物 | 3.0% | 2.0% | 2.0% |
液体石蜡;凡士林;地蜡;油酸甘油酯;羊毛脂醇(PROTEGIN ® XN, Evonik OperationsGmbH) | - | 1.0% | 1.0% |
蓖麻蜡 | 0.1% | 0.1% | 0.1% |
微晶蜡 | 0.1% | 0.1% | 0.1% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 1.0% | 1.0% | 1.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 3.8% | 3.8% | 3.8% |
棕榈酸乙基己酯(TEGOSOFT® OP, Evonik Operations GmbH) | 1.0% | 1.0% | 1.0% |
杏仁油 | 1.0% | 1.0% | 1.0% |
氧化锌 | 20.0% | 20.0% | 20.0% |
甘油 | 3.0% | 3.0% | 3.0% |
七水合硫酸镁 | 1.0% | 1.0% | 1.0% |
乳酸钠;PCA钠;甘氨酸;果糖;脲;烟酰胺;肌醇;苯甲酸钠;乳酸(LACTIL, EvonikOperations GmbH) | 5.0% | 5.0% | 5.0% |
甜菜碱(TEGO® Natural Betaine, Evonik Operations GmbH) | 3.0% | 3.0% | 3.0% |
水 | 至100% | 至100% | 至100% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% | |
对茴香酸(dermosoft® 688; Evonik Dr. Straetmans GmbH) | 0.12% | ||
戊二醇(dermosoft® Pentiol eco;Evonik Dr. Straetmans GmbH) | 2.5% |
配方34a、34b和34c:足部护理产品
配方 | 34a | 34b | 34c |
实施例5的组合物 | 3.0% | 2.5% | 2.5% |
凡士林;地蜡;氢化蓖麻油;异硬脂酸甘油酯;聚甘油-3油酸酯(PROTEGIN ® W, EvonikOperations GmbH) | - | 0.5% | 0.5% |
蓖麻蜡 | 0.1% | 0.1% | 0.1% |
微晶蜡 | 0.1% | 0.1% | 0.1% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 9.0% | 9.0% | 9.0% |
棕榈酸乙基己酯(TEGOSOFT® OP, Evonik Operations GmbH) | 9.0% | 9.0% | 9.0% |
庚酸硬脂酯(TEGOSOFT® SH, Evonik Operations GmbH) | 8.8% | 8.8% | 8.8% |
甘油 | 3.0% | 3.0% | 3.0% |
七水合硫酸镁 | 1.0% | 1.0% | 1.0% |
神经酰胺NP;神经酰胺 AP;神经酰胺 EOP;植物鞘氨醇;胆固醇;月桂酰乳酸钠;卡波姆;黄原胶(SK-INFLUX V,Evonik Operations GmbH) | 5.0% | 5.0% | 5.0% |
甜菜碱(TEGO® Natural Betaine, Evonik Operations GmbH) | 3.0% | 3.0% | 3.0% |
水 | 至100% | 至100% | 至100% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% | |
苯氧乙醇;苯甲酸(Verstatil® BP; Evonik Dr. Straetmans GmbH) | 1.0% |
配方35a和35b:带有驱虫防护的防晒露SPF 30 UVA
配方 | 35a | 35b |
实施例5的组合物 | 3.0% | 2.0% |
聚甘油-2二聚羟基硬脂酸酯(Dehymuls PGPH, BASF SE) | - | 1.0% |
芥酸油酯(TEGOSOFT® OER, Evonik Operations GmbH) | 1.5% | 1.5% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 1.5% | 1.5% |
二乙基氨基羟基苯甲酰基苯甲酸己酯(Uvinul A Plus,BASF SE) | 5.4% | 5.4% |
甲氧基肉桂酸乙基己酯 | 10.0% | 10.0% |
奥克立林 | 2.0% | 2.0% |
聚丙烯酰胺;C13-14异链烷烃;Laureth-7(Sepigel 305, Seppic) | 2.1% | 2.1% |
丁基乙酰基氨基丙酸乙酯(R3535, Merck KGaA) | 4.0% | 4.0% |
生育酚乙酸酯 | 0.5% | 0.5% |
甘油 | 3.0% | 3.0% |
乙醇 | 0.5% | 0.5% |
七水合硫酸镁 | 1.0% | 1.0% |
水 | 至100% | 至100% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% |
香水 | 0.1% | 0.1% |
配方36a和36b:根据Ecocert标准的防晒露SPF 30 UVA
配方 | 36a | 36b |
实施例5的组合物 | 3.0% | 2.0% |
聚甘油-3聚蓖麻油酸酯(Cithrol PG3PR, (Croda Int. Plc) | - | 1.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik Operations GmbH) | 2.0% | 2.0% |
椰油酸癸酯(TEGOSOFT® DC, Evonik Operations GmbH) | 10.0% | 10.0% |
棕榈酸异丙酯(TEGOSOFT® P,Evonik Operations GmbH) | 10.0% | 10.0% |
氧化锌(氧化锌PI,Symrise) | 16.0% | 16.0% |
二氧化钛(纳米);氧化铝;硬脂酸(Eusolex T-S, Merck KGaA) | 9.0% | 9.0% |
水 | 至100% | 至100% |
甘油 | 3.0% | 3.0% |
七水合硫酸镁 | 1.0% | 1.0% |
苯甲酸钠、山梨酸钾(Euxyl K 712, Schülke & Mayr GmbH) | 0.5% | 0.5% |
配方37a、37b、37c和37d:防晒喷雾SPF 30 UVA
配方 | 37a | 37b | 37c | 37d |
实施例5的组合物 | 3.0% | 2.0% | 3.0% | 2.0% |
十六烷基PEG/PPG-10/1聚二甲基硅氧烷(ABIL® EM 90, Evonik OperationsGmbH) | - | 1.0% | - | - |
聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯(ISOLAN® GPS, EvonikOperations GmbH) | - | - | - | 1.0% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 13.0% | 13.0% | 11.3% | 11.3% |
苯甲酸C12-15烷基酯 | 13.0% | 13.0% | 11.3% | 11.3% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 1.0% | 1.0% | 1.5% | 1.5% |
丁基甲氧基二苯甲酰基甲烷 | - | - | 3.0% | 3.0% |
甲氧基肉桂酸乙基己酯 | 5.0% | 5.0% | - | - |
奥克立林 | - | - | 6.0% | 6.0% |
胡莫柳酯 | - | - | 4.0% | 4.0% |
二乙基氨基羟基苯甲酰基苯甲酸己酯(Uvinul A Plus,BASF SE) | 5.0% | 5.0% | - | - |
水 | 至100% | 至100% | 至100% | 至100% |
甘油 | 3.0% | 3.0% | 3.0% | 3.0% |
七水合硫酸镁 | 1.0% | 1.0% | 1.0% | 1.0% |
UV滤光液(20%苯基苯并咪唑磺酸(Eusolex 232, Merck KGaA,8.8% 三(羟甲基)氨基甲烷,水至100%) | 15.0% | 15.0% | 15.0% | 15.0% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% | 0.7% | 0.7% |
配方38a、38b、38c和38d:防晒露 SPF 50 UVA
配方 | 38a | 38b | 38c | 38d |
实施例5的组合物 | 3.0% | 2.5% | 3.0% | 2.5% |
十六烷基PEG/PPG-10/1聚二甲基硅氧烷(ABIL® EM 90, Evonik OperationsGmbH) | - | 1.0% | - | 1.0% |
微晶蜡 | 0.3% | 0.3% | 0.3% | 0.3% |
蓖麻蜡 | 0.3% | 0.3% | 0.3% | 0.3% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 2.4% | 2.4% | - | - |
辛酸苯氧基乙酯(TEGOSOFT® XC,Evonik Operations GmbH) | - | - | 3.9% | 3.9% |
双乙基己基氧基苯酚甲氧基苯基三嗪(Tinosorb S,BASF SE) | 6.0% | 6.0% | - | - |
二乙基氨基羟基苯甲酰基苯甲酸己酯(Uvinul A Plus,BASF SE) | 7.0% | 7.0% | 5.0% | 5.0% |
丁基甲氧基二苯甲酰基甲烷 | - | - | 4.5% | 4.5% |
水杨酸乙基己酯 | 3.0% | 3.0% | 5.0% | 5.0% |
甲氧基肉桂酸乙基己酯 | 7.0% | 7.0% | - | - |
奥克立林 | - | - | 9.0% | 9.0% |
胡莫柳酯 | 3.0% | 3.0% | 5.0% | 5.0% |
乙基己基三嗪酮(Uvinul T 150, BASF SE) | 1.0% | 1.0% | 2.0% | 2.0% |
二氧化钛;二氧化硅;聚二甲基硅氧烷(Parsol TX (DSM Nutritional ProductsLlc.) | 2.0% | 2.0% | 2.0% | 2.0% |
水 | 至100% | 至100% | 至100% | 至100% |
甘油 | 3.0% | 3.0% | 3.0% | 3.0% |
七水合硫酸镁 | 1.5% | 1.5% | 1.5% | 1.5% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% | 0.7% | |
天然苯乙醇 | 0.7% |
配方39a、39b和39c:根据FDA标准的防晒露SPF 50
配方 | 39a | 39b | 39c |
实施例5的组合物 | 2.0% | 1.5% | 1.5% |
月桂基PEG-10三(三甲基甲硅烷氧基)甲硅烷基乙基聚二甲基硅氧烷 (ES-5300配制助剂, Dow Corning Corp.) | - | 0.5% | 0.5% |
甲氧基肉桂酸乙基己酯;二乙氨基羟基苯甲酰基苯甲酸己酯(Uvinul A+B, BASF SE) | 7.5% | 7.5% | 7.5% |
水杨酸乙基己酯 | 5.0% | 5.0% | 5.0% |
胡莫柳酯 | 15.0% | 15.0% | 15.0% |
丁基甲氧基二苯甲酰基甲烷 | 3.0% | 3.0% | 3.0% |
二苯甲酮-3 | 6.0% | 6.0% | 6.0% |
奥克立林 | 10.0% | 10.0% | 10.0% |
三异硬脂精 | 2.0% | 2.0% | 2.0% |
微晶蜡 | 1.2% | 1.2% | 1.2% |
蓖麻蜡 | 0.8% | 0.8% | 0.8% |
十六烷基聚二甲基硅氧烷(ABIL® Wax 9801, Evonik Operations GmbH) | 2.0% | 2.0% | 2.0% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 2.0% | 2.0% | 2.0% |
水 | 至100% | 至100% | 至100% |
氯化钠 | 1.0% | 1.0% | 1.0% |
乙二胺四乙酸 | 0.1% | 0.1% | 0.1% |
丙二醇 | 3.0% | 3.0% | 3.0% |
苯氧基乙醇;乙基己基甘油(Euxyl PE 9010, Schülke & Mayr GmbH) | 0.7% | 0.7% | |
Verstatil PC | 1.0% |
配制剂40a、40b、40c、40d、40e和40f:粉底
配方 | 40a | 40b | 40c | 40d | 40e | 40f |
实施例5的组合物 | 4.5% | 2.5% | 3.0% | 2.5% | 2.0% | 2.0% |
双-(甘油基/月桂基)甘油基月桂基聚二甲基硅氧烷;辛酸/癸酸甘油三酯(ABIL® EM 120, EvonikOperations GmbH) | - | 2.0% | - | - | - | - |
聚甘油-4异硬脂酸酯(ISOLAN® GI 34, EvonikOperations GmbH) | - | - | 1.0% | - | - | - |
十六烷基二甘油基三(三甲基甲硅烷氧基)甲硅烷基乙基 聚二甲基硅氧烷(DC-5600, Dow CorningCorp.) | - | - | - | 1.0% | - | - |
月桂基聚甘油-3聚二甲基甲硅烷氧乙基聚二甲基硅氧烷(KF-6105, Shin-Etsu Chemical Co.) | - | - | - | - | 1.0% | - |
聚甘油-4异硬脂酸酯;十六烷基PEG/PPG-10/1聚二甲基硅氧烷;月桂酸己酯(ABIL® WE 09, EvonikOperations GmbH) | - | - | - | - | - | 2.0% |
椰油酸异戊酯(TEGOSOFT® AC,Evonik OperationsGmbH) | 10.8% | 10.8% | 10.8% | 10.8% | 10.8% | 10.8% |
芥酸油酯(TEGOSOFT® OER, Evonik OperationsGmbH) | 8.0% | 8.0% | 8.0% | 8.0% | 8.0% | 8.0% |
二氧化钛、氧化铝、三乙氧基辛基硅烷(HombitanAC360, Sachtleben) | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% |
氧化铁(Sicovit Brown 70 E 172, Rockwood) | 2.1% | 2.1% | 2.1% | 2.1% | 2.1% | 2.1% |
尼龙-12 (TEGOLON® 12-20, Evonik OperationsGmbH) | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% |
环戊硅氧烷 | 3.5% | 3.5% | 3.5% | 3.5% | 3.5% | 3.5% |
二硬脂二甲铵锂蒙脱石(Bentone 38 V CG,Elementis) | 1.0% | 1.0% | 1.0% | 1.0% | 1.0% | 1.0% |
碳酸丙烯酯 | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% |
水 | 至100% | 至100% | 至100% | 至100% | 至100% | 至100% |
七水合硫酸镁 | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% |
甘油 | 5.0% | 5.0% | 5.0% | 5.0% | 5.0% | 5.0% |
肌酸(TEGO<sup>®</sup> Cosmo C 100, Evonik OperationsGmbH) | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% |
鲸蜡硬脂醇聚醚-25;甘油;鲸蜡醇;山嵛酸;胆固醇;神经酰胺EOP;神经酰胺EOS;神经酰胺NP;神经酰胺NS;神经酰胺AP;己酰基植物鞘氨醇;己酰基鞘氨醇(SKINMIMICS, Evonik Operations GmbH) | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% |
苯甲醇;乙基己基甘油;生育酚(Euxyl K 900, Schülke & Mayr GmbH) | 0.7% | 0.7% | 0.7% | 0.7% | 0.7% | 0.7% |
配制剂41a、41b、41c、41d、41e、41f和41g:CC(颜色控制)流体
配方 | 41a | 41b | 41c | 41d | 41e | 41f | 41g |
实施例5的组合物 | 3.0% | 2.0% | 2.5% | 3.0% | 2.5% | 2.0% | 1.0% |
聚甘油-4二异硬脂酸酯/聚羟基硬脂酸酯/癸二酸酯(ISOLAN®GPS, Evonik Operations GmbH) | - | 1.0% | - | - | - | - | - |
脱水山梨糖醇油酸酯(TEGO® SMO V, Evonik Operations GmbH) | - | - | 0.5% | - | - | - | - |
PEG-30二聚羟基硬脂酸酯(Arlacel P135, Croda) | - | - | - | 1.0% | - | - | - |
聚甘油-3二异硬脂酸酯(Lameform TGI, BASF SE) | - | - | - | - | 1.5% | - | - |
油酸甘油酯、聚甘油-3聚蓖麻油酸酯、油橄榄(橄榄)油非皂化物(Plantasens天然乳化剂CP5, Clariant) | - | - | - | - | - | 1.0% | - |
月桂基PEG-9聚二甲基甲硅烷氧乙基聚二甲基硅氧烷(KF-6038,Shin-Etsu Chemical Co.) | - | - | - | - | - | - | 1.0% |
甲氧基肉桂酸乙基己酯;二乙氨基羟基苯甲酰基苯甲酸己酯(Uvinul A+B, BASF SE) | 10.0% | 10.0% | 10.0% | 10.0% | 10.0% | 10.0% | 10.0% |
环戊硅氧烷 | 3.5% | 3.5% | 3.5% | 3.5% | 3.5% | 3.5% | 3.5% |
二硬脂二甲铵锂蒙脱石(Bentone 38 V CG, Elementis) | 1.0% | 1.0% | 1.0% | 1.0% | 1.0% | 1.0% | 1.0% |
碳酸亚丙酯 | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% | 0.5% |
二氧化钛、氧化铝、三乙氧基辛基硅烷(Hombitan AC360,Sachtleben) | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% |
滑石 | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% |
氧化铁;三乙氧基辛基硅烷(Unipure Yellow LC 182 AS-EM,Sensient) | 0.4% | 0.4% | 0.4% | 0.4% | 0.4% | 0.4% | 0.4% |
氧化铁;三乙氧基辛基硅烷(Unipure Red LC 381 AS-EM,Sensient) | 0.12% | 0.12% | 0.12% | 0.12% | 0.12% | 0.12% | 0.12% |
氧化铁;三乙氧基辛基硅烷(Unipure Black LC 989 AS-EM,Sensient) | 0.08% | 0.08% | 0.08% | 0.08% | 0.08% | 0.08% | 0.08% |
碳酸二乙基己酯(TEGOSOFT® DEC,Evonik Operations GmbH) | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% |
苯甲酸C12-15烷基酯 | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% |
棕榈酸异丙酯(TEGOSOFT® P,Evonik Operations GmbH) | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% | 4.0% |
尼龙-12 (TEGOLON® 12-20, Evonik Operations GmbH) | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% | 2.0% |
水 | 至100% | 至100% | 至100% | 至100% | 至100% | 至100% | 至100% |
甘油 | 5.0% | 5.0% | 5.0% | 5.0% | 5.0% | 5.0% | 5.0% |
氯化钠 | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% | 1.5% |
四肽-30;甘油(TEGO® Pep 4-Even, Evonik Operations GmbH) | 0.3% | 0.3% | 0.3% | 0.3% | 0.3% | 0.3% | 0.3% |
苯氧乙醇;对羟基苯甲酸甲酯;对羟基苯甲酸乙酯;对羟基苯甲酸丙酯 (Phenonip XB,Clariant) | 0.7% | 0.7% | 0.7% | 0.7% | 0.7% | 0.7% | 0.7% |
配方42a、42b、42c、42d和42e:止汗/除臭喷雾或气溶胶喷雾
配方43a、43b、43c和43d:防晒气溶胶 SPF 50 UVA
配制剂44:沐浴露
水 | 至100.0% |
实施例1、2或3的组合物 | 1.5% |
月桂醇聚醚硫酸钠(Texapon NSO, BASF, 28%) | 25.0% |
椰油基-葡糖苷(Plantacare 818 UP, BASF, 51%) | 8.0% |
椰油酰胺丙基甜菜碱(TEGO® Betain F 50, Evonik, 38%) | 8.0% |
PEG-18甘油油酸酯/椰油酸酯(ANTIL® 171, Evonik) | 1.5% |
脱水山梨糖醇倍半辛酸酯(ANTIL® Soft SC, Evonik) | 0.8% |
油酸甘油酯(TEGIN® O V, Evonik) | 0.8% |
香辛草(IFF) | 0.2% |
聚甘油-4癸酸酯(TEGOSOFT® PC 41, Evonik) | 0.6% |
向日葵籽油(AEC葵花籽油,A & E Connock, Perfumery & Cosmetics Ltd.) | 0.2% |
芳樟醇(Lipofresh, Lipo Chemicals, Inc.) | 0.1% |
香豆素(Rhodiascent extra pure, Solvay Rhodia) | 0.1% |
甘油(甘油EP,植物,Spiga Nord) | 0.4% |
羟丙基甲基纤维素(TEGOCEL ® HPM 50, Evonik) | 0.2% |
二硬脂酸乙二醇酯(TEGIN ® G 1100 Pellets, Evonik) | 0.4% |
氯化钠 | 0.5% |
羟丙基瓜尔胶羟丙基三甲基氯化铵(Jaguar C-162, Solvay Rhodia) | 0.2% |
dermofeel TOCO 70 non GMO | 0.1% |
EDTA二钠(Dissolvine NA-2-P, AkzoNobel) | 0.1% |
防腐剂 | 适量 |
柠檬酸 | 至pH5.2 |
配制剂45:沐浴露
配制剂46:香波
配方47a和47b:洗发水
配方 | 47a | 47b |
水 | 至100.0% | 至100.0% |
实施例1、2或3的组合物 | 2.5% | 2.5% |
实施例4的组合物 | 1.5% | 1.5% |
椰油酰胺丙基甜菜碱(TEGO® Betain F 50, Evonik, 38%) | 22.0% | 22.0% |
月桂基-葡糖苷(Plantacare 1200 UP, BASF, 50%) | 6.0% | 6.0% |
椰油酰谷氨酸钠(Plantapon ACG HC, BASF) | 1.5% | 1.5% |
椰油酰甘氨酸钠(Hostapon SG, Clariant) | 0.8% | 0.8% |
吡啶硫酮锌(Microcare ZP, Thor) | 0.1% | 0.1% |
PEG-120甲基葡萄糖二油酸酯(ANTIL® 120 Plus, Evonik) | 0.4% | 0.4% |
氯化钠 | 0.5% | 0.5% |
异硬脂酰胺 MIPA;月桂酸甘油酯(ANTIL® SPA 80, Evonik) | 0.5% | 0.5% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 0.3% | 0.3% |
羟丙基瓜尔胶羟丙基三甲基氯化铵(Jaguar C-162, Solvay Rhodia) | 0.3% | 0.3% |
季铵盐-80 (ABIL® Quat 3272, Evonik) | 0.4% | 0.4% |
棕榈酰胺丙基三甲基氯化铵(VARISOFT® PATC, Evonik) | 0.4% | 0.4% |
刺阿干树油(摩洛哥坚果油, DSM Nutritional Products Ltd.) | 0.1% | 0.1% |
甘油(甘油EP,植物,Spiga Nord) | 0.6% | 0.6% |
EDTA四钠(Versene 100, The Dow Chemical Company) | 0.1% | 0.1% |
咖啡因(Merck KGaA/EMD Chemicals, Inc.) | 0.1% | 0.1% |
水解小麦蛋白(Gluadin WLM, BASF) | 0.1% | 0.1% |
柠檬烯(双戊烯122号, Hercules Inc.) | 0.1% | 0.1% |
柠檬酸 | 至pH5.5 | 至pH5.5 |
植酸钠;水;醇(dermofeel® PA-3; Evonik Dr. Straetmans GmbH (PA-3) | 0.1% | |
香水 | 0.2% | |
防腐剂 | 适量 | |
水;乙酰丙酸钠;苯甲酸钠(Verstatil® BL non-GMO;Evonik Dr. Straetmans GmbH) | 1.2% |
配制剂48:洗手液
水 | 至100% |
甘油(甘油EP,植物,Spiga Nord) | 4.0% |
醇 | 4.0% |
椰油醇硫酸钠(Texapon HC G, BASF) | 3.0% |
月桂基-葡糖苷(Plantacare 1200 UP, BASF, 50%) | 6.0% |
实施例1、2或3的组合物 | 3.0% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 1.5% |
芒果(芒果)果实提取物(芒果提取物,Draco Natural Products) | 0.5% |
柠檬烯(双戊烯122号, Hercules Inc.) | 0.1% |
芳樟醇(Lipofresh, Lipo Chemicals, Inc.) | 0.1% |
柠檬酸 | 至pH4.9 |
防腐剂 | 适量 |
染料 | 适量 |
配制剂49:肥皂膏
水 | 至100% |
丙二醇(Euxyl K 320, Schülke & Mayr GmbH) | 2.0% |
椰油基-葡糖苷(Plantacare 818 UP, BASF, 51%) | 10.0% |
甘油(甘油EP,植物,Spiga Nord) | 5.0% |
实施例1、2或3的组合物 | 2.5% |
椰油酰谷氨酸二钠(Planatpon ACG LC, BASF) | 2.5% |
黄原胶(Keltrol CG-SFT,CP Kelco) | 1.2% |
硬脂酸(Pristerene 4922, Croda Europe, Ltd.) | 1.2% |
柠檬酸 | 至pH5.5 |
油橄榄果油(Cropure Olive, Croda Europe, Ltd.) | 0.2% |
油酸甘油酯(TEGIN® O V, Evonik) | 1.0% |
椰油酰谷氨酸钠(Plantapon ACG HC, BASF) | 0.8% |
EDTA四钠(Versene 100, The Dow Chemical Company) | 0.2% |
香水 | 0.1% |
防腐剂 | 适量 |
染料 | 适量 |
配制剂50:油浴
水 | 至100.0% |
甘氨酸大豆油(Cropure Soybean, Croda Europe, Ltd.) | 20.0% |
实施例1、2或3的组合物 | 12.0% |
聚甘油-3棕榈酸酯(Dermofeel® PP, Evonik Dr. Straetmans) | 4.5% |
辛酸甘油酯(Dermosoft® GMCY, Evonik Dr. Straetmans) | 3.0% |
荷荷巴油(AEC精制荷荷巴油, A & E Connock, Perfumery & Cosmetics Ltd.) | 1.2% |
甜扁桃(甜杏仁)油(Cropure Almond, Croda Europe, Ltd.) | 1.0% |
小麦胚芽油(Cropure Wheatgerm, Croda Europe, Ltd.) | 0.5% |
生育酚(Euxyl K 700, Schülke & Mayr GmbH) | 0.2% |
柠檬烯(Dipentene No. 122, Hercules Inc.) | 0.1% |
柠檬醛 | 0.1% |
防腐剂 | 适量 |
染料 | 适量 |
配制剂51:卸妆用胶束水
水 | 至100.0% |
香水 | 0.1% |
实施例1、2或3的组合物 | 2.0% |
辛基/癸酰胺丙基甜菜碱(TEGO® Betain 810, Evonik, 38%) | 1.3% |
聚甘油-6辛酸酯;聚甘油-3椰油酸酯;聚甘油-4癸酸酯;聚甘油-6蓖麻油酸酯(TEGO® Solve 61, Evonik) | 1.0% |
甜菜碱(TEGO® Natural Betaine, Evonik) | 2.0% |
甘油(甘油EP,植物,Spiga Nord) | 1.0% |
防腐剂 | 适量 |
配方52a和52b:湿巾用溶液
配方 | 52a | 52b |
实施例1、2或3的组合物 | 3.5% | 3.5% |
库拉索芦荟叶提取物(Aloe-Con UP 40, Florida Food Products Inc.) | 0.2% | 0.2% |
肉豆蔻酸异丙酯(TEGOSOFT® M, Evonik) | 0.2% | 0.2% |
椰油酰两性基二乙酸二钠(REWOTERIC® AM 2 C NM, Evonik, 39%) | 1.5% | 1.5% |
香水 | 0.2% | 0.2% |
丙二醇(Euxyl K 320, Schülke & Mayr GmbH) | 2.5% | 2.5% |
水解蚕丝(Crosilk 10000, Croda Inc.) | 0.2% | 0.2% |
辛基/癸基葡糖苷(Plantacare 810 UP, BASF) | 1.0% | 1.0% |
水 | 至100.0% | 至100.0% |
柠檬酸 | 至pH5.0 | 至pH5.0 |
苯氧乙醇(S&M Phenoxyethanol, Schülke & Mayr GmbH) | 0.5% | 0.5% |
脱氢乙酸(Unisept DHA (Universal Preserv-A-Chem, Inc.) | 0.1% | 0.1% |
苯甲酸钠(Euxyl K 712, Schülke & Mayr GmbH) | 0.4% | 0.4% |
水杨酸(天然水杨酸;Evonik Dr. Straetmans GmbH) | 0.5% |
配制剂53:止汗除臭剂
配制剂54:漱口水
配制剂55:牙膏
Claims (15)
1.木糖醇羧酸酯,其包含
木糖醇的羧酸酯、1,4-脱水木糖醇的羧酸酯、1,4-脱水阿拉伯糖醇的羧酸酯和1,4-脱水核糖醇的羧酸酯,其中所述木糖醇羧酸酯中包含的木糖醇残基与所述木糖醇羧酸酯中包含的所有1,4-脱水木糖醇残基、1,4-脱水阿拉伯糖醇残基和1,4-脱水核糖醇残基的总和的重量比大于或等于96:4,优选大于97:3,更优选大于98:2,最优选大于99:1,
其特征在于:所述木糖醇的羧酸酯中的酯化伯羟基与酯化仲羟基的摩尔比为80:20至20:80,优选75:25至25:75,甚至更优选70:30至30:70,甚至更优选65:35至40:60。
2.根据权利要求1所述的木糖醇羧酸酯,其特征在于:所述羧酸部分衍生自含有2至34,优选4至24,更优选6至22个碳原子的羧酸,尤其是天然脂肪酸或其混合物。
3.根据权利要求1或2所述的木糖醇羧酸酯,其特征在于:所包含的木糖醇的羧酸酯的平均酯化度为0.3至4.0,优选1.0至3.0,更优选1.1至2.7,特别优选1.3至2.6。
4.根据前述权利要求中至少一项所述的木糖醇羧酸酯,其特征在于:所包含的木糖醇的羧酸酯包含木糖醇单酯、木糖醇二酯和木糖醇三酯,其中优选以基于所有包含的木糖醇的羧酸酯计10重量%至50重量%,优选15重量%至45重量%,更优选20重量%至40重量%的量包含所述木糖醇三酯。
5.根据前述权利要求中至少一项所述的木糖醇羧酸酯,其特征在于:它含有
0.05重量%至40重量%,优选0.2重量%至25重量%,更优选0.5重量%至10重量%的游离木糖醇。
6.根据前述权利要求中至少一项所述的木糖醇羧酸酯,其特征在于:它含有
小于25重量%,优选0.01重量%至20重量%,更优选0.05重量%至10重量%的至少一种游离羧酸。
7.根据前述权利要求中至少一项所述的木糖醇羧酸酯,其特征在于:所述木糖醇的羧酸酯的整个单酯部分中包含5重量%至25重量%,优选7重量%至15重量%,更优选9重量%至13重量%的仲酯区域异构体。
8.根据前述权利要求中至少一项所述的木糖醇羧酸酯,其特征在于:所述木糖醇的羧酸酯的整个单酯部分中和所述木糖醇的羧酸酯的整个二酯部分中各自包含至少两种区域异构体。
9.酶促制备木糖醇羧酸酯,优选根据权利要求1至8中至少一项所述的木糖醇羧酸酯的方法,其包括以下方法步骤:
A) 提供木糖醇和至少一种酰基供体,优选脂肪酸酰基供体,特别选自脂肪酸酯和脂肪酸,特别优选脂肪酸,
B) 在75℃至110℃,优选77℃至100℃,甚至更优选80℃至95℃的温度下,在脂肪酶存在下使木糖醇与所述至少一种酰基供体反应,得到木糖醇羧酸酯,并任选地
C) 纯化所述木糖醇羧酸酯。
10.根据权利要求9所述的方法,其特征在于:所述方法步骤A)包括
将木糖醇和所述至少一种酰基供体共混至少十分钟,优选30分钟,甚至更优选60分钟,
其中所述共混优选在80℃至120℃,优选90℃至120℃,甚至更优选95℃至120℃,甚至更优选100℃至120℃的温度范围内进行。
11.根据权利要求9或10所述的方法,其特征在于:所述木糖醇和所述至少一种酰基供体占基于方法步骤B)开始时整个反应混合物计至少80重量%,优选至少90重量%,更优选至少95重量%。
12.根据权利要求9至11中至少一项所述的方法,其特征在于:所述脂肪酶选自:来自绵毛嗜热丝菌(Thermomyces lanuginosus)的脂肪酶(登录号O59952)、来自南极假丝酵母(Candida antarctica)的脂肪酶A和B(登录号P41365)和来自米赫毛霉(Mucor miehei)的脂肪酶(登录号P19515)、来自腐质霉属(Humicola sp.)的脂肪酶(登录号 O59952)、来自爪哇根毛霉(Rhizomucor javanicus)的脂肪酶(登录号 S32492)、来自米根霉(Rhizopus oryzae)的脂肪酶(登录号 P61872)、来自皱褶假丝酵母(Candida rugosa)的脂肪酶(登录号 P20261、P32946、P32947、P3294和P32949)、来自雪白根霉(Rhizopus niveus)的脂肪酶(登录号P61871)、来自卡门培尔青霉(Penicillium camemberti)的脂肪酶(登录号P25234)、来自黑曲霉(Aspergillus niger)的脂肪酶(ABG73613、ABG73614和ABG37906)和来自圆弧青霉(Penicillium cyclopium)的脂肪酶(登录号 P61869),以及各自它们在氨基酸水平上至少60%的同源物。
13.根据权利要求9至12中至少一项所述的方法,其特征在于:所述方法步骤B)在小于1bar,优选小于0.5bar,更优选小于0.1bar的压力下进行。
14.根据权利要求9至13中至少一项所述的方法可得的木糖醇羧酸酯。
15.根据权利要求1至8或14所述的至少一种木糖醇羧酸酯的用途,其作为粘度调节剂、护理活性成分、泡沫促进剂或增溶剂、抗微生物剂、抗静电剂、粘合剂、腐蚀抑制剂、分散剂、乳化剂、成膜剂、保湿剂、遮光剂、口腔护理剂、防腐剂、护肤剂、亲水性润肤剂、泡沫稳定剂和非离子表面活性剂,优选作为粘度调节剂、乳化剂、抗微生物剂和亲水性润肤剂,特别优选作为粘度调节剂,尤其是作为增稠剂,尤其是在清洁或护理配制剂中。
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EP19218421.6 | 2019-12-20 | ||
PCT/EP2020/086737 WO2021122972A1 (de) | 2019-12-20 | 2020-12-17 | Xylitol-carbonsäureester und verfahren zu ihrer enzymatischen herstellung |
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CN202080086956.1A Pending CN114787118A (zh) | 2019-12-20 | 2020-12-17 | 木糖醇羧酸酯及其酶促制备方法 |
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JP2023507446A (ja) | 2023-02-22 |
CN114787368A (zh) | 2022-07-22 |
WO2021122972A1 (de) | 2021-06-24 |
WO2021122973A1 (de) | 2021-06-24 |
BR112022011988A2 (pt) | 2022-08-30 |
EP3839052A1 (de) | 2021-06-23 |
JP2023507448A (ja) | 2023-02-22 |
BR112022011457A2 (pt) | 2022-08-23 |
CN114829617A (zh) | 2022-07-29 |
US20230023141A1 (en) | 2023-01-26 |
BR112022011453A2 (pt) | 2022-08-23 |
EP4077698A1 (de) | 2022-10-26 |
JP2023507450A (ja) | 2023-02-22 |
EP4077697A1 (de) | 2022-10-26 |
WO2021122971A1 (de) | 2021-06-24 |
EP4077696A1 (de) | 2022-10-26 |
US20230033620A1 (en) | 2023-02-02 |
US20230055814A1 (en) | 2023-02-23 |
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