CN1300207A - 头发调理组合物 - Google Patents
头发调理组合物 Download PDFInfo
- Publication number
- CN1300207A CN1300207A CN99804712.0A CN99804712A CN1300207A CN 1300207 A CN1300207 A CN 1300207A CN 99804712 A CN99804712 A CN 99804712A CN 1300207 A CN1300207 A CN 1300207A
- Authority
- CN
- China
- Prior art keywords
- amino
- compositions
- functional silicone
- siloxanes
- aliphatic alcohol
- Prior art date
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- Granted
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Abstract
一种含水头发调理组合物,其中除了水之外,还包含:i)至少一种调理表面活性剂,和ii)氨基官能硅氧烷的乳化颗粒,其通式为:Si(CH3)3-O-[Si(CH3)2-O-]X-[Si(CH)3)[R-NH-CH2CH2NH2)-O-]Y-Si(CH3)3其中,x+y为数字约50~约500,和R是含有2—5个碳原子的亚烷基基团;其中氨基官能硅氧烷的摩尔百分数氨基官能度为至少1mol%。
Description
发明领域
本发明涉及清洗头发用的头发调理组合物。尤其是,本发明涉及含有氨基官能硅氧烷的乳化颗粒的头发调理组合物,该组合物调理头发使其更柔软和更易于梳理。
背景和现有技术
硅氧烷作为调理剂在化妆品配制物中的应用是众所周知的,广泛记载在专利文献之中。含有氨基官能聚硅氧烷的护理头发的组合物也已见述于一些出版物中。例如,美国专利4,563,347公开了一种氨烷基取代的聚二甲基硅氧烷的水乳液,对护理头发是有用处的,因为它利于梳理头发,并且赋予头发光滑的手感。其它含有氨基官能聚硅氧烷的护理头发的组合物叙述在美国专利4,586,518、美国专利4,601,902和美国专利4,618,819中。氨基官能微乳液在护发领域中也已见述。例如,美国专利4,749,732叙述了采用烷氧基羰基烷基取代基改性的含有氨烷基基团的聚二有机硅氧烷在头发护理中的应用。美国专利4,620,878概括地叙述了含有极性取代基的硅氧烷乳液的制备,以及公开了一种制备胺官能聚有机硅氧烷的透明微乳液的方法,其能够与十二烷基醚硫酸钠洗发剂碱和水混合产生稳定的透明的组合物。
混入氨基官能硅氧烷的调理头发的配方所遇到的问题是,对于许多人来说,所供给的护理性能可能是不足的,尤其是日本和东南亚等地区的人,在那里顾客要求对头发进行高水平的调理,还要求头发具有“重”感。
现在我们发现,在具有限定摩尔百分数的氨基官能度的特定种类的氨基官能硅氧烷的头发调理组合物中的内容物,显著地改善了湿和干调理性能。
发明概述
本发明提供了一种含水头发调理组合物,其中除了水之外,还包含:
ⅰ)至少一种调理表面活性剂,和
ⅱ)氨基官能硅氧烷的乳化颗粒,其通式为:Si(CH3)3-O-[Si(CH3)2-O-]x-[Si(CH3)(R-NH-CH2CH2 NH2)-O-]y-Si(CH3)3其中,x+y为数字约50~约500,和R是含有2-5个碳原子的亚烷基基团;其中氨基官能硅氧烷的摩尔百分数氨基官能度为至少1mol%。
发明详述
调理表面活性剂
按照本发明的组合物包含一种或几种化妆可接受的、适用于头发这一专门应用的调理表面活性剂。
适用的调理表面活性剂选自阳离子表面活性剂,以单一的形式或混合物的形式应用。其例子一般包括氢氧化铵或其盐,例如氯化物。
适用于本发明头发调理组合物的阳离子表面活性剂包括:氯化十六烷基三甲基铵、氯化二十二烷基三甲基铵、氯化十六烷基吡啶鎓、氯化四甲基铵,氯化四乙基铵、氯化辛基三甲基铵、氯化十二烷基三甲基铵、氯化十六烷基三甲基铵、氯化辛基二甲基苄基铵、氯化癸基二甲基苄基铵、氯化十八烷基二甲基苄基铵、氯化二(十二烷基)二甲基铵、氯化二(十八烷基)二甲基铵、氯化牛脂三甲基铵、氯化可可三甲基铵及它们的相应氢氧化物。另外适宜的阳离子表面活性剂包括CTFA命名的那些化合物Quaternium-5、Quaternium-31和Quaternium-18。任何上述物料的混合物也是适用的。特别适用于本发明头发护理剂的阳离子表面活性剂是氯化十六烷基三甲基铵和氯化二十二烷基三甲基铵。
在本发明头发护理组合物中,阳离子表面活性剂的含量优选为0.01~10wt%,更优选为0.05-5wt%最优选为0.1-2wt%,以组合物总重量为基准计。
乳化的氨基官能化的硅氧烷
按照本发明的头发调理组合物包括如下通式的氨基官能化硅氧烷的乳化颗粒:Si(CH3)3-O-[Si(CH3)2-O-]x-[Si(CH3)(R-NH-CH2CH2 NH2)-O-]y-Si(CH3)3其中x+y是数字约50-约500,和其中R是含2-5个碳原子的亚烷基基团。
优选,数字x+y为约100-约300。
氨基官能硅氧烷不溶于头发调理组合物的含水基体,因此其以乳化的形式存在,该硅氧烷以分散颗粒的形式存在。
我们已经发现,适用于本发明的氨基官能硅氧烷需要具有至少1.0mol%摩尔百分数氢基官能度。氨基官能硅氧烷的适宜摩尔百分数氨基官能度为约1-约8.0mol%,优选为约1-约5.0mol%,例如约1.7mol%。
能够得到制造用于本发明的氨基官能硅氧烷颗粒乳液的许多方法,这些方法是众所周知的,并载于本领域文献之中。例如,乳液可以采用硅氧烷和水的高度剪切机械混合进行制备,或者采用水和乳化剂将硅氧烷乳化(例如将硅氧烷混合入加热的乳化剂溶液中)来制备,或者采用机械乳化和化学乳化相结合的方法来制备。另外的适宜制备硅氧烷颗粒乳液的方法是乳液聚合。就乳液聚合的硅氧烷而论叙述在美国专利2 891 820(Hyde)、美国专利3 294 725(Find lay)和美国专利3 360 491(Axon)。
对氨基官能硅氧烷本身(并不是最终头发护理组合物乳液)的粘度没有特别严格的要求,适宜的范围可以是50-500,000cst。粘度可以采用玻璃毛细管粘度计进行测定,按照Dow Corning Corporate试验法CTM 004,1970年7月20日所述实施。
在头发调理组合物中氨基官能硅氧烷的乳化颗粒的平均硅氧烷颗粒粒度优选为20以下,更优选为10微米以下。我们发现减少粒度,一般能改善调理性能。最优选在头发调理组合物中的平均氨基官能硅氧烷的粒度小于2微米,理想的范围为0.01-1微米。平均硅氧烷粒度≤0.15微米的硅氧烷乳液一般称为微乳液。
可以采用激光散射法测定粒度,所用的是自Malvern Instruments的2600D粒度仪。
适用于本发明的氨基官能硅氧烷的具体例子是氨基硅油DC2-8220、DC2-8166、DC2-8466和DC2-8950-114(所有例子均得自DowCorning)和GE 1149-75(如得自General Electric Silicones)。
氨基官能硅油与非离子和/或阳离子表面活性剂的预制乳液也是适宜的。这是特别优选的,因为预制的乳液能够通过简单的混合混合成头发调理组合物。
氨基官能化硅氧烷的预制乳液可以得自硅油供应厂商,如DowCorning、General Electric、Union Carbide、Wacker Chemie、ShinEtsu、Toshiba、Toyo Beauty以及Toray Silicone公司。其例子包括乳液DC2-8320、DC2-8306、DC2-8177和DC2-8467,全部均可得自Dow Corning公司。
任选成分
乳化的非氨基官能化的硅氧烷
本发明的头发调理组合物也可以适当地包含非氨基官能化硅氧烷的乳化颗粒,其不溶于该组合物的含水基体,因此以乳化的形式存在,该硅氧烷以分散的粒子形式存在。
适宜的非氨基官能化的硅氧烷包括聚二有机硅氧烷,特别是聚二甲基硅氧烷,其CTFA命名为聚二甲基硅氧烷。也适用于本发明的头发调理组合物的是含有羟端基的聚二甲基硅氧烷,其CTFA命名为聚二甲基硅氧烷醇。也适用于本发明的头发调理组合物的是具有轻度交联的硅橡胶纯胶料,正如,例如,在WO 96/31188中所述。这些材料能够赋予头发身骨、膨松和发式稳定性以及良好的湿和干调理性能。
乳化的非氨基官能化硅氧烷本身(不是乳液也不是最终头发调理组合物)的粘度一般至少为10,000cst。概括地说,我们发现调理性能随着粘度的增加而增加。所以,该硅氧烷本身的粘度优选为至少60,000cst,最优选为至少500,000cst,理想的是至少1,000,000cst。为了易于配制,优选粘度不超过109cst。
用于本发明头发调理组合物的乳化非氨基官能硅氧烷,在该组合物中的平均硅氧烷粒度一般小于30,优选小于20,更优选小于10微米。我们还发现,粒度减少一般能改善调理性能。最优选在该组合物中的乳化非氨基官能硅烷的平均硅氧烷粒度小于2微米,理想的范围是0.01-1微米。
用于本发明的适宜非氨基官能硅氧烷乳液也能以预乳化的形式从商业渠道得到。
适宜的预制乳液的例子包括乳液DC2-1766、DC2-1784以及微乳液DC2-1865和DC2-1870,全部可得自Dow Corning。所有这些均是聚二甲基硅氧烷醇乳液/微乳液。交联的硅橡胶纯胶料也可以以预乳化的形式得的,其有利于容易地进行配制。优选的例子是得自Dow Corning公司的DCX2-1787物料,它是一种交联的聚二甲基硅氧烷醇胶料的乳液。另外优选的例子是得自Dow Corning的DC X2-1391物料,它是一种交联的聚二甲基硅氧烷醇胶料的微乳液。
混入本发明头发调理组合物的硅氧烷(氨基官能的和非氨基官能的,如果存在的话)的总量,取决于所要求的调理水平和所使用的物料。优选量为总组合物的0.01-约10wt%,但是该限定范围并不是绝对的。其下限由所要求的最低调理水平决定,上限由所要求的最高调理水平决定,以避免产生头发和皮肤不能接受的油腻。
我们发现,适宜的水平是,硅氧烷总量为总组合物的0.3-5wt%,优选0.5-3wt%。
脂族醇
有利的是,本发明头发调理组合物包含脂族醇物料。认为将脂族醇物料和阳离子表面活性剂在调理组合物中混合使用是特别有利的,因为这样能形成层状相,阳离子表面活性剂能分散于其中。
典型的脂族醇包含8-22个碳原子,更优选包含16-20个碳原子。适宜的脂族醇的例子包括十六烷醇、十八烷醇、及其混合物。应用这些物料也是有利的,因为它们对本发明组合物的总调理性能有所贡献。
烷氧基化的(如乙氧基化或丙氧基化的)在烷基链中含有约12-约18个碳原子的脂族醇能够用来代替,或者加入到,脂族醇本身。适宜的例子包括乙二醇十六烷基醚、聚氧乙烯(2)十八烷基醚、聚氧乙烯(24)十六烷基醚、及其混合物。
在本发明调理剂中脂族醇和/或烷氧基化的脂族醇物料的量,合宜的是该组合物的0.01-10wt%,优选为0.1-5wt%。
阳离子表面活性剂与脂族醇和/或烷氧基化的脂族醇的重量比,适宜的是10∶1至1∶10,优选4∶1至1∶8,最佳为1∶1至1∶4。
其它任选成分
本发明组合物可以包含一般在调理头发配方中使用的任何其它成分。这些其它成分可以包括粘度改进剂、防腐剂、着色剂、多元醇如甘油和聚丙二醇、螯合剂如EDTA、抗氧剂、芳香剂及防晒剂。每一种这些成分的存在量以有效达到其目的为准。一般说,这些任选成分的含量,单独地说,最多为总组合物的约5wt%。
优选,本发明的组合物还含有适于护发的辅助试剂。一般说,这些成分的含量,单独地说,最多为总组合物的2wt%,优选最多1wt%。
适于护理头发的辅助剂是:
(ⅰ)头发根天然营养素,如氨基酸和糖。适宜的氨基酸的例子包括精氨酸、半胱氨酸、谷氨酰胺、谷氨酸、异亮氨酸、亮氨酸、蛋氨酸、丝氨酸和缬氨酸,和/或其前体和衍生物。氨基酸可以单独地、或以混合物的形式、或者以缩氨酸的形式加入,例如二缩氨酸和三缩氨酸。氨基酸也可以以蛋白质水解产物的形式加入,如角蛋白或胶原蛋白水解产物。适宜的糖是的葡萄糖、右旋糖和果糖。这些可以单个加入或者以,例如,水果提取液的形式加入。对于本发明组合物的内容物来说,发根的天然营养素的特别优选的组合是异亮氨酸和葡萄糖。特别优选的氨基酸营养素是精氨酸。
(ⅱ)头发纤维护理剂,例子是:
-N-脂酰基鞘氨醇,用来增湿纤维和保持角质层完整性。N-脂酰基鞘氨醇可通过从天然产物中提纯得到,或者以合成N-脂酰基鞘氨醇和假N-脂酰基鞘氨醇的形式得到。所优选的N-脂酰基鞘氨醇是Ceramide(N-脂醛基鞘氨醇)Ⅱ,例如Quest。N-脂酰基鞘氨醇的混合物也是适用的,例如Ceramide(N-脂酰基鞘氨醇)LS,如Lablratoires Serobiologiques。
-脂肪酸,用来修补角质层和防止角质层损坏。例子是支链脂肪酸如18-甲基二十(碳)烷酸和该系列的其它类似物,直链脂肪酸如硬脂酸、肉豆蔻酸、棕榈酸,和不饱和脂肪酸如油酸、亚油酸、亚麻酸和花生四烯酸。所优选的脂肪酸是油酸。脂肪酸可以以单一的形式、以混合物的形式、或者自以诸如羊毛脂之类的提取液的共混物的形式加入。
也可以使用任何上述活性成分的混合物。特别优选的组合是精氨酸和油酸。
现借助于如下非限制性实例进一步举例说明本发明。
实例
头发调理组合物通过混合所述量的下列组分来制备:
成份
%wt
Arquad 16-50 1.4 1.4 1.4
Laurex CS 1.8 5.0 3.1
石蜡 -- -- 1.0
硅氧烷DC-1766 2.5 -- 2.216
硅氧烷DC-8177 3.1 10.0 2.063
Polysurf 67 0.02 -- --
防腐剂 < qs >
香料 0.3 0.3 0.3
Arquad 16-50是50%氯化十六烷基三甲基铵的异丙醇溶液
Laurex CS是十六烷醇和十八烷醇的混合物
Silicone DC-1766是60%聚二甲基硅氧烷醇乳液
Silicone DC-8177是15%的粒度为40nm的三甲基甲硅烷基amodimethicone乳液
Polysurf 67是十六烷基羟乙基纤维素
Claims (8)
1.一种含水头发调理组合物,其中除了水之外,还包含:
ⅰ)至少一种调理表面活性剂,和
ⅱ)氨基官能硅氧烷的乳化颗粒,其通式为:Si(CH3)3-O-[Si(CH3)2-O-]x-[Si(CH3)(R-NH-CH2CH2 NH2)-O-]y-Si(CH3)3其中,x+y为数字约50~约500,和R是含有2-5个碳原子的亚烷基基团;其中氨基官能硅氧烷的摩尔百分数氨基官能度为至少1mol%。
2.按照权利要求1的组合物,其中氨基官能硅氧烷的摩尔百分数氨基官能度为约1-约8.0mol%。
3.按照权利要求1或权利要求2的组合物,其中,在头发护理组合物中的氨基官能硅氧烷的平均粒度为2微米以下。
4.按照任何前述权利要求的组合物,它还包含非氨基官能化的硅氧烷的乳化颗粒。
5.按照权利要求4的组合物,其中,乳化非氨基官能化的硅氧烷本身的粘度为至少60,000cst。
6.按照权利要求4或权利要求5的组合物,其中,在头发护理组合物中的非氨基官能硅氧烷的平均粒度为2微米以下。
7.按照任何上述权利要求的组合物,还包含脂肪醇和/或烷氧基化的脂肪醇。
8.按照权利要求7的组合物,其中,阳离子表面活性剂与脂肪醇和/或烷氧基化的脂肪醇的重量比为1∶1至1∶4。
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---|---|
EP (1) | EP1067899B1 (zh) |
JP (1) | JP2002509868A (zh) |
CN (1) | CN1188101C (zh) |
AR (1) | AR039574A1 (zh) |
AU (1) | AU739034B2 (zh) |
BR (1) | BR9909229A (zh) |
CA (1) | CA2324349A1 (zh) |
ES (1) | ES2377058T3 (zh) |
GB (1) | GB9806826D0 (zh) |
HU (1) | HUP0101855A3 (zh) |
ID (1) | ID26370A (zh) |
IN (1) | IN192725B (zh) |
MX (1) | MXPA00009602A (zh) |
PL (1) | PL343560A1 (zh) |
TR (1) | TR200002797T2 (zh) |
WO (1) | WO1999049836A1 (zh) |
ZA (1) | ZA200005146B (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103648475A (zh) * | 2011-05-12 | 2014-03-19 | 荷兰联合利华有限公司 | 毛发处理组合物 |
Families Citing this family (22)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1088543A1 (en) * | 1999-09-30 | 2001-04-04 | The Procter & Gamble Company | Hair care compositions |
US6808701B2 (en) | 2000-03-21 | 2004-10-26 | Johnson & Johnson Consumer Companies, Inc. | Conditioning compositions |
US6986886B2 (en) | 2000-12-13 | 2006-01-17 | The Procter & Gamble Company | Hair conditioning compositions and their use in hair coloring compositions |
US7056351B2 (en) | 2000-12-13 | 2006-06-06 | The Procter & Gamble Company | Oxidative hair dye composition containing polyakyleneglyco(n)alkylamine and a solid fatty compound |
AU2002312762A1 (en) | 2001-04-06 | 2002-12-09 | Unilever Plc | Hair treatment compositions comprising silicones |
US7211243B2 (en) | 2001-05-14 | 2007-05-01 | The Procter & Gamble Company | Terminal aminofunctional polysiloxane hair conditioning compositions and their use in hair coloring compositions |
GB0209485D0 (en) | 2002-04-25 | 2002-06-05 | Procter & Gamble | Durable fiber treatment composition |
AU2004275713B2 (en) | 2003-09-24 | 2008-03-06 | The Procter & Gamble Company | Conditioning composition comprising aminosilicone |
EP1591102A1 (en) | 2004-04-30 | 2005-11-02 | The Procter & Gamble Company | Process and kit-of-parts for improved hair conditioning after coloring, bleaching or perming |
US20060127345A1 (en) * | 2004-12-10 | 2006-06-15 | Hilvert Jennifer E | Conditioning shampoo containing stabilized silicone particles |
EP1754517A1 (en) | 2005-08-17 | 2007-02-21 | The Procter and Gamble Company | A fiber and hair fiber conditioning treatment composition |
DE102007012908A1 (de) | 2007-03-19 | 2008-09-25 | Momentive Performance Materials Gmbh | Neue Polyamid-Polysiloxan-Verbindungen |
DE102007023869A1 (de) | 2007-05-21 | 2008-12-18 | Momentive Performance Materials Gmbh & Co. Kg | Neue Polycarbonat- und/oder Polyurethan-Polyorganosiloxan-Verbindungen |
DE102007027027A1 (de) | 2007-06-08 | 2008-12-11 | Momentive Performance Materials Gmbh & Co. Kg | Neue Polyharnstoff- und/oder Polyurethan-Polyorganosiloxan-Verbindungen |
DE102007030642A1 (de) | 2007-07-02 | 2009-01-08 | Momentive Performance Materials Gmbh | Verfahren zur Herstellung von Polyorganosiloxanen mit (C6-C60)-Alkylmethylsiloxygruppen und Dimethylsiloxygruppen |
DE102008013584A1 (de) | 2008-03-11 | 2009-09-17 | Momentive Performance Materials Gmbh | Neue Polycarbonat-Polyorganosiloxan- und/oder Polyurethan-Polyorganosiloxan-Verbindungen |
TWI526226B (zh) | 2008-07-10 | 2016-03-21 | 聯合利華公司 | 組合物 |
US20100247474A1 (en) * | 2009-03-25 | 2010-09-30 | Shin-Etsu Chemical Co., Ltd. | Cosmetic hair preparation |
EP2706979B1 (en) | 2011-05-12 | 2018-07-04 | Unilever PLC | Hair treatment compositions |
KR102674231B1 (ko) | 2015-12-21 | 2024-06-11 | 바커 메트로아크 케미컬스 피브이티. 엘티디. | 실리콘 폴리머의 혼합물을 포함하는 에멀젼 및 이의 제조방법 |
BR112021006024A2 (pt) | 2018-10-31 | 2021-06-29 | Unilever Ip Holdings B.V. | composição condicionadora, uso e método de tratamento de cabelos |
US20240189214A1 (en) * | 2022-11-29 | 2024-06-13 | The Procter & Gamble Company | Silicone Mixture for Hair Conditioning |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0152194A2 (en) * | 1984-01-25 | 1985-08-21 | The Procter & Gamble Company | Shampoo compositions |
LU85303A1 (fr) * | 1984-04-13 | 1985-11-27 | Oreal | Composition capillaire et procede de traitement des cheveux |
US4586518A (en) * | 1984-08-06 | 1986-05-06 | Dow Corning Corporation | Hair setting method using aminoalkyl substituted polydiorganosiloxane |
GB2316615A (en) * | 1996-08-29 | 1998-03-04 | R & C Products Pty Ltd | Quaternary ammonium compounds and silicone polymers for hair conditioning |
-
1998
- 1998-03-30 GB GBGB9806826.5A patent/GB9806826D0/en not_active Ceased
-
1999
- 1999-03-17 IN IN192BO1999 patent/IN192725B/en unknown
- 1999-03-22 TR TR2000/02797T patent/TR200002797T2/xx unknown
- 1999-03-22 ID IDW20001940A patent/ID26370A/id unknown
- 1999-03-22 HU HU0101855A patent/HUP0101855A3/hu unknown
- 1999-03-22 PL PL99343560A patent/PL343560A1/xx not_active Application Discontinuation
- 1999-03-22 EP EP99917832A patent/EP1067899B1/en not_active Revoked
- 1999-03-22 BR BR9909229-8A patent/BR9909229A/pt not_active Application Discontinuation
- 1999-03-22 MX MXPA00009602A patent/MXPA00009602A/es active IP Right Grant
- 1999-03-22 CN CNB998047120A patent/CN1188101C/zh not_active Expired - Lifetime
- 1999-03-22 CA CA002324349A patent/CA2324349A1/en not_active Abandoned
- 1999-03-22 JP JP2000540803A patent/JP2002509868A/ja active Pending
- 1999-03-22 AU AU35975/99A patent/AU739034B2/en not_active Ceased
- 1999-03-22 WO PCT/EP1999/001902 patent/WO1999049836A1/en active IP Right Grant
- 1999-03-22 ES ES99917832T patent/ES2377058T3/es not_active Expired - Lifetime
- 1999-03-29 AR ARP990101392A patent/AR039574A1/es active IP Right Grant
-
2000
- 2000-09-26 ZA ZA200005146A patent/ZA200005146B/en unknown
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103648475A (zh) * | 2011-05-12 | 2014-03-19 | 荷兰联合利华有限公司 | 毛发处理组合物 |
Also Published As
Publication number | Publication date |
---|---|
EP1067899B1 (en) | 2012-01-11 |
ID26370A (id) | 2000-12-14 |
AR039574A1 (es) | 2005-03-02 |
TR200002797T2 (tr) | 2001-01-22 |
MXPA00009602A (es) | 2002-08-06 |
HUP0101855A2 (hu) | 2001-10-28 |
HUP0101855A3 (en) | 2003-04-28 |
AU3597599A (en) | 1999-10-18 |
IN192725B (zh) | 2004-05-15 |
EP1067899A1 (en) | 2001-01-17 |
JP2002509868A (ja) | 2002-04-02 |
PL343560A1 (en) | 2001-08-27 |
ZA200005146B (en) | 2001-09-26 |
AU739034B2 (en) | 2001-10-04 |
ES2377058T3 (es) | 2012-03-22 |
WO1999049836A1 (en) | 1999-10-07 |
CN1188101C (zh) | 2005-02-09 |
BR9909229A (pt) | 2001-09-04 |
CA2324349A1 (en) | 1999-10-07 |
GB9806826D0 (en) | 1998-05-27 |
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