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    • 1. 发明授权
    • Basic aluminum antiperspirant active materials having enhanced activity,
antiperspirant active compositions containing such materials, and
methods for preparation of such materials and compositions
    • 具有增强活性的碱性铝止汗剂活性物质,含有这些材料的止汗活性组合物,以及制备这种材料和组合物的方法
    • US5624665A
    • 1997-04-29
    • US456482
    • 1995-06-01
    • Morton L. BarrPaul J. VincentiElaine L. Vanderhoof
    • Morton L. BarrPaul J. VincentiElaine L. Vanderhoof
    • A61K8/19A61K8/26A61K8/28A61K8/29A61K8/44A61Q15/00C01B11/14C01B11/18C01B11/22C01F7/00C01F7/48C01F7/66A61K7/38A61K7/32
    • C01F7/66A61K8/19A61K8/26A61K8/28A61K8/29A61K8/44A61Q15/00C01B11/14C01B11/18C01B11/22C01F7/002C01F7/48A61K2800/58C01P2002/86C01P2002/87
    • Disclosed are basic aluminum antiperspirant materials having univalent complex oxoanions (e.g., nitrate); methods of making such materials; antiperspirant compositions containing such basic aluminum materials, another antiperspirant active material (e.g., a basic zirconium halide salt), and optionally a neutral amino acid: and methods of making such compositions. Size exclusion high performance liquid chromatography chromatograms of the disclosed basic aluminum materials have a peak 4 relative area of at least 25%, a peak 3 relative area of less than 60%, the sum of the peaks 3 and 4 being at least 50%; and less than 10% of the chromatographic peaks eluting at peaks 1 and 2. The disclosed basic aluminum materials have less than 25% of the aluminum in the form of Al.sup.b polyhydroxyaquoaluminum, and have a .sup.27 Al NMR spectrum in which the area of the 71.5-73.5 ppm resonance line includes more than 50% of the combined areas of the 62.5-63.5 ppm and 71.5-73.5 ppm resonance lines, and 5%-30% of the total area under the spectrum from 140 ppm to -80 ppm is contained in the resonance line at 71.5-73.5 ppm. The basic aluminum material of the present invention can be produced by adding a stoichiometric or near-stoichiometric amount of aluminum metal to a solution of an aluminum salt having a univalent complex oxoanion; the basic aluminum material can also be made by adding to such solution of the aluminum salt, aluminum metal having, in total, a relatively small surface area (large-sized particles of aluminum).
    • 公开了具有单价复合氧代阴离子(例如硝酸盐)的碱性止汗剂材料; 制作这种材料的方法; 含有这种碱性铝材料的止汗组合物,另一种止汗剂活性物质(例如碱性卤化锆盐)和任选的中性氨基酸:以及制备这种组合物的方法。 所公开的碱性铝材料的尺寸排阻高效液相色谱色谱图具有至少25%的峰4相对面积,峰3相对面积小于60%,峰3和4的总和至少为50%; 并且在峰1和2处洗脱的色谱峰小于10%。所公开的碱性铝材料具有少于25%的Alb聚羟基铝形式的铝,并且具有27Al NMR谱,其中71.5- 73.5ppm共振线包括62.5-63.5ppm和71.5-73.5ppm共振线的组合面积的50%以上,并且在140ppm至-80ppm的光谱范围内的总面积的5%-30%包含在 共振线为71.5-73.5ppm。 本发明的碱性铝材料可以通过将化学计量或近化学计量的铝金属加入到具有一价复合氧阴离子的铝盐溶液中来制备; 碱性铝材料也可以通过向铝盐,总共具有相对小的表面积(大尺寸的铝颗粒)的铝金属溶液中加入来制备。
    • 2. 发明授权
    • Basic aluminum antiperspirant active materials having enhanced activity,
antiperspirant active compositions containing such materials, and
methods for preparation of such materials and compositions
    • 具有增强活性的碱性铝止汗剂活性物质,含有这些材料的止汗活性组合物,以及制备这种材料和组合物的方法
    • US5595729A
    • 1997-01-21
    • US97620
    • 1993-07-27
    • Morton L. BarrPaul J. VincentiElaine L. Vanderhoof
    • Morton L. BarrPaul J. VincentiElaine L. Vanderhoof
    • A61K8/19A61K8/26A61K8/28A61K8/29A61K8/44A61Q15/00C01B11/14C01B11/18C01B11/22C01F7/00C01F7/48C01F7/66A61K7/38
    • C01F7/66A61K8/19A61K8/26A61K8/28A61K8/29A61K8/44A61Q15/00C01B11/14C01B11/18C01B11/22C01F7/002C01F7/48A61K2800/58C01P2002/86C01P2002/87
    • Disclosed are basic aluminum antiperspirant materials having univalent complex oxoanions (e.g., nitrate); methods of making such materials; antiperspirant compositions containing such basic aluminum materials, another antiperspirant active material (e.g., a basic zirconium halide salt), and optionally a neutral amino acid; and methods of making such compositions. Size exclusion high performance liquid chromatography chromatograms of the disclosed basic aluminum materials have a peak 4 relative area of at least 25%, a peak 3 relative area of less than 60%, the sum of the peaks 3 and 4 being at least 50%; and less than 10% of the chromatographic peaks eluting at peaks 1 and 2. The disclosed basic aluminum materials have less than 25% of the aluminum in the form of Al.sup.b polyhydroxyaquoaluminum, and have a .sup.27 Al NMR spectrum in which the area of the 71.5-73.5 ppm resonance line includes more than 50% of the combined areas of the 62.5-63.5 ppm and 71.5-73.5 ppm resonance lines, and 5%-30% of the total area under the spectrum from 140 ppm to -80 ppm is contained in the resonance line at 71.5-73.5 ppm. The basic aluminum material of the present invention can be produced by adding a stoichiometric or near-stoichiometric amount of aluminum metal to a solution of an aluminum salt having a univalent complex oxoanion; the basic aluminum material can also be made by adding to such solution of the aluminum salt, aluminum metal having, in total, a relatively small surface area (large-sized particles of aluminum).
    • 公开了具有单价复合氧代阴离子(例如硝酸盐)的碱性止汗剂材料; 制作这种材料的方法; 含有这种碱性铝材料的止汗组合物,另一种止汗剂活性物质(例如碱性卤化锆盐)和任选的中性氨基酸; 以及制备这种组合物的方法。 所公开的碱性铝材料的尺寸排阻高效液相色谱色谱图具有至少25%的峰4相对面积,峰3相对面积小于60%,峰3和4的总和至少为50%; 并且在峰1和2处洗脱的色谱峰小于10%。所公开的碱性铝材料具有少于25%的Alb聚羟基铝形式的铝,并且具有27Al NMR谱,其中71.5- 73.5ppm共振线包括62.5-63.5ppm和71.5-73.5ppm共振线的组合面积的50%以上,并且在140ppm至-80ppm的光谱范围内的总面积的5%-30%包含在 共振线为71.5-73.5ppm。 本发明的碱性铝材料可以通过将化学计量或近化学计量的铝金属加入到具有一价复合氧阴离子的铝盐溶液中来制备; 碱性铝材料也可以通过向铝盐,总共具有相对小的表面积(大尺寸的铝颗粒)的铝金属溶液中加入来制备。
    • 8. 发明授权
    • Basic aluminum antiperspirant active material having enhanced activity,
antiperspirant active composition containing such material, and methods
for preparation of such material and composition
    • 具有增强活性的碱性止汗剂活性物质,含有这种物质的止汗活性组合物,以及制备这种物质和组合物的方法
    • US5348720A
    • 1994-09-20
    • US21136
    • 1993-02-23
    • Paul J. VincentiMorton L. Barr
    • Paul J. VincentiMorton L. Barr
    • A61K8/19A61K8/26A61K8/28A61K8/29A61K8/44A61Q15/00C01B11/14C01B11/18C01B11/22C01F7/48C01F7/56C01F7/66C01B9/02
    • C01F7/66A61K8/19A61K8/26A61K8/28A61K8/29A61K8/44A61Q15/00C01B11/14C01B11/18C01B11/22C01F7/48A61K2800/58
    • Disclosed is a basic aluminum material having enhanced antiperspirant activity, the material having the empirical formula Al.sub.2 (OH).sub.6-a X.sub.a, where 0.5.ltoreq.a.ltoreq.5.0, and X is a univalent complex oxoanion of nitrogen, chlorine and other halogens, which forms salts with Al.sup.3+ in aqueous solution so that these salts are essentially completely dissociated, which is readily soluble in water with metallic ions in the solution, and which forms conjugate acids that are strong acids; and wherein the material is characterized by:(a) size exclusion high performance liquid chromatography peaks corresponding to peak 3 and peak 4 of size exclusion chromatograms formed by HPLC technique;(b) a peak 4 relative area of at least 25%, a peak 3 relative area of less than 60%, the sum of the relative peak 3 and peak 4 areas being at least 50%; and(c) less than 10% chromatographic peaks eluting at shorter retention times than peak 3, corresponding to peaks 1 and 2.Illustratively, the univalent oxoanion can be ClO.sub.3.sup.-, ClO.sub.4.sup.-, IO.sub.4.sup.-, and preferably NO.sub.3.sup.-. The material is characterized by having at least 25% by weight thereof in the form of Al.sup.b polyhydroxyaquoaluminum species. Also disclosed are antiperspirant compositions including the basic aluminum material, a zirconium, hafnium, titanium and/or tin antiperspirant active material and a neutral amino acid, and methods of forming the basic aluminum material and the antiperspirant composition. The basic aluminum material can be formed at relatively low temperature, without first forming a dilute solution of a basic aluminum compound, and the basic aluminum material has a stable enhanced activity in aqueous solution over a relatively long period of time.
    • 公开了具有增强的止汗活性的碱性铝材料,该材料具有经验式Al 2(OH)6-aXa,其中0.5≤a≤5.0,X是氮,氯和其它卤素的一价复合氧阴离子 ,其在水溶液中与Al 3+形成盐,使得这些盐基本上完全解离,其易溶于溶液中的金属离子的水中,并且形成作为强酸的共轭酸; 并且其中所述材料的特征在于:(a)尺寸排除高效液相色谱峰对应于通过HPLC技术形成的尺寸排阻色谱图的峰3和峰4; (b)峰值4相对面积为至少25%,峰3相对面积小于60%,相对峰3和峰4面积之和为至少50%; 和(c)相对于峰1和2,在比峰3更短的保留时间洗脱的少于10%的色谱峰。说明性地,单价氧阴离子可以是ClO 3 - ,ClO 4 - ,I 4 - ,优选NO 3 - 。 该材料的特征在于其具有至少25重量%的Alb聚羟基铝的形式。 还公开了包含碱性铝材料,锆,铪,钛和/或锡止汗剂活性物质和中性氨基酸的止汗组合物,以及形成碱性铝材料和止汗组合物的方法。 碱性铝材料可以在相对低的温度下形成,而不首先形成碱性铝化合物的稀释溶液,并且碱性铝材料在相对长的时间内在水溶液中具有稳定的增强的活性。