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1. 发明授权

US08603833B2 Germania-silica-based sol-gel monolith and uses thereof 有权
标题翻译：日本 - 二氧化硅基溶胶 - 凝胶整料及其用途
公开(公告)号：US08603833B2
公开(公告)日：2013-12-10
申请号：US13152720
申请日：2011-06-03
申请人： Abdul Malik , Erica B. Turner , Scott S. Segro
发明人： Abdul Malik , Erica B. Turner , Scott S. Segro
IPC分类号： B01D15/26
CPC分类号： B01D15/38 , B01D15/206 , B01J20/0251 , B01J20/103 , B01J20/28047 , B01J20/282 , B01J20/283 , B01J20/285 , B01J20/291 , B01J2220/82 , B01J2220/86 , C07F7/04 , C23C18/1216 , C23C18/122 , C23C18/1254 , C23C18/127 , G01N1/405
摘要： The present invention provides germania-silica-based sol-gel monoliths that form the solid-phase material for extraction, isolation, preconcentration, and separation of analytes. In one embodiment, the germania-silica-based sol-gel monolith can be used to coat surfaces of the inner walls of extraction and chromatographic columns. In a preferred embodiment, the sol-gel germania-silica monolith of the present invention is formed from hydrolysis and polycondensation of precursors comprising tetraethoxygermane, tetramethoxysilane, and polyethylene glycol. Also provided are methods of preparing the germania-silica-based sol-gel monolith of the present invention.
摘要翻译：本发明提供形成分析物的萃取，分离，预浓缩和分离的固相材料的基于锗 - 二氧化硅的溶胶 - 凝胶整料。在一个实施方案中，可以使用基于二氧化硅的溶胶 - 凝胶整料来涂覆萃取层和色谱柱的内壁表面。在一个优选的实施方案中，本发明的溶胶 - 凝胶锗 - 二氧化硅整料由包含四乙氧基锗烷，四甲氧基硅烷和聚乙二醇的前体的水解和缩聚形成。还提供了制备本发明的基于氧化锗 - 二氧化硅的溶胶 - 凝胶整料的方法。

2. 发明申请

US20120004434A1 GERMANIA-SILICA-BASED SOL-GEL MONOLITH AND USES THEREOF 有权
标题翻译：基于硅胶的溶胶凝胶及其用途
公开(公告)号：US20120004434A1
公开(公告)日：2012-01-05
申请号：US13152720
申请日：2011-06-03
申请人： Abdul Malik , Erica B. Turner , Scott S. Segro
发明人： Abdul Malik , Erica B. Turner , Scott S. Segro
IPC分类号： B01D15/38 , B05D5/00 , B01D53/02 , H01J49/00 , C07F7/30 , G01N27/447
CPC分类号： B01D15/38 , B01D15/206 , B01J20/0251 , B01J20/103 , B01J20/28047 , B01J20/282 , B01J20/283 , B01J20/285 , B01J20/291 , B01J2220/82 , B01J2220/86 , C07F7/04 , C23C18/1216 , C23C18/122 , C23C18/1254 , C23C18/127 , G01N1/405
摘要： The present invention provides germania-silica-based sol-gel monoliths that form the solid-phase material for extraction, isolation, preconcentration, and separation of analytes. In one embodiment, the germania-silica-based sol-gel monolith can be used to coat surfaces of the inner walls of extraction and chromatographic columns. In a preferred embodiment, the sol-gel germania-silica monolith of the present invention is formed from hydrolysis and polycondensation of precursors comprising tetraethoxygermane, tetramethoxysilane, and polyethylene glycol. Also provided are methods of preparing the germania-silica-based sol-gel monolith of the present invention.
摘要翻译：本发明提供形成分析物的萃取，分离，预浓缩和分离的固相材料的基于锗 - 二氧化硅的溶胶 - 凝胶整料。在一个实施方案中，可以使用基于二氧化硅的溶胶 - 凝胶整料来涂覆萃取层和色谱柱的内壁表面。在一个优选的实施方案中，本发明的溶胶 - 凝胶锗 - 二氧化硅整料由包含四乙氧基锗烷，四甲氧基硅烷和聚乙二醇的前体的水解和缩聚形成。还提供了制备本发明的基于氧化锗 - 二氧化硅的溶胶 - 凝胶整料的方法。

3. 发明授权

US09528921B2 Materials and methods for capillary microextraction in combination with high-performance liquid chromatography comprising a sol-gel germania triblock polymer 有权
标题翻译：与高效液相色谱组合的毛细管微萃取的材料和方法，其包括溶胶 - 凝胶锗纳三烯聚合物
公开(公告)号：US09528921B2
公开(公告)日：2016-12-27
申请号：US13641640
申请日：2011-04-18
申请人： Abdul Malik , Scott S. Segro
发明人： Abdul Malik , Scott S. Segro
IPC分类号： G01N1/40 , G01N30/08 , B01J20/26 , B01J20/285 , B01J20/286 , G01N30/74
CPC分类号： G01N1/405 , B01J20/262 , B01J20/285 , B01J20/286 , B01J2220/86 , G01N30/08 , G01N30/74 , Y10T436/255 , G01N21/33 , G01N2030/009 , G01N2030/062
摘要： Germania-based sol-gel organic-inorganic hybrid coatings were prepared for on-line coupling of capillary microextraction with high-performance liquid chromatography. A germania-based sol-gel precursor, tetra-n-butoxygermane and a hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), were chemically anchored to the inner walls of a fused silica capillary (0.25 mm I.D.). Scanning electron microscopy images of the sol-gel germania triblock polymer coating were obtained to estimate the coating thickness. The analyte distribution constants between a sol-gel germania organic-inorganic hybrid coating and the samples (Kcs) were determined. For a variety of analytes from different chemical classes, including polycyclic aromatic hydrocarbons (PAHs), ketones, alcohols, phenols, and amines, the Kcs values ranged from 1.8×101 to 2.0×104. The sol-gel germania triblock polymer coatings survived exposure to high temperature solvent conditions (200° C.) with little change in extraction capabilities. Reproducibility of the method for preparation of the sol-gel germania triblock polymer coatings was also evaluated, and the capillary-to-capillary RSD values ranged from 5.3% to 6.5%. The use of higher flow rates in extraction was found to significantly reduce the time required (from 30-40 minutes to 10-15 minutes) to reach equilibrium between the sol-gel germania triblock polymer coating and the analytes in the sample solution.
摘要翻译：制备了基于Germania的溶胶凝胶有机 - 无机杂化涂层，用于毛细管微萃取与高效液相色谱的在线偶联。将基于锗酸盐的溶胶 - 凝胶前体，四正丁氧基锗烷和羟基封端的三嵌段共聚物，聚（环氧乙烷） - 嵌段 - 聚（环氧丙烷） - 嵌段 - 聚（环氧乙烷）化学地锚定到内部熔融石英毛细管的壁（0.25mm ID）。获得溶胶 - 凝胶锗三嵌段聚合物涂层的扫描电子显微镜图像以估计涂层厚度。测定溶胶 - 凝胶锗有机 - 无机杂化涂层和样品（Kcs）之间的分析物分布常数。对于不同化学类别的各种分析物，包括多环芳烃（PAHs），酮类，醇类，酚类和胺类，Kcs值范围为1.8×101〜2.0×104。溶胶 - 凝胶锗三嵌段聚合物涂层在暴露于高温溶剂条件（200℃）下存活，萃取能力几乎没有变化。还评估了溶胶 - 凝胶锗三嵌段聚合物涂层的制备方法的重现性，毛细管与毛细管的RSD值为5.3％至6.5％。发现在提取中使用更高的流速显着地减少了所需的时间（从30-40分钟到10-15分钟）以达到溶胶 - 凝胶锗三嵌段聚合物涂层和样品溶液中分析物之间的平衡。

4. 发明申请

US20130071945A1 MATERIALS AND METHODS FOR CAPILLARY MICROEXTRACTION IN COMBINATION WITH HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 有权
标题翻译：与高性能液相色谱联用的毛细微萃取的材料和方法
公开(公告)号：US20130071945A1
公开(公告)日：2013-03-21
申请号：US13641640
申请日：2011-04-18
申请人： Abdul Malik , Scott S. Segro
发明人： Abdul Malik , Scott S. Segro
IPC分类号： G01N1/40
CPC分类号： G01N1/405 , B01J20/262 , B01J20/285 , B01J20/286 , B01J2220/86 , G01N30/08 , G01N30/74 , Y10T436/255 , G01N21/33 , G01N2030/009 , G01N2030/062
摘要： Germania-based sol-gel organic-inorganic hybrid coatings were prepared for on-line coupling of capillary microextraction with high-performance liquid chromatography. A germania-based sol-gel precursor, tetra-n-butoxygermane and a hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), were chemically anchored to the inner walls of a fused silica capillary (0.25 mm I.D.). Scanning electron microscopy images of the sol-gel germania triblock polymer coating were obtained to estimate the coating thickness. The analyte distribution constants between a sol-gel germania organic-inorganic hybrid coating and the samples (Kcs) were determined. For a variety of analytes from different chemical classes, including polycyclic aromatic hydrocarbons (PAHs), ketones, alcohols, phenols, and amines, the Kcs values ranged from 1.8×101 to 2.0×104. The sol-gel germania triblock polymer coatings survived exposure to high temperature solvent conditions (200° C.) with little change in extraction capabilities. Reproducibility of the method for preparation of the sol-gel germania triblock polymer coatings was also evaluated, and the capillary-to-capillary RSD values ranged from 5.3% to 6.5%. The use of higher flow rates in extraction was found to significantly reduce the time required (from 30-40 minutes to 10-15 minutes) to reach equilibrium between the sol-gel germania triblock polymer coating and the analytes in the sample solution.
摘要翻译：制备了基于Germania的溶胶凝胶有机 - 无机杂化涂层，用于毛细管微萃取与高效液相色谱的在线偶联。将基于锗酸盐的溶胶 - 凝胶前体，四正丁氧基锗烷和羟基封端的三嵌段共聚物，聚（环氧乙烷） - 嵌段 - 聚（环氧丙烷） - 嵌段 - 聚（环氧乙烷）化学地锚定到内部熔融石英毛细管的壁（0.25mm ID）。获得溶胶 - 凝胶锗三嵌段聚合物涂层的扫描电子显微镜图像以估计涂层厚度。测定溶胶 - 凝胶锗有机 - 无机杂化涂层和样品（Kcs）之间的分析物分布常数。对于不同化学类别的各种分析物，包括多环芳烃（PAHs），酮类，醇类，酚类和胺类，Kcs值范围为1.8×101〜2.0×104。溶胶 - 凝胶锗三嵌段聚合物涂层在暴露于高温溶剂条件（200℃）下存活，萃取能力几乎没有变化。还评估了溶胶 - 凝胶锗三嵌段聚合物涂层的制备方法的重现性，毛细管与毛细管的RSD值为5.3％至6.5％。发现在提取中使用更高的流速显着地减少了所需的时间（从30-40分钟到10-15分钟）以达到溶胶 - 凝胶锗三嵌段聚合物涂层和样品溶液中分析物之间的平衡。

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