Novel 3-hydroxypropyl-bonded phase by direct hydrosilylation of allyl alcohol on amorphous hydride silica.
Novel 3-hydroxypropyl-bonded phase by direct hydrosilylation of allyl alcohol on amorphous hydride silica.
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通过烯丙醇在无定形氢化物二氧化硅上直接氢化硅烷化得到新型 3-羟丙基键合相。
DOI：
10.1002/elps.201400216
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发表时间：
2014
期刊：
影响因子：
2.9
通讯作者：
Sandoval,JuniorE
中科院分区：
文献类型：
--
作者：
Gómez,JorgeE;Navarro,FabiánH;Sandoval,JuniorE
在铂(0)-二乙烯基四甲基二硅氧烷（Karstedt的催化剂）存在下，烯丙醇在氢化二氧化硅中间体上进行硅氢化反应，制备了一种新型的3 -羟丙基（丙醇）键合二氧化硅相。该合成方法的区域选择性已被先前的报道正确预测，这些报道涉及到八甲基硅氧烷（二甲基硅氧烷）八硅氧烷（Q8M8H）和氢硅氧烷（T8H8）作为氢化无定形二氧化硅的分子类似物。因此，C‐硅基化比O‐硅基化占主导地位（约94%），并且在这项工作中通常获得了高的丙醇基团表面覆盖率（5±1 μmol/m2）。丙醇键合相通过光谱（红外（IR）和固体核磁共振在硅微粒上）、接触角（在熔融硅晶圆上）和CE（在熔融硅管上）技术进行了表征。用CE研究了吡啶、咖啡因、Tris（2,2′-联吡啶）Ru（II）氯和溶菌酶在丙醇修饰的毛细血管上的迁移行为。比较了这些硅醇敏感溶质在未改性和氢化物改性管上的吸附性能。研究发现，固定丙醇部分下面的SiH物质的水解主要导致与碱性溶质在pH 4下发生强烈的离子交换相互作用，特别是与溶菌酶的相互作用。有趣的是，与水接触角和电渗透迁移率数据一致，缓冲液暴露（水解）氢化物表面上的硅醇-探针相互作用与原始未修饰管的相互作用大不相同。
A novel 3‐hydroxypropyl (propanol)‐bonded silica phase has been prepared by hydrosilylation of allyl alcohol on a hydride silica intermediate, in the presence of platinum (0)‐divinyltetramethyldisiloxane (Karstedt's catalyst). The regio‐selectivity of this synthetic approach had been correctly predicted by previous reports involving octakis(dimethylsiloxy)octasilsesquioxane (Q8M8H) and hydrogen silsesquioxane (T8H8), as molecular analogs of hydride amorphous silica. Thus, C‐silylation predominated (∼94%) over O‐silylation, and high surface coverages of propanol groups (5 ± 1 μmol/m2) were typically obtained in this work. The propanol‐bonded phase was characterized by spectroscopic (infrared (IR) and solid‐state NMR on silica microparticles), contact angle (on fused‐silica wafers) and CE (on fused‐silica tubes) techniques. CE studies of the migration behavior of pyridine, caffeine, Tris(2,2′‐bipyridine)Ru(II) chloride and lysozyme on propanol‐modified capillaries were carried out. The adsorption properties of these select silanol‐sensitive solutes were compared to those on the unmodified and hydride‐modified tubes. It was found that hydrolysis of the SiH species underlying the immobilized propanol moieties leads mainly to strong ion‐exchange‐based interactions with the basic solutes at pH 4, particularly with lysozyme. Interestingly, and in agreement with water contact angle and electroosmotic mobility figures, the silanol–probe interactions on the buffer‐exposed (hydrolyzed) hydride surface are quite different from those of the original unmodified tube.
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影响因子：
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作者：
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影响因子：
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作者：
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影响因子：
4.8
作者：
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通讯作者：
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DOI：
--
发表时间：
1985
期刊：
影响因子：
--
作者：
P. Winichagoon;S. Fucharoen;D. Weatherall;P. Wasi
通讯作者：
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DOI：
10.1073/pnas.81.9.2821
发表时间：
1984-01-01
期刊：
PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA-BIOLOGICAL SCIENCES
影响因子：
--
作者：
CHENG, TC;ORKIN, SH;KAZAZIAN, HH
通讯作者：
KAZAZIAN, HH