Shape-selective separation of polycyclic aromatic hydrocarbons on protoporphyrin-silica phases. Effect of surface porphyrin distribution on column efficiency.
Shape-selective separation of polycyclic aromatic hydrocarbons on protoporphyrin-silica phases. Effect of surface porphyrin distribution on column efficiency.
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原卟啉-二氧化硅相上多环芳烃的择形分离。
DOI：
10.1016/s0021-9673(99)00840-7
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发表时间：
1999
期刊：
影响因子：
--
通讯作者：
M. Meyerhoff
中科院分区：
文献类型：
--
作者：
S. Chen;U. Ruedel;M. Meyerhoff
考察了采用不同的卟啉固定化方案制备的各种金属原卟啉-二氧化硅(MProP-SiO_2)填充材料的色谱性能。多环芳烃(PAHs)择形分离的柱效率和溶质分离度可以通过制备具有更低的卟啉覆盖率和更均匀的表面卟啉物种分布的相来显著提高。后者是通过在这一初步反应步骤中混合惰性的甲基三甲氧基硅烷和3-氨丙基三乙氧基硅烷来扩展/稀释二氧化硅表面上的氨丙基反应中心数量来实现的。随后通过酰胺键将支撑物共价连接到侧胺位置，导致卟啉在表面上的分布更加均匀。使用谱带形状和保留时间作为注入溶质浓度的函数，以及对多环芳烃的各种测试混合物(包括标准参考物质SRM 869)的高效液相色谱分离，以确认这些所谓的“扩散”相的增强性能。通过氧化还原/紫外-可见吸收光谱的耦合方法进一步探讨了固定化的卟啉在二氧化硅表面分布的性质的变化，结果表明以聚集体的形式固定在二氧化硅表面的支撑物种类减少了。
The chromatographic performance of various metalloprotoporphyrin-silica (MProP-silica) packing materials prepared using different porphyrin immobilization schemes is examined. Column efficiency and solute resolution for the shape-selective separation of polycyclic aromatic hydrocarbons (PAHs) can be improved significantly by preparing phases with lower porphyrin coverages and with a more homogeneous distribution of the porphyrin species on the surface. The latter is accomplished by spreading/diluting the number of aminopropyl reactive sites on the silica surface via mixing an inert methyltrimethoxysilane with 3-aminopropyltriethoxysilane during this preliminary reaction step. Subsequent covalent attachment of the ProP via amide bonds to the pendant amine sites results in a more even distribution of the porphyrins on the surface. Band shapes and retention times as a function of injected solute concentration as well as HPLC separation of various test mixtures of PAHs (including standard reference material SRM 869) are used to confirm the enhanced performance of these so-called “spread” phases. Changes in the nature of the immobilized porphyrin distribution on the silica surface are further probed by a coupled redox/UV–Vis absorbance method, and results suggest a decrease in the number of ProP species immobilized as aggregates on the surface.
影响因子：
7.4
作者：
KIBBEY, CE;MEYERHOFF, ME
通讯作者：
MEYERHOFF, ME
化学改性二氧化硅动态流动相条件下的电子自旋共振研究。
DOI：
10.1016/s0021-9673(00)90569-7
发表时间：
1988
期刊：
Journal of chromatography
影响因子：
--
作者：
Miller,C;Dadoo,R;Kooser,RG;Gorse,J
通讯作者：
Gorse,J