Physique de la Matière Condensée, Ecole Polytechnique, CNRS, 91128 Palaiseau, France.
Langmuir. 2010 Jan 19;26(2):809-14. doi: 10.1021/la902220a.
Infrared spectroscopy is used to investigate the transformation of carboxyl-terminated alkyl chains immobilized on a surface into succinimidyl ester-terminated chains by reaction with an aqueous solution of N-ethyl-N'-(3-(dimethylamino)propyl)carbodiimide (EDC) and N-hydroxysuccinimide (NHS). The acid chains are covalently grafted at the surface of hydrogenated porous silicon whose large specific surface area allows for assessing the activation yield in a semiquantitative way by infrared (IR) spectroscopy and detecting trace amounts of surface products and/or reaction products of small IR cross section. In this way, we rationalize the different reaction paths and optimize the reaction conditions to obtain as pure as possible succinimidyl ester-terminated surfaces. A diagram mapping the surface composition after activation was constructed by systematically varying the solution composition. Results are accounted for by NHS surface adsorption and a kinetic competition between the various EDC-induced surface reactions.
红外光谱用于研究通过与 N-乙基-N'-(3-(二甲基氨基)丙基)碳二亚胺 (EDC) 和 N-羟基琥珀酰亚胺 (NHS) 的水溶液反应,将固定在表面上的羧基末端烷基链转化为琥珀酰亚胺酯末端链的过程。这些酸链通过氢化多孔硅的表面共价接枝,其大的比表面积允许通过红外(IR)光谱以半定量的方式评估活化产率,并检测痕量的表面产物和/或小的 IR 横截面积的反应产物。通过这种方式,我们可以合理化不同的反应途径并优化反应条件,以获得尽可能纯的琥珀酰亚胺酯末端表面。通过系统地改变溶液组成,构建了一个表示活化后表面组成的图谱。结果可以通过 NHS 表面吸附和各种 EDC 诱导的表面反应之间的动力学竞争来解释。