Department of Chemistry, Stanford University , Stanford, California 94305, United States.
Department of Chemistry-BMC, Uppsala University , SE-75124 Uppsala, Sweden.
Anal Chem. 2016 Jun 21;88(12):6195-8. doi: 10.1021/acs.analchem.6b01246. Epub 2016 Jun 8.
We developed a technique to monitor spatially confined surface reactions with mass spectrometry under ambient conditions, without the need for voltage or organic solvents. Fused-silica capillaries immersed in an aqueous solution, positioned in close proximity to each other and the functionalized surface, created a laminar flow junction with a resulting reaction volume of ∼5 pL. The setup was operated with a syringe pump, delivering reagents to the surface through a fused-silica capillary. The other fused-silica capillary was connected to a Venturi easy ambient sonic-spray ionization source, sampling the resulting analytes at a slightly higher flow rate compared to the feeding capillary. The combined effects of the inflow and outflow maintains a chemical microenvironment, where the rate of advective transport overcomes diffusion. We show proof-of-concept where acetylcholinesterase was immobilized on an organosiloxane polymer through electrostatic interactions. The hydrolysis of acetylcholine by acetylcholinesterase into choline was monitored in real-time for a range of acetylcholine concentrations, fused-silica capillary geometries, and operating flow rates. Higher reaction rates and conversion yields were observed with increasing acetylcholine concentrations, as would be expected.
我们开发了一种在环境条件下使用质谱监测空间受限表面反应的技术,无需施加电压或使用有机溶剂。浸没在水溶液中的熔融石英毛细管彼此靠近并与功能化表面一起形成层流结,其反应体积约为 5 pL。该装置通过注射器泵操作,通过熔融石英毛细管将试剂输送到表面。另一个熔融石英毛细管连接到文丘里易环境超声喷雾电离源,与进料毛细管相比,以稍高的流速对得到的分析物进行采样。流入和流出的综合作用维持了化学微环境,其中平流输送的速率超过了扩散。我们通过静电相互作用将乙酰胆碱酯酶固定在有机硅氧烷聚合物上来证明其概念。实时监测了乙酰胆碱酯酶将乙酰胆碱水解成胆碱的过程,研究了一系列乙酰胆碱浓度、熔融石英毛细管几何形状和操作流速下的水解反应。随着乙酰胆碱浓度的增加,反应速率和转化率均升高,这是预期的结果。