Real-Time Reaction Monitoring of an Organic Multistep Reaction by Electrospray Ionization-Ion Mobility Spectrometry.,ChemPlusChem

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Real-Time Reaction Monitoring of an Organic Multistep Reaction by Electrospray Ionization-Ion Mobility Spectrometry.
ChemPlusChem ( IF 3.0 ) Pub Date : 2017-10-01 , DOI: 10.1002/cplu.201700296
Martin Zühlke ₁ , Stephan Sass ₁ , Daniel Riebe ₁ , Toralf Beitz ₁ , Hans-Gerd Löhmannsröben ₁

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The capability of electrospray ionization (ESI)-ion mobility (IM) spectrometry for reaction monitoring is assessed both as a stand-alone real-time technique and in combination with HPLC. A three-step chemical reaction, consisting of a Williamson ether synthesis followed by a hydrogenation and an N-alkylation step, is chosen for demonstration. Intermediates and products are determined with a drift time to mass-per-charge correlation. Addition of an HPLC column to the setup increases the separation power and allows the determination of further species. Monitoring of the intensities of the various species over the reaction time allows the detection of the end of reaction, determination of the rate-limiting step, observation of the system response in discontinuous processes, and optimization of the mass ratios of the starting materials. However, charge competition in ESI influences the quantitative detection of substances in the reaction mixture. Therefore, two different methods are investigated, which allow the quantification and investigation of reaction kinetics. The first method is based on the pre-separation of the compounds on an HPLC column and their subsequent individual detection in the ESI-IM spectrometer. The second method involves an extended calibration procedure, which considers charge competition effects and facilitates nearly real-time quantification.

中文翻译：

通过电喷雾电离-离子迁移谱法实时监测有机多步反应。

电喷雾电离（ESI）离子迁移（IM）光谱用于反应监测的能力既可以通过独立的实时技术进行评估，也可以与HPLC相结合进行评估。选择三步化学反应进行演示，该反应由威廉姆森醚合成，氢化和N-烷基化步骤组成。中间体和产品的确定时间与每次充电质量相关。将HPLC色谱柱添加到设置中可提高分离能力，并可以确定其他种类。监测反应时间内各种物质的强度，可以检测反应的结束，确定限速步骤，观察不连续过程中的系统反应，并优化起始物料的质量比。然而，ESI中的电荷竞争影响反应混合物中物质的定量检测。因此，研究了两种不同的方法，它们允许定量和研究反应动力学。第一种方法是基于化合物在HPLC色谱柱上的预分离以及随后在ESI-IM光谱仪中的单独检测。第二种方法涉及扩展的校准程序，该程序考虑了电荷竞争效应并促进了几乎实时的定量。第一种方法是基于化合物在HPLC色谱柱上的预分离以及随后在ESI-IM光谱仪中的单独检测。第二种方法涉及扩展的校准程序，该程序考虑了电荷竞争效应并促进了几乎实时的定量。第一种方法是基于化合物在HPLC色谱柱上的预分离以及随后在ESI-IM光谱仪中的单独检测。第二种方法涉及扩展的校准程序，该程序考虑了电荷竞争效应并促进了几乎实时的定量。

更新日期：2017-10-13

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