Quantitative Perspective on Online Flow Reaction Profiling Using a Miniature Mass Spectrometer,Organic Process Research & Development

当前位置： X-MOL 学术 › Org. Process Res. Dev. › 论文详情

Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)

Quantitative Perspective on Online Flow Reaction Profiling Using a Miniature Mass Spectrometer
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2020-11-10 , DOI: 10.1021/acs.oprd.0c00294
Huaming Sheng ₁ , Emily B. Corcoran ₂ , Zachary E. X. Dance ₃ , Joseph P. Smith ₃ , Zhihao Lin ₄ , Victoria Ordsmith ₅ , Simon Hamilton ₃ , Ping Zhuang ₃

Affiliation

Online mass spectrometry has proven to be a useful tool for characterizing many aspects of chemical reactions. However, to the best of the authors’ knowledge, no reference standard (RS) quantitation approach has been applied in online MS profiling work to date. In this study, we present a RS approach for online quantitation of an aerobic oxidation reaction in flow using a miniature mass spectrometer, with both internal RS and external RS quantitation approaches being evaluated. Quinoline, a structurally similar and chemically inert compound under these reaction conditions, was chosen as the RS to quantify the pyridine aldehyde product. To investigate the optimal RS concentration and instrument attenuation, calibration curves were established by plotting the product/RS peak intensity ratio against the theoretical product yield at different attenuation (dilution factor) values. The MS quantitation results for the actual flow reactions were validated with conventional offline ¹H NMR analysis.

中文翻译：

使用微型质谱仪进行在线流动反应分析的定量观点

在线质谱已被证明是表征化学反应许多方面的有用工具。但是，据作者所知，迄今为止，在线MS分析工作尚未采用参考标准（RS）定量方法。在这项研究中，我们提出了一种使用微型质谱仪在线定量分析流动性好氧氧化反应的RS方法，同时评估了内部RS和外部RS定量方法。选择喹啉（在这些反应条件下在结构上相似且化学惰性的化合物）作为RS定量吡啶醛产物。为了研究最佳的RS浓度和仪器衰减，通过绘制在不同衰减（稀释因子）值下产物/ RS峰强度比与理论产物产率之间的关系来建立校正曲线。使用常规离线方法验证了实际流动反应的质谱定量结果¹ H NMR分析。

更新日期：2020-11-21

点击分享查看原文

点击收藏

阅读更多本刊最新论文本刊介绍/投稿指南11