High-throughput screening of organic reactions in microdroplets using desorption electrospray ionization mass spectrometry (DESI-MS): hardware and software implementation.,Analytical Methods

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High-throughput screening of organic reactions in microdroplets using desorption electrospray ionization mass spectrometry (DESI-MS): hardware and software implementation.
Analytical Methods ( IF 2.7 ) Pub Date : 2020-07-01 , DOI: 10.1039/d0ay00072h
Tiago Jose P Sobreira ₁ , Larisa Avramova , Botond Szilagyi , David L Logsdon , Bradley P Loren , Zinia Jaman , Ryan T Hilger , Richard S Hosler , Christina R Ferreira , Andy Koswara , David H Thompson , R Graham Cooks , Zoltan K Nagy

Affiliation

This study describes an automated system used for high throughput screening of reaction conditions based on accelerated reactions occurring in small volumes of reagents. Reaction mixtures are prepared in array format using a fluid handling robot and spotted on a flat polytetrafluoroethylene plate at densities up to 6144 per plate. The reaction and analysis steps are performed simultaneously using desorption electrospray ionization (DESI) to release microdroplets containing the reaction mixture from the plate for reaction prior to arrival at a mass spectrometer. Analysis rates are up to 1 reaction mixture per second and data are recorded in real time using an ion trap mass spectrometer. Beacon compounds are used to triangulate position on the plate and this allows tandem mass spectrometry (MS/MS) to be performed on confirm products of interest. Custom software allows the user to control the system. It is also used to receive data from the DESI mass spectrometer to screen the spectra for compounds of interest, to perform MS/MS and to save data. This custom software also communicates with the software controlling the fluid handling robot (Biomek i7) as well as the Beckman software used to prepare reaction mixtures and also the software that controls the solvent used as the DESI spray. Data were recorded for N-alkylation, N-acylation and N-sulfonylation reactions in three 8 hour experiments on successive days to establish the ruggedness and repeatability of the system. Repeatability is high (94–97%) over this period with false negative 6% (depending on noise threshold chosen). Plates containing 384 reaction mixtures are analyzed in 7 min by moving the DESI sprayer in steps under the sprayer instead of continuously.

中文翻译：

使用解吸电喷雾电离质谱（DESI-MS）高通量筛选微滴中的有机反应：硬件和软件实现。

这项研究描述了一种自动系统，该系统可用于基于少量试剂中发生的加速反应的反应条件的高通量筛选。使用流体处理机器人以阵列形式制备反应混合物，并以每块板高达6144的密度点在平坦的聚四氟乙烯板上。使用解吸电喷雾电离（DESI）同时执行反应和分析步骤，以在到达质谱仪之前从板上释放含有反应混合物的微滴以进行反应。分析速率高达每秒1种反应混合物，并使用离子阱质谱仪实时记录数据。信标化合物用于对板上的位置进行三角测量，这使得可以对感兴趣的确认产物进行串联质谱分析（MS / MS）。定制软件允许用户控制系统。它还可用于从DESI质谱仪接收数据，以筛选目标化合物的光谱，执行MS / MS并保存数据。该定制软件还与控制流体处理机器人（Biomek i7）的软件以及用于制备反应混合物的贝克曼软件以及控制用作DESI喷雾剂的溶剂的软件进行通信。记录了数据该定制软件还与控制流体处理机器人（Biomek i7）的软件以及用于制备反应混合物的贝克曼软件以及控制用作DESI喷雾剂的溶剂的软件进行通信。记录了数据该定制软件还与控制流体处理机器人（Biomek i7）的软件以及用于制备反应混合物的贝克曼软件以及控制用作DESI喷雾剂的溶剂的软件进行通信。记录了数据在连续八天的三个8小时实验中，进行N-烷基化，N-酰化和N-磺酰化反应，以建立系统的坚固性和可重复性。在此期间，重复性很高（94–97％），假阴性为6％（取决于所选的噪声阈值）。在7分钟内，通过逐步将DESI喷雾器移至喷雾器下方而不是连续移动来分析包含384种反应混合物的板。

更新日期：2020-07-23

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