Simultaneous Online Monitoring of Multiple Reactions Using a Miniature Mass Spectrometer.

Advances in chemical sampling using miniature mass spectrometer technology are used to monitor slow reactions at a frequency of ca. 180 h-1 (on the Mini 12) with no sample carryover and with inline derivatization in the case of poorly ionizing compounds. Moreover, we demonstrate high reproducibility with a relative error of less than 10% for major components. Monitoring is enabled using a continuous-flow nanoelectrospray (CF-nESI) probe contained in a custom-built 3D-printed rotary holder. The holder position is automatically set using a stepper motor controlled by a microcontroller. Reaction progress of up to six reactions, including hydrazone formation and Katritzky transamination, can be monitored simultaneously without carryover for several hours.