Friday, September 18th 2020                           

EBSI Team | Monitoring

17. Benchtop NMR for flow chemistry and bioprocess monitoring

Current team members: Dylan Bouillaud, BenoÎt Charrier, Jonathan Farjon*, Patrick Giraudeau*

Past members: Shrikant Kunjir, Boris Gouilleux

Collaborations (past and present): Olivier Gonçalves (GEPEA, Univ. Nantes), Julien Legros (COBRA, Rouen), Mireia Rodriguez-Zubiri and François-Xavier Felpin (CEISAM, Univ. Nantes)

Benchtop NMR spectrometer dedicated to reaction monitoring and its implementation in an intelligent flow chemistry setting.

NMR is ideally suited for the online, real-time monitoring of (bio)chemical processes, but it can be limited by size, cost and accessibility considerations that make high-field NMR incompatible with the environment where the targeted processes take place, such as fume hoods or production sites. In this context, we are exploring the potential of benchtop NMR for the online monitoring and control of such processes. In order to circumvent the limitations inherent to low magnetic field (low sensitivity and resolution), we are adapting pulse sequences akin to those developed at high field, thanks to state-of-the-art benchtop spectrometers equipped with a gradient coil and including pulse sequence programming capabilities.

In particular, we have implemented solvent suppression and ultrafast 2D NMR pulse sequences suited to flow measurements. In collaboration with synthetic chemistry groups, we explore their potential for the online monitoring of catalytic reactions, and we use such experiments as an online detector in flow chemistry settings, including intelligent flow experiments where the NMR data are analyzed automatically in real time to optimize the reaction. We are also exploring the potential of benchtop NMR for the monitoring of bioprocesses.

Key References:
  • B. Gouilleux, B. Charrier, E. Danieli, J.-N. Dumez, S. Akoka, F.-X. Felpin, M. Rodriguez-Zubiri, P. Giraudeau, Real-time reaction monitoring by ultrafast 2D NMR on a benchtop spectrometer, Analyst, 140, 7854 (2015)
  • B. Gouilleux, B. Charrier, S. Akoka, F.-X. Felpin, M. Rodriguez-Zubiri, P. Giraudeau, Ultrafast 2D NMR on a benchtop spectrometer: Applications and perspectives, Trends Anal. Chem. 83, 65 (2016)
  • B. Gouilleux, S. Akoka, P. Giraudeau, Gradient-based solvent suppression methods on a benchtop spectrometer, Magn. Reson. Chem. 55, 91 (2017)
  • B. Picard, B. Gouilleux, T. Lebleu, J. Maddaluno, I. Chataigner, M. Penhoat, F.X. Felpin, P. Giraudeau, J. Legros, Oxidative Neutralization of Mustard-Gas Simulants in an On-Board Flow Device with In-Line NMR Monitoring, Angew. Chem. Int. Ed. 56, 7568 (2017)
  • D. Bouillaud, J. Farjon, O. Gonçalves, P. Giraudeau, Benchtop NMR for the monitoring of bioprocesses, Magn. Reson. Chem. in press (2019)

  • Supported by: Région Pays de la Loire (Paris scientifiques RésoNantes and AMER-METAL), CNRS (Projet interdisciplinarité RMN-(ME)2-TAL and Projet Emergence ARES-TATION)