NMR spectrometer case study

18th December 2017

Boris Gouilleux (left) and engineer Benoît Charrier with their Magritek Spinsolve benchtop NMR spectrometer

Magritek, a leading provider of compact NMR and MRI instruments, reports on the research & development work of Professor Patrick Giraudeau and his group at the University of Nantes. The Faculty of Science & Technology has applied Magritek's benchtop NMR spectrometers to produce enhanced analytical capabilities including the introduction of pulse sequence developments to enable the implementation of ultrafast quantitative 2D NMR. 

Patrick Giraudeau is a professor in the Faculty of Science & Technology at the University of Nantes located in the Loire Valley in Upper Brittany, western France. His research group deals with the development of liquid-state NMR methods for accurate and precise quantitative analysis. Their methods encompass a broad range of application fields, from metabolomics to reaction monitoring. The development of tailored NMR pulse sequences is required as the central tool and the group has contributed to the field with a few success stories. Among these is the development of ultrafast 2D NMR, an approach that, although they did not invent, was improved and developed by them to make it a useful tool for analytical chemistry. 

Their main focus is quantitative analysis and using NMR for its ability to quantify multiple chemical species in complex mixtures with a high accuracy and non-destructively. But why pick NMR? Professor Giraudeau explains: "My real motivation for NMR is that I fell in love with it when I was a Masters student and this has not changed in the last 15 years! I am having more fun with NMR than I could have with any other technique: it is at the interface between physics, chemistry and biology; it has applications in all the fields of science, and it makes you play with so many different concepts!

"We are big users of high-field NMR spectroscopy; these spectrometers are characterised by fantastic resolution and sensitivity, but also by a very high price and size requiring dedicated rooms and specialised staff. When benchtop spectrometers emerged on the market (I remember seeing my first Magritek Spinsolve at SMASH in Santiago de Compostela in 2013), I had the intuition that it would be interesting to explore their potential for method development. This was challenging because benchtop spectrometers were initially designed for teaching and routine research use. We were having quite a lot of success with ultrafast 2D NMR at high field at this time, so we went to talk with several manufacturers of benchtop spectrometers to see if any would be willing to sell us a version of their equipment that would be adapted to pulse sequence operation so that we could implement ultrafast 2D NMR on it. We needed a gradient coil (which had not been done on a benchtop equipment at this time) and we needed to have access to the programming interface of the spectrometer. Magritek was convinced, and they sold us the very first benchtop NMR spectrometer in the world equipped with a gradient coil.

"Since we received our Spinsolve in 2015, we have enjoyed great success. I had an exceptional PhD student working on the system (Boris Gouilleux), as well as a very efficient engineer (Benoît Charrier). In just a few weeks, they managed to implement ultrafast 2D NMR on the Spinsolve. This was really impressive as ultrafast 2D NMR is one of the most demanding methods to implement. Boris also developed several solvent suppression methods, all of which have paved the way to new applications for the Spinsolve. These demonstrated the exceptional technical performance and versatility of Spinsolve, results that were actually far beyond our initial hopes when we started this project. We are now able to tackle applications in the field of reaction monitoring, flow chemistry and food authentication. These are reported in a number of publications. Overall, the important point is that we showed that high-field NMR methods could be implemented on a benchtop spectrometer thus magnifying its performance. I believe that these developments and initial applications will open opportunities for bringing the Spinsolve into environments that are not compatible with high field systems. This is the case with reaction or process monitoring under a fume hood in the lab. It will also be used for quality control in the food industry.

"This is only the beginning of a long story, since we are now buying a second Spinsolve system to explore the potential of benchtop NMR spectroscopy in the monitoring of bioprocesses."


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