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Mechanochemistry: a unique opportunity for oxygen isotopic labelling and NMR spectroscopy

Periodic Reporting for period 3 - MISOTOP (Mechanochemistry: a unique opportunity for oxygen isotopic labelling and NMR spectroscopy)

Período documentado: 2021-10-01 hasta 2023-03-31

Oxygen is everywhere. In mass, it is the most abundant element on Earth and the 3rd most abundant in the Universe. It is a major component of both living organisms and inert matter, and is present in all states of matter (solid, liquid or gas).
At the atomic scale, oxygen can be found in many different bonding environments. Yet, the details on how it binds to other atoms are still not fully understood, and there are many molecules and materials in which its local environment is still unknown. This is an obstacle which needs to be overcome, so that we can to develop a more complete understanding of the structure and properties of a variety of systems around us (whether living or inert). For example, it could help us learn more about the structure of bone, and thereby help develop more efficient treatments for bone repair and regeneration.

The overall purpose of this project is thus to develop new tools for studying the local viscinity of oxygen in molecules in materials, which can be readily used by a wide community of chemists.
Information on the local viscinity of oxygen in molecules and materials can be obtained by looking at one of its stable isotopes (oxygen-17), which can be "manipulated" using magnetic fields. This technique is called "nuclear magnetic resonance" (NMR). However, because oxygen-17 is poorly abundant on Earth (representing only ~ 0.04% of all oxygen atoms), it is very difficult to detect.

To counter this issue, since the beginning of the project, we have been working on the development of new rapid, user-friendly and low-cost protocols for enriching in oxygen-17 a wide variety of organic molecules (including fatty acids like oleic acid) and minerals (including silica), so that the signal of this isotope is easier to detect. The technique we have been using for this is related to "mechanochemistry", and is called "ball-milling". We have shown that this method is highly efficient for these applications. More importantly, it is the first time that this environmentally-friendly method is being used for this oxygen isotopic labeling.

Thanks to these newly-available enriched molecules and materials, we have been working towards further developments in oxygen-17 NMR spectroscopy. Moreover, using this technique, we have started to investigate in detail the structure and properties of several nanomaterials and biomaterials. One case-study has concerned nanoparticles like those found in some sunscreens. Thanks to oxygen-17 labeling, we have started to learn new aspects about their evolution under UV-irradiation (by "looking" specifically at the surface of the nanoparticles), which is important for their future applications.
The oxygen-17 enrichment strategies we have been developing using mechanochemistry are already pushing the boundaries of what can be learnt about the structure and properties of a wide variety of (bio)molecules and functional materials. For the remaining of the project, we will thus continue to develop such oxygen-17 enrichment methodologies, with the goal of making them accessible and attractive to a wide community of chemists. Indeed, for each new molecule or compound, we are endeavouring to establish protocols which are fast, user-friendly, safe, and low-cost, so that they can become widely used not only in research labs, but also in teaching labs.

Thanks to some of these new developments on oxygen-17 enrichment, we also aim at answering intrinsically complex questions about the structure of mineralized tissues like bone, by studying at the atomic scale the interfaces between the mineral and organic components. Such levels of detail have never been reached before, and this could be of use to help develop better cures for bone-diseases.
From oxygen-17 labeling to elucidating the structure of complex (bio)materials