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Multi-way diffusion NMR data analysis applied to chemical reaction monitoring

Grant number: 15/19229-3
Support type:Scholarships abroad - Research Internship - Doctorate
Effective date (Start): January 19, 2016
Effective date (End): July 18, 2016
Field of knowledge:Physical Sciences and Mathematics - Chemistry - Organic Chemistry
Principal researcher:Roberto Rittner Neto
Grantee:Thaís Mendonça Barbosa
Supervisor abroad: Lars Mathias Nilsson
Home Institution: Instituto de Química (IQ). Universidade Estadual de Campinas (UNICAMP). Campinas , SP, Brazil
Research place: University of Manchester, England  
Associated to the scholarship:14/12776-6 - Development and application of NMR techniques to analyse complex mixtures, BP.DR

Abstract

Mixture analysis is among the most important areas of chemistry research: most of Mother Nature's interesting problems present themselves as mixtures. In the work proposed here a novel approach to the use of NMR spectroscopy to monitor organic reactions will be investigated. NMR is well suited to following chemical reactions, especially when signals are well resolved. However, when signals in spectra do overlap, which is common, advanced data analysis tools are needed. One of the most widely used techniques for intact mixture analysis by NMR is diffusion-ordered spectroscopy (DOSY), but even here spectral overlap is a problem. Fortunately, the combination of DOSY and advanced statistical methods (chemometrics) has been shown to handle such overlap surprisingly well. The experimental part of the project will monitor the formation of N-acylhydrazones, running DOSY experiments during the reaction course. The use of DOSY, rather than simple proton NMR, allows the use of powerful chemometric approaches such as the PARAFAC (PARAllel FACtor analysis) multi-way decomposition method. This uses the trilinear structure of the data to obtain separate matrices containing the N spectra, diffusion decays, and concentration time courses, respectively. This approach should allow us to obtain both accurate kinetic data for reactants, intermediates and products, and an isolated 1H NMR spectrum of each species involved in the reaction, together with information on its diffusion, even where the experimental spectra are severely overlapped.

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Scientific publications (4)
(References retrieved automatically from Web of Science and SciELO through information on FAPESP grants and their corresponding numbers as mentioned in the publications by the authors)
BARBOSA, THAIS M.; CASTANAR, LAURA; MOUTZOURI, PINELOPI; NILSSON, MATHIAS; MORRIS, GARETH A.; RITTNER, ROBERTO; TORMENA, CLAUDIO F. Improving the Sensitivity of FESTA Methods for the Analysis of Fluorinated Mixtures. Analytical Chemistry, v. 92, n. 2, p. 2224-2228, JAN 21 2020. Web of Science Citations: 0.
CASTANAR, LAURA; MOUTZOURI, PINELOPI; BARBOSA, THAIS M.; TORMENA, CLAUDIO F.; RITTNER, ROBERTO; PHILLIPS, ANDREW R.; COOMBES, STEVEN R.; NILSSON, MATHIAS; MORRIS, GARETH A. FESTA: An Efficient Nuclear Magnetic Resonance Approach for the Structural Analysis of Mixtures Containing Fluorinated Species. Analytical Chemistry, v. 90, n. 8, p. 5445-5450, APR 17 2018. Web of Science Citations: 2.
BARBOSA, T. M.; MORRIS, G. A.; NILSSON, M.; RITTNER, R.; TORMENA, C. F. H-1 and F-19 NMR in drug stress testing: the case of voriconazole. RSC ADVANCES, v. 7, n. 54, p. 34000-34004, 2017. Web of Science Citations: 2.
BARBOSA, T. M.; RITTNER, R.; TORMENA, C. F.; MORRIS, G. A.; NILSSON, M. Convection in liquid-state NMR: expect the unexpected. RSC ADVANCES, v. 6, n. 97, p. 95173-95176, 2016. Web of Science Citations: 16.

Please report errors in scientific publications list by writing to: cdi@fapesp.br.