Probing intermolecular interactions in a diethylcarbamazine citrate salt by fast MAS1H solid-state NMR spectroscopy and GIPAW calculations.
Fast magic-angle spinning (MAS) NMR is used to probe intermolecular interactions in a diethylcarbamazine salt, that is widely used as a treatment against adult worms of Wuchereria bancrofti which cause a common disease in tropical countries named filariasis. Specifically, a dihydrogen citrate salt that has improved thermal stability and solubility as compared to the free form is studied. One-dimensional1H,13C and15N and two-dimensional1H-13C and14N-1H heteronuclear correlation NMR experiments under moderate and fast MAS together with GIPAW (CASTEP) calculations enable the assignment of the1H,13C and14N/15N resonances. A two-dimensional1H-1H double-quantum (DQ) -single-quantum (SQ) MAS spectrum recorded with BaBa recoupling at 60kHz MAS identifies specific proton-proton proximities associated with citrate-citrate and citrate-diethylcarbamazine intermolecular interactions.
Departamento de Química, Universidade Federal de São Carlos, Rodovia Washington Luis, km 235, São Carlos, SP 13565-905, Brazil; Department of Physics, University of Warwick, Coventry CV4 7AL, UK. Electronic address: venancio@ufscar.br.
Tiago
T
Venâncio
Departamento de Química, Universidade Federal de São Carlos, Rodovia Washington Luis, km 235, São Carlos, SP 13565-905, Brazil.
Lyege Magalhaes
LM
Oliveira
Instituto de Física de São Carlos, Universidade de São Paulo, Av. Trabalhador são-carlense, 400, São Carlos, SP 13566-590, Brazil.
Javier
J
Ellena
Fundação Oswaldo Cruz - FioCruz, Instituto de Tecnologia em Fármacos-FarManguinhos, Rua Sizenando Nabuco 100, Rio de Janeiro, RJ 21041-250, Brazil.
Nubia
N
Boechat
Department of Physics, University of Warwick, Coventry CV4 7AL, UK.
Steven P
SP
Brown
(1)H NMR; Diethylcarbamazine citrate; Fast MAS NMR; GIPAW calculations; Salt