Probing intermolecular interactions in a diethylcarbamazine citrate salt by fast MAS H-1 solid-state NMR spectroscopy and GIPAW calculations

Autor(es)

Venancio, Tiago ^{[1, 2]} ; Oliveira, Lyege Magalhaes ^[2] ; Ellena, Javier ^[3] ; Boechat, Nubia ^[4] ; Brown, Steven P. ^[1]

Afiliação do(s) autor(es)

^[1] Univ Warwick, Dept Phys, Coventry CV4 7AL, W Midlands - England

^[2] Univ Fed Sao Carlos, Dept Quim, Rodovia Washington Luis, Km 235, BR-13565905 Sao Carlos, SP - Brazil

^[3] Univ Sao Paulo, Inst Fis Sao Carlos, Av Trabalhador Sao Carlos 400, BR-13566590 Sao Carlos, SP - Brazil

^[4] Fundacao Oswaldo Cruz FioCruz, Inst Tecnol Farmacos Farmanguinhos, Rua Sizenando Nabuco 100, BR-21041250 Rio De Janeiro, RJ - Brazil

• Tipo de documento: Artigo Científico
• Fonte: SOLID STATE NUCLEAR MAGNETIC RESONANCE; v. 87, p. 73-79, OCT 2017.
• Citações Web of Science: 4

Resumo

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-dimensional H-1, C-13 and N-15 and two-dimensional H-1-C-13 and N-14-H-1 heteronuclear correlation NMR experiments under moderate and fast MAS together with GIPAW (CASTEP) calculations enable the assignment of the H-1, C-13 and N-14/N-15 resonances. A two-dimensional H-1-H-1 double-quantum (DQ) -single-quantum (SQ) MAS spectrum recorded with BaBa recoupling at 60 kHz MAS identifies specific proton-proton proximities associated with citrate-citrate and citrate-diethylcarbamazine intermolecular interactions. (AU)

• Processo FAPESP: 09/13860-2 - Aplicação da ressonância magnética nuclear no estado sólido aliada a ferramentas quimiométricas na caracterização de polimorfismo em fármacos
• Beneficiário: Tiago Venancio
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 15/21708-7 - Caracterização de complexos supramoleculares de sólidos farmacêuticos por Ressonância Magnética Nuclear no estado sólido e abordagens computacionais
• Beneficiário: Tiago Venancio
• Modalidade de apoio: Bolsas no Exterior - Pesquisa