| Autor: |
Almeida LS; São Carlos Institute of Chemistry, University of São Paulo, 13566-590 São Carlos, Brazil., Garcia RHDS; São Carlos Institute of Physics, University of São Paulo, 13566-590 São Carlos, Brazil., Ticona J; Instituto de Ciência e Tecnologia, Universidade Federal de São Paulo, 12231-280 São José dos Campos, Brazil., Cuffini SL; Instituto de Ciência e Tecnologia, Universidade Federal de São Paulo, 12231-280 São José dos Campos, Brazil., deAzevedo ER; São Carlos Institute of Physics, University of São Paulo, 13566-590 São Carlos, Brazil., Colnago LA; Embrapa Instrumentação Agropecuária, 13560-970 São Carlos, Brazil. |
| Jazyk: |
angličtina |
| Zdroj: |
Analytical chemistry [Anal Chem] 2024 May 28; Vol. 96 (21), pp. 8317-8324. Date of Electronic Publication: 2024 May 13. |
| DOI: |
10.1021/acs.analchem.3c04935 |
| Abstrakt: |
Nuclear magnetic resonance (NMR) longitudinal rotating frame relaxation time (T 1ρ ), rarely used in low-field NMR, can be more effective than conventional T 1 and T 2 relaxation times to differentiate polymorphic forms of solid pharmaceuticals. This could be attributed to T 1ρ sensibility to structural and molecular dynamics that can be enhanced by changing the strength of the oscillating magnetic field ( B 1 ) of spinlock pulses. Here, we compared the capacity of T 1 , T 2 , and T 1ρ to differentiate inactive (A) and active (C) crystalline forms of the World Health Organization essential drug Mebendazole. The results showed that T 1 and T 2 values of both forms were statistically identical at 0.47 T. Conversely, T 1ρ of both forms measured with weak spinlock B 1 fields, ranging from 0.08 to 0.80 mT were statistically different in the same spectrometer. The T 1ρ also has the limit of detection to detect the presence of at least 10% of inactive A form in the active C form. Therefore, T 1ρ , measured with weak spinlock B 1 fields can be an effective, streamlined, and complementary approach for characterizing not only solid active pharmaceutical ingredients but other solid-state materials as well. |
| Databáze: |
MEDLINE |
| Externí odkaz: |
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