NMR Longitudinal Rotating Frame Relaxation Time (T1ρ) with a Weak Spin Locking Field as an Approach to Characterize Solid-State Active Pharmaceutical Ingredients: Proof of Concept

Nuclear magnetic resonance (NMR) longitudinal rotating frame relaxation time (T1ρ), rarely used in low-field NMR, can be more effective than conventional T1 and T2 relaxation times to differentiate polymorphic forms of solid pharmaceuticals. This could be attributed to T1ρ sensibility to structural...

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Bibliographic Details
Published in:Analytical chemistry (Washington) 2024-05, Vol.96 (21), p.8317-8324
Main Authors: Almeida, Luisa Souza, Garcia, Rodrigo Henrique dos Santos, Ticona, Julian, Cuffini, Silvia L., deAzevedo, Eduardo Ribeiro, Colnago, Luiz Alberto
Format: Article
Language:English
Subjects:
Bulk Drugs
Ingredients
Magnetic Fields
Magnetic Resonance Spectroscopy - methods
Mebendazole
Mebendazole - chemistry
Molecular dynamics
NMR
Nuclear magnetic resonance
Pharmaceutical Preparations - analysis
Pharmaceutical Preparations - chemistry
Pharmaceuticals
Proof of Concept Study
Relaxation time
Rotation
Solid state
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Summary:Nuclear magnetic resonance (NMR) longitudinal rotating frame relaxation time (T1ρ), rarely used in low-field NMR, can be more effective than conventional T1 and T2 relaxation times to differentiate polymorphic forms of solid pharmaceuticals. This could be attributed to T1ρ 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 T1, T2, and T1ρ to differentiate inactive (A) and active (C) crystalline forms of the World Health Organization essential drug Mebendazole. The results showed that T1 and T2 values of both forms were statistically identical at 0.47 T. Conversely, T1ρ 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 T1ρ also has the limit of detection to detect the presence of at least 10% of inactive A form in the active C form. Therefore, T1ρ, 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.
ISSN:0003-2700
1520-6882
1520-6882
DOI:10.1021/acs.analchem.3c04935