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 and molecular dynamics that can be enhanced by changing the strength of the oscillating magnetic field (B1) 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 B1 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 B1 fields can be an effective, streamlined, and complementary approach for characterizing not only solid active pharmaceutical ingredients but other solid-state materials as well.

Quality Attributes and Metabolic Profiles of Uvaia (Eugenia pyriformis), a Native Brazilian Atlantic Forest Fruit.

The uvaia is a native Brazilian Atlantic Forest Myrtaceae fruit with a soft pulp, ranging from yellow to orange, with a sweet acidic flavor and sweet fruity aroma. Uvaias present consumption potential, but their physicochemical characteristics are still understudied. In this context, we describe herein the metabolites of uvaia that have been determined by nuclear magnetic resonance spectroscopy. We screened 41 accessions and selected 10 accessions based on their diversity of physicochemical attributes, i.e., their fresh mass, height, diameter, yield, seed mass, total soluble solids, and titratable acidity. Twenty-six metabolites were identified, including sugars, acids, and amino acids. The results of this study comprise the most complete report on sugars and acids in uvaias. The relevant metabolites in terms of abundance were the reducing sugars glucose and fructose, as well as malic and citric acids. Furthermore, this study represents the first description of the uvaia amino acid profile and an outline of its metabolic pathways. Uvaia quality attributes differ among accessions, demonstrating high variability, diversity, and several possibilities in different economic areas. Our findings may help in future breeding programs in the selection of plant material for industries such as food and pharmaceuticals.