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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
Analytical Chemistry ( IF 7.4 ) Pub Date : 2024-05-13 , DOI: 10.1021/acs.analchem.3c04935
Luisa Souza Almeida 1 , Rodrigo Henrique dos Santos Garcia 2 , Julian Ticona 3 , Silvia L. Cuffini 3 , Eduardo Ribeiro deAzevedo 2 , Luiz Alberto Colnago 4
Affiliation  

Nuclear magnetic resonance (NMR) longitudinal rotating frame relaxation time (T), 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 T 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 T 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, T 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 T 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, 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.

中文翻译:


具有弱自旋锁定场的 NMR 纵向旋转框架弛豫时间 (T1ρ) 作为表征固态活性药物成分的方法:概念验证



核磁共振 (NMR) 纵向旋转框架弛豫时间 (T ) 在低场 NMR 中很少使用,但比传统的 T 1 和 T 2 对结构和分子动力学的敏感性,可以通过改变自旋锁脉冲的振荡磁场 (B 1 ) 的强度来增强这种敏感性。在这里,我们比较了 T 1 、 T 2 和 T 区分世界非活性 (A) 和活性 (C) 晶型的能力卫生组织基本药物甲苯咪唑。结果表明,两种形式的T 1 和T 2 值在统计上相同,均为0.47 T。相反,用弱自旋锁B测量的两种形式的T 1 场,范围从 0.08 到 0.80 mT,在同一光谱仪中具有统计差异。 T 还具有检测限,可检测活性 C 形式中是否存在至少 10% 的非活性 A 形式。因此,用弱自旋锁 B 1 场测量的 T 可以是一种有效、简化和补充的方法,不仅可以表征固体活性药物成分,还可以表征其他固态材料。
更新日期:2024-05-13
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