ArticleThe journal of physical chemistry. B2017
In Situ Characterization of Pharmaceutical Formulations by Dynamic Nuclear Polarization Enhanced MAS NMR.
Article in The journal of physical chemistry. B, 2017. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 18 papers.
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Who cites it
18 citing papers in PubMed.
- Accessible hybrid DFT-quality NMR crystallographyChemical science · 2026Article
- Systematic Evaluation of Polarizing Agents for Dynamic Nuclear Polarization Enhanced NMR.Angewandte Chemie (International ed. in English) · 2025Article
- Quantitative Solid-State NMR Spectroscopy (qSSNMR) in Pharmaceutical Analysis.Magnetic resonance in chemistry : MRC · 2025Review
- Spiers Memorial Lecture: NMR crystallography.Faraday discussions · 2025Article
- Cryogenic and Dissolution DNP NMR on γ-Irradiated Organic Molecules.Journal of the American Chemical Society · 2024Article
- Atomic-level structure determination of amorphous molecular solids by NMR.Nature communications · 2023Article
- Spin Hyperpolarization in Modern Magnetic Resonance.Chemical reviews · 2023Review
- New Development in Understanding Drug-Polymer Interactions in Pharmaceutical Amorphous Solid Dispersions from Solid-State Nuclear Magnetic Resonance.Molecular pharmaceutics · 2022Review
- pH-Dependent supersaturation from amorphous solid dispersions of weakly basic drugs.Pharmaceutical research · 2022Article
- A Machine Learning Model of Chemical Shifts for Chemically and Structurally Diverse Molecular Solids.The journal of physical chemistry. C, Nanomaterials and interfaces · 2022Article
- Tools shaping drug discovery and development.Biophysics reviews · 2022Review
- Spinning-Driven Dynamic Nuclear Polarization with Optical Pumping.The journal of physical chemistry. A · 2022Article
- Article
- Synergy of Solid-State NMR, Single-Crystal X-ray Diffraction, and Crystal Structure Prediction Methods: A Case Study of Teriflunomide (TFM).Crystal growth & design · 2021Article
- Solid-state NMR spectroscopy.Nature reviews. Methods primers · 2021Article
- Enabling Natural AbundanceThe journal of physical chemistry letters · 2020Article
- UltrafastMolecular pharmaceutics · 2020Article
- Continuous wave electron paramagnetic resonance of nitroxide biradicals in fluid solution.Concepts in magnetic resonance. Part A, Bridging education and research · 2018Article
Corrections and comments
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Authors and funding
13 authors.
Funding
Abstract
A principal advantage of magic angle spinning (MAS) NMR spectroscopy lies in its ability to determine molecular structure in a noninvasive and quantitative manner. Accordingly, MAS should be widely applicable to studies of the structure of active pharmaceutical ingredients (API) and formulations. However, the low sensitivity encountered in spectroscopy of natural abundance APIs present at low concentration has limited the success of MAS experiments. Dynamic nuclear polarization (DNP) enhances NMR sensitivity and can be used to circumvent this problem provided that suitable paramagnetic polarizing agent can be incorporated into the system without altering the integrity of solid dosages. Here, we demonstrate that DNP polarizing agents can be added in situ during the preparation of amorphous solid dispersions (ASDs) via spray drying and hot-melt extrusion so that ASDs can be examined during drug development. Specifically, the dependence of DNP enhancement on sample composition, radical concentration, relaxation properties of the API and excipients, types of polarizing agents and proton density, has been thoroughly investigated. Optimal enhancement values are obtained from ASDs containing 1% w/w radical concentration. Both polarizing agents TOTAPOL and AMUPol provided reasonable enhancements. Partial deuteration of the excipient produced 3× higher enhancement values. With these parameters, an ASD containing posaconazole and vinyl acetate yields a 32-fold enhancement which presumably results in a reduction of NMR measurement time by ∼1000. This boost in signal intensity enables the full assignment of the natural abundance pharmaceutical formulation through multidimensional correlation experiments.
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Registered trials
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