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231225s2022 xx |||||o 00| ||eng c |
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|a 10.1002/mrc.5267
|2 doi
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|a pubmed24n1126.xml
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|e rakwb
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|a eng
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|a Scheidel, Sebastian
|e verfasserin
|4 aut
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|a You cannot fight the pressure
|b Structural rearrangements of active pharmaceutical ingredients under magic angle spinning
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|c 2022
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|a Text
|b txt
|2 rdacontent
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|a ƒaComputermedien
|b c
|2 rdamedia
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|a ƒa Online-Ressource
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|a Date Completed 26.04.2022
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|a Date Revised 28.04.2022
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|a published: Print-Electronic
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|a Citation Status MEDLINE
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|a © 2022 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.
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|a Although solid-state nuclear magnetic resonance (NMR) is a versatile analytical tool to study polymorphs and phase transitions of pharmaceutical molecules and products, this work summarizes examples of spontaneous and unexpected (and unwanted) structural rearrangements and phase transitions (amorphous-to-crystalline and crystalline-to-crystalline) under magic angle spinning (MAS) conditions, some of them clearly being due to the pressure experienced by the samples. It is widely known that such changes can often be detected by X-ray powder diffraction (XRPD); here, the capability of solid-state NMR experiments with a special focus on 1 H-13 C frequency-switched Lee-Goldburg heteronuclear correlation (FSLG HETCOR)/MAS NMR experiments to detect even subtle changes on a molecular level not observable by conventional 1D NMR experiments or XRPD is presented. Furthermore, it is shown that a polymorphic impurity combined with MAS can induce a crystalline-to-crystalline phase transition. This showcases that solid-state NMR is not always noninvasive and such changes upon MAS should be considered in particular when compounds are studied over longer time spans
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|a Journal Article
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|a Research Support, Non-U.S. Gov't
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|a 19F
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|a 1H-13C HETCOR
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|a API
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|a MAS
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|a XRPD
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|a solid-state NMR
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|a structural changes
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|a Pharmaceutical Preparations
|2 NLM
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|a Östreicher, Laurina
|e verfasserin
|4 aut
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|a Mark, Isabelle
|e verfasserin
|4 aut
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|a Pöppler, Ann-Christin
|e verfasserin
|4 aut
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| 773 |
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|i Enthalten in
|t Magnetic resonance in chemistry : MRC
|d 1985
|g 60(2022), 6 vom: 30. Juni, Seite 572-582
|w (DE-627)NLM098179667
|x 1097-458X
|7 nnns
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| 773 |
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|g volume:60
|g year:2022
|g number:6
|g day:30
|g month:06
|g pages:572-582
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|u http://dx.doi.org/10.1002/mrc.5267
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