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231224s2012 xx |||||o 00| ||eng c |
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|a 10.1002/mrc.3798
|2 doi
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|a pubmed24n0719.xml
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|a (DE-627)NLM215743059
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|a (NLM)22367881
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|a DE-627
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|c DE-627
|e rakwb
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|a eng
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|a Suzuki, Kazuko
|e verfasserin
|4 aut
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|a Hartmann-Hahn 2D-map to optimize the RAMP-CPMAS NMR experiment for pharmaceutical materials
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|c 2012
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|a Text
|b txt
|2 rdacontent
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|a ƒaComputermedien
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|2 rdamedia
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|a ƒa Online-Ressource
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|2 rdacarrier
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|a Date Completed 29.06.2015
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|a Date Revised 03.11.2014
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|a published: Print-Electronic
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|a Citation Status MEDLINE
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|a Copyright © 2012 John Wiley & Sons, Ltd.
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|a Cross polarization-magic angle spinning (CPMAS) is the most used experiment for solid-state NMR measurements in the pharmaceutical industry, with the well-known variant RAMP-CPMAS its dominant implementation. The experimental work presented in this contribution focuses on the entangled effects of the main parameters of such an experiment. The shape of the RAMP-CP pulse has been considered as well as the contact time duration, and a particular attention also has been devoted to the radio-frequency (RF) field inhomogeneity. (13)C CPMAS NMR spectra have been recorded with a systematic variation of (13)C and (1)H constant radiofrequency field pair values and represented as a Hartmann-Hahn matching two-dimensional map. Such a map yields a rational overview of the intricate optimal conditions necessary to achieve an efficient CP magnetization transfer. The map also highlights the effects of sweeping the RF by the RAMP-CP pulse on the number of Hartmann-Hahn matches crossed and how RF field inhomogeneity helps in increasing the CP efficiency by using a larger fraction of the sample. In the light of the results, strategies for optimal RAMP-CPMAS measurements are suggested, which lead to a much higher efficiency than constant amplitude CP experiment
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|a Journal Article
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|a Research Support, Non-U.S. Gov't
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|a NMR
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|a RAMP-CPMAS
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|a pharmaceutical materials
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|a solid-state NMR
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|a Protons
|2 NLM
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|a Adamantane
|2 NLM
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|a PJY633525U
|2 NLM
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| 650 |
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|a Glycine
|2 NLM
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|a TE7660XO1C
|2 NLM
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|a Ibuprofen
|2 NLM
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| 650 |
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|a WK2XYI10QM
|2 NLM
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| 700 |
1 |
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|a Martineau, Charlotte
|e verfasserin
|4 aut
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| 700 |
1 |
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|a Fink, Gerhard
|e verfasserin
|4 aut
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| 700 |
1 |
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|a Steuernagel, Stefan
|e verfasserin
|4 aut
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|a Taulelle, Francis
|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 50(2012), 2 vom: 01. Feb., Seite 159-68
|w (DE-627)NLM098179667
|x 1097-458X
|7 nnns
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| 773 |
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|g volume:50
|g year:2012
|g number:2
|g day:01
|g month:02
|g pages:159-68
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|u http://dx.doi.org/10.1002/mrc.3798
|3 Volltext
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