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Title: 35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients

Abstract

In this paper, we show how to obtain efficient dynamic nuclear polarization (DNP) enhanced 35Cl solid-state NMR (SSNMR) spectra at 9.4 T and demonstrate how they can be used to characterize the molecular-level structure of hydrochloride salts of active pharmaceutical ingredients (APIs) in both bulk and low wt% API dosage forms. 35Cl SSNMR central-transition powder patterns of chloride ions are typically tens to hundreds of kHz in breadth, and most cannot be excited uniformly with high-power rectangular pulses or acquired under conditions of magic-angle spinning (MAS). Herein, we demonstrate the combination of DNP and 1H–35Cl broadband adiabatic inversion cross polarization (BRAIN-CP) experiments for the acquisition of high quality wideline spectra of APIs under static sample conditions, and obtain signals up to 50 times greater than in spectra acquired without the use of DNP at 100 K. We report a new protocol, called spinning-on spinning-off (SOSO) acquisition, where MAS is applied during part of the polarization delay to increase the DNP enhancements and then the MAS rotation is stopped so that a wideline 35Cl NMR powder pattern free from the effects of spinning sidebands can be acquired under static conditions. This method provides an additional two-fold signal enhancement compared to DNP-enhancedmore » SSNMR spectra acquired under purely static conditions. DNP-enhanced 35Cl experiments are used to characterize APIs in bulk and dosage forms with Cl contents as low as 0.45 wt%. These results are compared to DNP-enhanced 1H–13C CP/MAS spectra of APIs in dosage forms, which are often hindered by interfering signals arising from the binders, fillers and other excipient materials.« less

Authors:
 [1];  [2];  [3];  [1]
+ Show Author Affiliations
  1. Univ. of Windsor, Windsor, ON (Canada)
  2. Iowa State Univ., Ames, IA (United States); Ames Lab., Ames, IA (United States)
  3. Ecole Polytechnique Federale Lausanne (Switzlerland)
Publication Date:
Research Org.:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1335033
Report Number(s):
IS-J-9134
Journal ID: ISSN 1463-9076; PPCPFQ
Grant/Contract Number:  
AC02-07CH11358
Resource Type:
Accepted Manuscript
Journal Name:
Physical Chemistry Chemical Physics. PCCP
Additional Journal Information:
Journal Volume: 18; Journal Issue: 37; Journal ID: ISSN 1463-9076
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY

Citation Formats

Hirsh, David A., Rossini, Aaron J., Emsley, Lyndon, and Schurko, Robert W. 35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients. United States: N. p., 2016. Web. doi:10.1039/c6cp04353d.
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Hirsh, David A., Rossini, Aaron J., Emsley, Lyndon, & Schurko, Robert W. 35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients. United States. https://doi.org/10.1039/c6cp04353d
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Hirsh, David A., Rossini, Aaron J., Emsley, Lyndon, and Schurko, Robert W. Wed . "35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients". United States. https://doi.org/10.1039/c6cp04353d. https://www.osti.gov/servlets/purl/1335033.
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@article{osti_1335033,
title = {35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients},
author = {Hirsh, David A. and Rossini, Aaron J. and Emsley, Lyndon and Schurko, Robert W.},
abstractNote = {In this paper, we show how to obtain efficient dynamic nuclear polarization (DNP) enhanced 35Cl solid-state NMR (SSNMR) spectra at 9.4 T and demonstrate how they can be used to characterize the molecular-level structure of hydrochloride salts of active pharmaceutical ingredients (APIs) in both bulk and low wt% API dosage forms. 35Cl SSNMR central-transition powder patterns of chloride ions are typically tens to hundreds of kHz in breadth, and most cannot be excited uniformly with high-power rectangular pulses or acquired under conditions of magic-angle spinning (MAS). Herein, we demonstrate the combination of DNP and 1H–35Cl broadband adiabatic inversion cross polarization (BRAIN-CP) experiments for the acquisition of high quality wideline spectra of APIs under static sample conditions, and obtain signals up to 50 times greater than in spectra acquired without the use of DNP at 100 K. We report a new protocol, called spinning-on spinning-off (SOSO) acquisition, where MAS is applied during part of the polarization delay to increase the DNP enhancements and then the MAS rotation is stopped so that a wideline 35Cl NMR powder pattern free from the effects of spinning sidebands can be acquired under static conditions. This method provides an additional two-fold signal enhancement compared to DNP-enhanced SSNMR spectra acquired under purely static conditions. DNP-enhanced 35Cl experiments are used to characterize APIs in bulk and dosage forms with Cl contents as low as 0.45 wt%. These results are compared to DNP-enhanced 1H–13C CP/MAS spectra of APIs in dosage forms, which are often hindered by interfering signals arising from the binders, fillers and other excipient materials.},
doi = {10.1039/c6cp04353d},
journal = {Physical Chemistry Chemical Physics. PCCP},
number = 37,
volume = 18,
place = {United States},
year = {Wed Aug 24 00:00:00 EDT 2016},
month = {Wed Aug 24 00:00:00 EDT 2016}
}
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