About: Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR     Goto   Sponge   NotDistinct   Permalink

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  • Solid dispersions of active pharmaceutical ingredients are of increasing interest due to their versatile use. In the present study polyvinylpyrrolidone (PVP), poly[N-(2-hydroxypropyl)-metacrylamide] (pHPMA), poly(2-ethyl-2-oxazoline) (PEOx), and polyethylene glycol (PEG), each in three Mw, were used to demonstrate structural diversity of solid dispersions. Acetylsalicylic acid (ASA) was used as a model drug. The obtained structural data confirmed that the type of solid dispersion can be primarily controlled by the chemical constitutions of the applied polymers, while the molecular weight of the polymers had no detectable impact. The molecular structure of the prepared dispersions was characterized using solid-state NMR, wide-angle X-ray scattering (WAXS), and differential scanning calorimetry (DSC). By applying various 1H–13C and 1H–1H correlation experiments combined with T1(1H) and T1ρ(1H) relaxation data, the extent of the molecular mixing was determined over a wide range of distances, from intimate intermolecular contacts (0.1–0.5 nm) up to the phase-separated nanodomains reaching ca. 500 nm. Hydrogen-bond interactions between ASA and polymers were probed by the analysis of 13C and 15N CP/MAS NMR spectra combined with the measurements of 1H–15N dipolar profiles. Overall potentialities and limitations of individual experimental techniques were thoroughly evaluated.
  • Solid dispersions of active pharmaceutical ingredients are of increasing interest due to their versatile use. In the present study polyvinylpyrrolidone (PVP), poly[N-(2-hydroxypropyl)-metacrylamide] (pHPMA), poly(2-ethyl-2-oxazoline) (PEOx), and polyethylene glycol (PEG), each in three Mw, were used to demonstrate structural diversity of solid dispersions. Acetylsalicylic acid (ASA) was used as a model drug. The obtained structural data confirmed that the type of solid dispersion can be primarily controlled by the chemical constitutions of the applied polymers, while the molecular weight of the polymers had no detectable impact. The molecular structure of the prepared dispersions was characterized using solid-state NMR, wide-angle X-ray scattering (WAXS), and differential scanning calorimetry (DSC). By applying various 1H–13C and 1H–1H correlation experiments combined with T1(1H) and T1ρ(1H) relaxation data, the extent of the molecular mixing was determined over a wide range of distances, from intimate intermolecular contacts (0.1–0.5 nm) up to the phase-separated nanodomains reaching ca. 500 nm. Hydrogen-bond interactions between ASA and polymers were probed by the analysis of 13C and 15N CP/MAS NMR spectra combined with the measurements of 1H–15N dipolar profiles. Overall potentialities and limitations of individual experimental techniques were thoroughly evaluated. (en)
Title
  • Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR
  • Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR (en)
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  • Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR
  • Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR (en)
skos:notation
  • RIV/61389013:_____/14:00426114!RIV14-GA0-61389013
http://linked.open...avai/riv/aktivita
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  • I, P(GPP106/11/P426)
http://linked.open...iv/cisloPeriodika
  • 2
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http://linked.open...aciTvurceVysledku
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  • 47856
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  • RIV/61389013:_____/14:00426114
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  • solid dispersions; acetylsalicylic acid; polymers (en)
http://linked.open.../riv/klicoveSlovo
http://linked.open...odStatuVydavatele
  • US - Spojené státy americké
http://linked.open...ontrolniKodProRIV
  • [70052D7418E1]
http://linked.open...i/riv/nazevZdroje
  • MOLECULAR PHARMACEUTICS
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  • 11
http://linked.open...iv/tvurceVysledku
  • Hrubý, Martin
  • Urbanová, Martina
  • Brus, Jiří
  • Kobera, Libor
  • Zhigunov, Alexander
  • Kredatusová, Jana
  • Policianová, Olivia
http://linked.open...ain/vavai/riv/wos
  • 000330812500015
issn
  • 1543-8384
number of pages
http://bibframe.org/vocab/doi
  • 10.1021/mp400495h
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