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Statements

Subject Item
n2:RIV%2F60461373%3A22310%2F13%3A43895363%21RIV14-MSM-22310___
rdf:type
skos:Concept n13:Vysledek
dcterms:description
Analysis of C cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and X-ray powder diffraction data of trospium chloride (TCl) products crystallized from different mixtures of waterethanol [phi(EtOH) = 0.51.0] at various temperatures (0 degrees C, 20 degrees C) and initial concentrations (saturated solution, 30%50% excess of solvent) revealed extensive structural variability of TCl. Although 13C CP/MAS NMR spectra indicated broad variety of structural phases arising from molecular disorder, temperature-modulated DSC identified presence of two distinct components in the products. FTIR spectra revealed alterations in the hydrogen bonding network (ionic hydrogen bond formation), whereas the X-ray diffraction reflected unchanged unit cell parameters. These results were explained by a two-component character of TCl products in which a dominant polymorphic form is accompanied by partly separated nanocrystalline domains of a secondary phase that does not provide clear Bragg reflections. These phases slightly differ in the degree of molecular disorder, in the quality of crystal lattice and hydrogen bonding network. It is also demonstrated that, for the quality control of such complex products, 13C CP/MAS NMR spectroscopy combined with factor analysis (FA) can satisfactorily be used for categorizing the individual samples: FA of 13C CP/MAS NMR spectra found clear relationships between the extent of molecular disorder and crystallization conditions. (c) 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:12351248, 2013 Analysis of C cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and X-ray powder diffraction data of trospium chloride (TCl) products crystallized from different mixtures of waterethanol [phi(EtOH) = 0.51.0] at various temperatures (0 degrees C, 20 degrees C) and initial concentrations (saturated solution, 30%50% excess of solvent) revealed extensive structural variability of TCl. Although 13C CP/MAS NMR spectra indicated broad variety of structural phases arising from molecular disorder, temperature-modulated DSC identified presence of two distinct components in the products. FTIR spectra revealed alterations in the hydrogen bonding network (ionic hydrogen bond formation), whereas the X-ray diffraction reflected unchanged unit cell parameters. These results were explained by a two-component character of TCl products in which a dominant polymorphic form is accompanied by partly separated nanocrystalline domains of a secondary phase that does not provide clear Bragg reflections. These phases slightly differ in the degree of molecular disorder, in the quality of crystal lattice and hydrogen bonding network. It is also demonstrated that, for the quality control of such complex products, 13C CP/MAS NMR spectroscopy combined with factor analysis (FA) can satisfactorily be used for categorizing the individual samples: FA of 13C CP/MAS NMR spectra found clear relationships between the extent of molecular disorder and crystallization conditions. (c) 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:12351248, 2013
dcterms:title
Characterizing crystal disorder of trospium chloride : A comprehensive, 13C CP/MAS NMR, DSC, FTIR, and XRPD study Characterizing crystal disorder of trospium chloride : A comprehensive, 13C CP/MAS NMR, DSC, FTIR, and XRPD study
skos:prefLabel
Characterizing crystal disorder of trospium chloride : A comprehensive, 13C CP/MAS NMR, DSC, FTIR, and XRPD study Characterizing crystal disorder of trospium chloride : A comprehensive, 13C CP/MAS NMR, DSC, FTIR, and XRPD study
skos:notation
RIV/60461373:22310/13:43895363!RIV14-MSM-22310___
n13:predkladatel
n14:orjk%3A22310
n3:aktivita
n11:P n11:I n11:Z
n3:aktivity
I, P(GPP106/11/P426), Z(MSM6046137302)
n3:cisloPeriodika
4
n3:dodaniDat
n9:2014
n3:domaciTvurceVysledku
n4:2013223 n4:4264533 n4:6248381
n3:druhVysledku
n5:J
n3:duvernostUdaju
n17:S
n3:entitaPredkladatele
n19:predkladatel
n3:idSjednocenehoVysledku
65131
n3:idVysledku
RIV/60461373:22310/13:43895363
n3:jazykVysledku
n21:eng
n3:klicovaSlova
disorder; DSC; FTIR; X-ray diffractometry; polymorphism; factor analysis; solid state NMR; trospium chloride
n3:klicoveSlovo
n7:disorder n7:FTIR n7:factor%20analysis n7:polymorphism n7:solid%20state%20NMR n7:DSC n7:trospium%20chloride n7:X-ray%20diffractometry
n3:kodStatuVydavatele
US - Spojené státy americké
n3:kontrolniKodProRIV
[3F9E3AD816E3]
n3:nazevZdroje
Journal of Pharmaceutical Sciences
n3:obor
n20:FR
n3:pocetDomacichTvurcuVysledku
3
n3:pocetTvurcuVysledku
11
n3:projekt
n15:GPP106%2F11%2FP426
n3:rokUplatneniVysledku
n9:2013
n3:svazekPeriodika
102
n3:tvurceVysledku
Brus, Jiří Sedenková, Ivana Čejka, Jan Šturcová, Adriana Beneš, Hynek Kobera, Libor Kratochvíl, Bohumil Skořepová, Eliška Šturc, Antonín Urbanová, Martina Policianová, Olivia
n3:wos
000315723700009
n3:zamer
n18:MSM6046137302
s:issn
0022-3549
s:numberOfPages
14
n6:doi
10.1002/jps.23457
n10:organizacniJednotka
22310