This study investigated the development of a novel approach to surface characterization of drug poly- morphism and the extension of the capabilities of this method to perform ＇real time＇ in situ measure- ments. This...This study investigated the development of a novel approach to surface characterization of drug poly- morphism and the extension of the capabilities of this method to perform ＇real time＇ in situ measure- ments. This was achieved using diffuse reflectance visible （DRV） spectroscopy and dye deposition, using the pH sensitive dye, thymol blue （TB）. Two polymorphs, SFN-β and SFN-γ, of the drug substance sulfanilamide （SFN） were examined. The interaction of adsorbed dye with polymorphs showed different behavior, and thus reported different DRV spectra. Consideration of the acid/base properties of the morphological forms of the drug molecule provided a rationalization of the mechanism of differential coloration by indicator dyes. The kinetics of the polymorphic transformation of SFN polymorphs was monitored using treatment with TB dye and DRV spectroscopy. The thermally-induced transformation fitted a first-order solid-state kinetic model （R2=0.992）, giving a rate constant of 2.43 × 10^- 2 s 1.展开更多
For the solid-solid transformation from form Ⅱ to form Ⅰ of isotactic polybutene-1(iPB),the temperature dependence of form Ⅰ nucleation and growth was deemed to control the transformation process.However,the relati...For the solid-solid transformation from form Ⅱ to form Ⅰ of isotactic polybutene-1(iPB),the temperature dependence of form Ⅰ nucleation and growth was deemed to control the transformation process.However,the relationship between formⅠ formation and form Ⅱ disappearance in the transformation process is not clear.In this work,the spontaneous crystal transformation from form Ⅱ to Ⅰ of iPB with 81 mol%mmmm sequence concentration is studied firstly by tracking the two processes,the decay of form Ⅱ and the yielding of form Ⅰ in a wide range of temperature spanning from 0℃ to 50℃ and in a long transformation time ranging from 5 min to 65 days with in situ FTIR and WAXD.Unlike the literature reports,the decay rate of form Ⅱ is firstly found to be lower than the yielding rate of form Ⅰ at all studied temperatures,especially at low transition temperature.This is attributed to the amorphous chains which locate near crystal lamella participating into the nucleation of form Ⅱ.The regular chain folding and growth of i PB form Ⅰ from amorphous chains containing short isotactic sequences also lead to an increase in crystallinity of form Ⅰ compared with that of initial form Ⅱ crystallized at 60℃.An increase in the annealing temperature results in decrease in crystallinity and increase in lamellae thickness of i PB formⅠ.展开更多
文摘This study investigated the development of a novel approach to surface characterization of drug poly- morphism and the extension of the capabilities of this method to perform ＇real time＇ in situ measure- ments. This was achieved using diffuse reflectance visible （DRV） spectroscopy and dye deposition, using the pH sensitive dye, thymol blue （TB）. Two polymorphs, SFN-β and SFN-γ, of the drug substance sulfanilamide （SFN） were examined. The interaction of adsorbed dye with polymorphs showed different behavior, and thus reported different DRV spectra. Consideration of the acid/base properties of the morphological forms of the drug molecule provided a rationalization of the mechanism of differential coloration by indicator dyes. The kinetics of the polymorphic transformation of SFN polymorphs was monitored using treatment with TB dye and DRV spectroscopy. The thermally-induced transformation fitted a first-order solid-state kinetic model （R2=0.992）, giving a rate constant of 2.43 × 10^- 2 s 1.
基金financially supported by the Major Science and Technology Innovation Project of Shandong Province (No. 2019JZZY010352)Natural Science Foundation of Shandong Province (ZR2019MB072)Taishan Scholar Program
文摘For the solid-solid transformation from form Ⅱ to form Ⅰ of isotactic polybutene-1(iPB),the temperature dependence of form Ⅰ nucleation and growth was deemed to control the transformation process.However,the relationship between formⅠ formation and form Ⅱ disappearance in the transformation process is not clear.In this work,the spontaneous crystal transformation from form Ⅱ to Ⅰ of iPB with 81 mol%mmmm sequence concentration is studied firstly by tracking the two processes,the decay of form Ⅱ and the yielding of form Ⅰ in a wide range of temperature spanning from 0℃ to 50℃ and in a long transformation time ranging from 5 min to 65 days with in situ FTIR and WAXD.Unlike the literature reports,the decay rate of form Ⅱ is firstly found to be lower than the yielding rate of form Ⅰ at all studied temperatures,especially at low transition temperature.This is attributed to the amorphous chains which locate near crystal lamella participating into the nucleation of form Ⅱ.The regular chain folding and growth of i PB form Ⅰ from amorphous chains containing short isotactic sequences also lead to an increase in crystallinity of form Ⅰ compared with that of initial form Ⅱ crystallized at 60℃.An increase in the annealing temperature results in decrease in crystallinity and increase in lamellae thickness of i PB formⅠ.
