PURPOSE: Effects of polyvinylpyrrolidone (PVP) molecular weight on the solid-state intermolecular interactions among probucol/PVP/sodium dodecyl sulfate (SDS) ternary ground mixtures (GM) and the formation of nanoparticles were investigated by solid-state NMR spectroscopy. MATERIALS AND METHODS: Ternary GMs of probucol were prepared with PVP (K12, K17, K30 or K90) and SDS at a weight ratio of 1:3:1 and were ground for 15, 30 and 60 min. Solid-state interactions were evaluated using powder X-ray diffraction (PXRD) and solid-state cross polarization/magic angle spinning (CP/MAS) (13)C NMR spectroscopy. A high resolution scanning electron microscopy (SEM) was employed to observe nanoparticles of probucol in the GM. RESULTS: The solid-state (13)C CP/MAS NMR results indicate that the low molecular weight PVP interacts with probucol and SDS more strongly than the high molecular weight PVP in the ternary GM. This finding was consistent with the result that smaller drug nanoparticles were obtained using low molecular weight of PVP. SEM images of probucol/PVP K12/SDS confirmed the presence of nanoparticles (15-25 nm) in the GM. CONCLUSIONS: Grinding-induced solid-state interactions among drug, PVP and SDS could be detected using solid state (13)C NMR. The interactions in both probucol-PVP and PVP-SDS should occur simultaneously to generate nanometer-sized particles of probucol.
PURPOSE: Effects of polyvinylpyrrolidone (PVP) molecular weight on the solid-state intermolecular interactions among probucol/PVP/sodium dodecyl sulfate (SDS) ternary ground mixtures (GM) and the formation of nanoparticles were investigated by solid-state NMR spectroscopy. MATERIALS AND METHODS: Ternary GMs of probucol were prepared with PVP (K12, K17, K30 or K90) and SDS at a weight ratio of 1:3:1 and were ground for 15, 30 and 60 min. Solid-state interactions were evaluated using powder X-ray diffraction (PXRD) and solid-state cross polarization/magic angle spinning (CP/MAS) (13)C NMR spectroscopy. A high resolution scanning electron microscopy (SEM) was employed to observe nanoparticles of probucol in the GM. RESULTS: The solid-state (13)C CP/MAS NMR results indicate that the low molecular weight PVP interacts with probucol and SDS more strongly than the high molecular weight PVP in the ternary GM. This finding was consistent with the result that smaller drug nanoparticles were obtained using low molecular weight of PVP. SEM images of probucol/PVPK12/SDS confirmed the presence of nanoparticles (15-25 nm) in the GM. CONCLUSIONS: Grinding-induced solid-state interactions among drug, PVP and SDS could be detected using solid state (13)C NMR. The interactions in both probucol-PVP and PVP-SDS should occur simultaneously to generate nanometer-sized particles of probucol.
Authors: E Merisko-Liversidge; P Sarpotdar; J Bruno; S Hajj; L Wei; N Peltier; J Rake; J M Shaw; S Pugh; L Polin; J Jones; T Corbett; E Cooper; G G Liversidge Journal: Pharm Res Date: 1996-02 Impact factor: 4.200
Authors: N Kondo; T Iwao; H Masuda; K Yamanouchi; Y Ishihara; N Yamada; T Haga; Y Ogawa; K Yokoyama Journal: Chem Pharm Bull (Tokyo) Date: 1993-04 Impact factor: 1.645