In the conventional RESS process, a supercritical solution is rapidly expanded through a nozzle to precipitate the solute as microparticles. The modeling of RESS has shown that the precipitated particles at the nozzle tip are on the order of 5-25 nm in size. However, for most solutes, the final particles experimentally obtained are on the order of 800-3000 nm in size, due to growth by coagulation in the expansion chamber. Another difficulty is that most of the pharmaceutical compounds have poor solubility in supercritical carbon dioxide (a fluid of choice). In this work, both challenges are addressed by utilizing a cosolvent that is solid at the nozzle exit conditions. The solid cosolvent (SC) enhances the solubility and provides a barrier for coagulation in the expansion chamber. The solid cosolvent is later remove from the solute particles by lyophilization (sublimation). The new process is termed as RESS-SC. A suitable solid cosolvent is menthol, which is solid below 35 °C (the typical nozzle exit temperature is 5-30 °C) and can be easily sublimed. The RESS-SC concept is demonstrated by producing nanoparticles of griseofulvin, an antifungal drug which has very low solubility in supercritical CO 2 . With the use of the menthol cosolvent, griseofulvin solubility in supercritical CO 2 is increased by about 28-fold. With the use of a simple capillary nozzle, griseofulvin particles in the range of 50-250 nm were obtained, which is a 10-fold reduction from the conventional RESS process. The final powder is pure griseofulvin, free of any stabilizing agents. Particles are characterized by SEM, XRD, and DSC analyses. In addition, data and modeling of the solubility enhancement are presented.
Vibrational spectroscopy has been used t o analyze the microstructures of disklike crystalline macromolecules. These analyses suggest that the structure of the polymethylene sequences are correlated t o the phase behavior of the three molecules studied. Spectroscopic analysis also suggests that two distinct conformations are associated with the ester groups attached to the "core" rings. The relative intensities of the two components correlate well with the phase transitions observed.ABSTRACT: A low-frequency band, the D-LAM band, which is characteristic of long-range conformational disorder in the chain, has been identified in the Raman spectrum of semicrystalline polyethylene. The position and shape that is observed for this band, when compared with the completely molten polymer, indicates that the noncrystalline component in bulk crystallized polyethylene is conformationally liquidlike for crystallinities up to a t least 90%.
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