Supercritical CO2 impregnation process applied to polymer samples preparation for dynamic nuclear polarization solid-state NMR.

In this study, supercritical CO2 (scCO2 ) was used to impregnate polymers with paramagnetic polarizing agents to prepare samples for dynamic nuclear polarization (DNP) solid-state NMR (ssNMR) experiments. As a proof of concept, we impregnated polystyrene samples with bTbK, which stands for bis-TEMPO-bisketal where TEMPO is 2,2,6,6-tetra-methylpiperindin-1-oxyl. Substantial DNP signal enhancements could be measured on DNP-enhanced 1 H → 13 C cross-polarization (CP) magic-angle spinning (MAS) spectra recorded at 9.4 T and ~100 K, reaching a maximum value of 8 in the most favorable case, which appeared comparable or even higher than what is typically obtained on similar systems for former sample preparation methods. These results highlight the potential of scCO2 impregnation as an efficient and possibly versatile methodology to prepare polymer samples for DNP ssNMR investigations.

Supercritical impregnation and optical characterization of loaded foldable intraocular lenses using supercritical fluids.

PURPOSE: To prepare drug-loaded intraocular lenses (IOLs) used to combine cataract surgery with postoperative complication treatment through supercritical impregnation while preserving their optical properties. SETTING: Aix-Marseille Université, CNRS, Centrale Marseille, Laboratoire de Mécanique, Modélisation & Procédés Propres, Marseille, France, and He University Eye Hospital, Liaoning Province, China. DESIGN: Experimental study. METHODS: Supercritical impregnations of commercial foldable IOLs used in cataract surgery with ciprofloxacin (an antibiotic) and dexamethasone 21-phosphate disodium salt (an antiinflammatory drug) were performed in a noncontinuous mode. Impregnation amounts were determined through drug-release kinetic studies. The optical characterizations of IOLs were determined by evaluating the dioptric power and the imaging quality by determining the modulating transfer function (MTF) at a specified spatial frequency according to the International Organization for Standardization (ISO 11979-2:2014). RESULTS: Transparent IOLs presenting an effective impregnation were obtained with a prolonged drug delivery during approximately 10 days. Optical characterizations (dioptric powers and MTF values) show preserved optical properties after supercritical treatment/impregnation. CONCLUSION: Supercritical treatments/impregnations do not damage the optical properties of IOLs and are therefore adequate for the preparation of delivery devices used for cataract surgery.

Impregnation of Fenofibrate on mesoporous silica using supercritical carbon dioxide.

Low oral bioavailability can be circumvented by the formulation of the poorly water soluble drug in ordered mesoporous silica (OMS-L-7). Fenofibrate is an orally administered, poorly water-soluble active pharmaceutical ingredient (API), used clinically to lower lipid levels. Fenofibrate was loaded into silica using two methods: incipient wetness and supercritical impregnation. This study investigates the impact of loading and the impact of varying supercritical carbon dioxide (scCO2) processing conditions. The objective is to enhance Fenofibrate loading into silica while reducing degree of the drug crystallinity, so as to increase the drug's dissolution rate and its bioavailability. The comparison of both impregnation processes was made in terms of impregnation yields and duration as well as physical characterization of the drug. While incipient wetness method led to a Fenofibrate loading up to 300 mgdrug/gsilica in 48 h of impregnation, the supercritical impregnation method yielded loading up to 485 mgdrug/gsilica in 120 min of impregnation duration, at 16 MPa and 308 K, with a low degree of crystallinity (about 1%) comparable to the crystallinity observed via the solvent method. In addition to the enhancement of impregnation efficiency, the supercritical route provides a solvent-free alternative for impregnation.