Theory of solvation and its application to the supercritical fluid extraction/supercritical fluid chromatographic analysis of pharmaceuticals

The main objectives of this PhD project were to relate analyte solubility in supercritical carbon dioxide via molecular structure and also to investigate the factors that influence the solubility and extraction of analytes in a supercritical fluid extraction (SFE) when using carbon dioxide as the solvent

Extraction of pharmaceuticals using pressurised carbon dioxide

This paper reviews the applications of super- and sub-critical carbon dioxide for the extraction of pharmaceuticals from various matrices. The matrices covered are divided into the following types: animal feed, formulations, biological and miscellaneous, with various sub-divisions as appropriate. The polar nature of most pharmaceuticals often precludes the use of carbon dioxide only, so it is common to find the addition of a more polar solvent, as modifier. As the majority of sample types covered are solid, little if any pre-treatment is required, with the exception of grinding, prior to insertion in the sample extraction cell. For liquid-type matrices, sample pre-treatment is the normal. Often this may involve adsorption on an inert support e.g. Celite or diatomaceous earth, or immobilisation on a functionalised silica surface, e.g. C18. The later may take the form of a solid phase extraction cartridge or disk. An attempt has also been made to sample from liquid matrices directly using a modified extraction cell. The variety of sample types, matrices and analyte polarity places stringent requirements on the use of pressurised carbon dioxide. Its potential for effective recovery is examined in this review

A comparison between solid phase extraction and supercritical fluid extraction for the determination of fluconazole from animal feed

The application of supercritical fluid extraction with carbon dioxide and modified carbon dioxide for the determination of fluconazole from an animal feed was studied. A fractional factorial design approach was used to examine the significant experimental variables for quantitative extraction of fluconazole. Gas chromatography with either flame ionisation or mass selective detection was used for quantitation of the extracts. The results indicated that modifier (methanol) had the greatest effect on the recovery of fluconazole from the animal feed

Estimation and determination of steroid solubility in supercritical carbon dioxide

The solubility of ten steroids in supercritical carbon dioxide is reported over a range of temperatures (35-100 °C) and pressures (84-231 kg cm -2). The solubility of testosterone, determined in this work, compares favourably with solubility data previously reported. The use of the solubility parameter and a hydrophobicity term (log P), has been shown to provide a qualitative estimate of steroid solubility

Determination of antifungals in rodent diet by supercritical fluid extraction followed by packed column supercritical fluid chromatography with ultraviolet detection

Supercritical fluid extraction (SFE) followed by packed column supercritical fluid chromatography with ultraviolet detection was evaluated as a quantitative method for determining 4 antifungals (fluconazole, tioconazole, hexaconazole, and UK-47,265) in rodent diet. Chromatography was achieved with a cyano-bonded silica column, UV detection at 210 nm, and methanol-modified supercritical carbon dioxide as mobile phase. The effects of modifier concentration, temperature, and column pressure on antifungal retention time was studied. Off-line SFE was optimized at 2 spike levels, ranging from 0.5 to 10 g/kg, for each of the 4 antifungals. Average recoveries ranged from 79.0% for UK-47,265 to 96.5% for hexaconazole. Overall, the procedure provides a suitable method for analyzing antifungals in spiked rodent diet

Research and development topics in Analytical Chemistry

Summaries of seven of the papers presented at a Meeting of the Analytical Division held on July 13-14, 1993, in the University of Bradford