Comparison by capillary SFC and SFC‐MS of soxhlet and supercritical fluid extraction of hamster feces

Abstract

SummaryComponents of hamster feces ranging from low molecular weight fatty acids through the expected range of triglycerides have been eluted in a single SFC run with simultaneous pressure and temperature pmgramming.Temperature programming from 140°C to 240°C was required to provide optimum conditions for separation of the fatty acids and to move the elution region of the sterol esters away from that of the triglycerides. Data from molecular weight triglycerides are not eluted using conventional capillary gas chromatography (GC) 121. High temperature GC extends the applicability of the technique to less volatile components [3]. However, certain higher molecular weight, unsaturated sterol esters and unsaturated triglycerides may undergo thermal decomposition reactions at the temperatures required for their elution [4]. chemical ionization and electron impact mass spectrometry of compounds separated by SFC were used to confirm identities suggested by retention measurements and to provide tentative identities of unknown compounds.SFC with flame ionization detection was used to compare Soxhlet extraction, off-line supercritical fluid extraction (SFE), and on-line SFE of the feces. Although samples obtained by Soxhlet extraction and SFE produced very similar chromatograms, SFE required far less time and consumed much smaller quantities of organic solvent.

Solute retention and selectivity behavior in linear‐temperature‐programmed, constant‐density supercritical fluid chromatography

“…Pinkston et nl. used simultaneous pressure-temperature programming to optimize the separations of free fatty acids and steryl esters in the same sample [16]. In this case, a low initial temperature was necessary to provide adequate retention of the free fatty acids, but resolution of the steryl esters from each other required a higher temperature.…”

Comparison of Supercritical Fluid Extraction with Solvent Sonication for Chemical Warfare Agent Determination in Alkyd Painted Plates

“…As expected, the amount of compound 4 (resulting from the degradation of 1) was less important. (Compounds 1, 2, and 3) Supercritical fluid extraction has been recognized as an important alternative to conventional extraction methods and offers many advantages, such as shorter extraction time, reduced use of organic solvents, and automation of extraction [7][8][9][10]. This last point permits a dramatic reduction in the handling of sample, which is especially attractive for the treatment of highly hazardous samples.…”

Guidelines for successful SFC/MS

“…The analysis of more polar ethoxylated surfactants has been a traditional strength of SFC (39). For example, ethoxylated alcohols are complex mixtures of considerable industrial importance.…”