Use of volatile organic solvents in headspace liquid-phase microextraction by direct cooling of the organic drop using a simple cooling capsule

A low-cost and simple cooling-assisted headspace liquid-phase microextraction device for the extraction and determination of 2,6,6-trimethyl-1,3 cyclohexadiene-1-carboxaldehyde (safranal) in Saffron samples, using volatile organic solvents, was fabricated and evaluated. The main part of the cooling-assisted headspace liquid-phase microextraction system was a cooling capsule, with a Teflon microcup to hold the extracting organic solvent, which is able to directly cool down the extraction phase while the sample matrix is simultaneously heated. Different experimental factors such as type of organic extraction solvent, sample temperature, extraction solvent temperature, and extraction time were optimized. The optimal conditions were obtained as: extraction solvent, methanol (10 mu L); extraction temperature, 60 degrees C; extraction solvent temperature, 0 degrees C; and extraction time, 20 min. Good linearity of the calibration curve (R-2 = 0.995) was obtained in the concentration range of 0.01-50.0 mu g/mL. The limit of detection was 0.001 mu g/mL. The relative standard deviation for 1.0 mu g/mL of safranal was 10.7% (n = 6). The proposed cooling-assisted headspace liquid-phase microextraction device was coupled (off-line) to high-performance liquid chromatography and used for the determination of safranal in Saffron samples. Reasonable agreement was observed between the results of the cooling-assisted headspace liquid-phase microextraction high-performance liquid chromatography method and those obtained by a validated ultrasound-assisted solvent extraction procedure.