Simple strategy for the optimization of solid-phase extraction procedures through the use of solid-liquid...

A practical strategy for the optimization of solid-phase extraction (SPE) systems is presented. Critical SPE volumes (sample loaded, rinsing and elution solvent) are calculated from solid-liquid extraction coefficients and from basic bed parameters determined in simple experiments, using the Lövkist Jonsson model and other expressions derived from the general theory of chromatography. The agreement between calculated and measured volumes is satisfactory, which makes it possible to consider different sorbents and rinsing and elution solvents in the SPE optimization with a relatively low experimental effort. The strategy has been successfully applied to the optimization of a SPE method directed to the selective extraction of aliphatic lactones from wine. Six different reversed-phase sorbents were studied and the one showing maximum extraction selectivity was selected. Wine (50 ml) is extracted in a 200 mg cartridge filled with Bond Elut-ENV resins. Interferences are removed with 20 ml of methanol-water (40:60) with 1% NaHCO3. Elution is carried out with 1.8 ml of dichloromethane. The extract is concentrated to 0.15 ml and analyzed by GC-ion trap MS. Eight odor-active aliphatic gamma and delta lactones (with 8-12 C atoms) from wine are recovered (R > 75%) in an extract free from wine major volatiles. Detection limits are in the 40-300 ng/l range, well below the odor detection threshold of these compounds. Linearity (r2 > 0.996) and precision (average R.S.D. 3.5%) are satisfactory in all cases. The levels in wine of some of these lactones (gamma-octa, undeca and dodecalactones) are reported by first time and results demonstrate that can be present at concentrations above or close to their corresponding odor thresholds.