Vortex-assisted liquid–liquid–liquid microextraction (VALLLME) technique: A new microextraction approach for direct liquid chromatography and capillary electrophoresis analysis

•A new three phase liquid microextraction technique named VALLLME is proposed.•The proposed technique is suitable for the direct HPLC and CE analyses.•VALLLME comprises of VALLME followed by μ-VALLE procedure.•The superiority of the proposed VALLLME over VALLME and HF-LPME was demonstrated.•This technique was used for the determination of carvedilol in biological fluids.

A new, rapid and sensitive microextraction technique named vortex-assisted liquid–liquid–liquid microextraction (VALLLME) is proposed. The complete extraction process involves two steps. First, a vortex-assisted liquid–liquid microextraction (VALLME) procedure was used to extract the analytes from a relatively large volume of sample (donor phase) to a small volume of organic solvent (intermediate phase). Next, a micro-vortex-assisted liquid–liquid extraction (µ-VALLE) was used to extract the target analytes from the intermediate phase to a smaller volume of aqueous solution (acceptor phase). The final extract (acceptor phase) can be directly injected into the high performance liquid chromatography or capillary electrophoresis units without any further treatments. The selection of the intermediate phase and the manipulation of pH are key parameters that ensure good extraction efficiency of the technique. The proposed technique has been successfully applied for the determination of carvedilol (used as model analyte) in biological fluid samples. The optimum extraction conditions were: toluene as intermediate phase (150 μL); pH of the donor phase, 9.5; vortex time of the VALLME, 45 s (maximum speed, 2500 rpm); 0.1 M HCl (15 μL) as acceptor phase; vortexing time of the µ-VALLME, 75 s (maximum stirring speed, 2500 rpm) and salt concentration in the donor phase, 5% (w/v). Under these conditions, enrichment factors of 51- and 418-fold for VALLME step and VALLLME procedure, respectively, were achieved.

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