New reversed phase dispersive liquid–liquid microextraction method for the determination of phenolic compounds in virgin olive oil by rapid resolution liquid chromathography with ultraviolet–visible and mass spectrometry detection

• DLLME directly over a non-aqueous sample is utilized with a more polar solvent (RP-DLLME).
• RP-DLLME provides a simple, fast, efficient and eco-friendly procedure for extraction.
• Rapid resolution LC method provides better performance with shorter analysis times.
• Two different detectors are intended expanding the utility of the developed procedure.

The determination of phenolic compounds in virgin olive oil using a new reversed phase dispersive liquid–liquid microextraction (RP-DLLME) procedure coupled with rapid resolution liquid chromatography-diode array and mass spectrometry detection (RRLC-DAD–MS) have been performed. A rapid resolution Zorbax Eclipse XDB-C18 column (4.6 mm × 50 mm, 1.8 μm particle size) has been employed and eighteen phenolic compounds belonging to different families have been identified and quantified spending a total time of 26 and 13 min with UV–visible and MS detection, respectively. Response surface methodology has been applied by means of a central composite design for the optimization of the variables affecting the extraction procedure searching for the best recovery. The validation of the methods was performed through the establishment of the external standard calibration curves and the analytical figures of merit. Limits of detection ranging from 10 to 400 ng mL−1 and 1 to 200 ng mL−1 were achieved using UV–visible and MS detection, respectively. The extraction of phenolic compounds from virgin olive oil was performed in a simple and rapid way by RP-DLLME with ethanol:water 60:40 (v/v) as extracting solvent and 1,4-dioxane as disperser solvent. The quantification of the phenolic compounds in virgin olive oils from different olive varieties was carried out by means of the standard addition method and, finally the procedure for the sample treatment was validated using the well established solid phase extraction procedure with Diol cartridges.