The new screening method for rapid evaluation of major phenolic compounds in apples has been developed. Suitability of coupling HPLC/UHPLC separation with the diode-array detection and universal charged aerosol detection with respect to the presence of interfering substances was tested. Characteristics of both detection techniques were compared and method linearity, limits of detection and quantitation, and selectivity of them determined. Student t-test based on slopes of calibration plots was applied for the detailed comparison. The diode-array detection provided the best results regarding sensitivity and selectivity of the developed method in terms of evaluation of phenolics profiles. The response of the charged aerosol detector was negatively affected by co-eluting substances during rapid-screening analyses. Coulometric detection was used for advanced characterization of extracts in terms of antioxidant content and strength to obtain more complex information concerning sample composition. This detection also allowed evaluation of unidentified compounds with antioxidant activity. HPLC/UHPLC separation using a combination of diode-array and coulometric detectors thus represented the best approach enabling quick, yet complex characterization of bioactive compounds in apples.

New extraction protocols, gas-expanded liquid extraction (GXLE), and ultrasound extraction (UE) have been optimized with an emphasis on using green solvents and maximizing the extraction of 14 selected phenolic compounds, including flavonoid-based compounds and phenolic acids from dried apples. The design of the experiments’ approach was applied to optimize the main extraction parameters. Fine tuning included optimization of the flow rate in GXLE and the extraction time for GXLE and UE. Optimized GXLE was carried out with CO2–ethanol–water (34/53.8/12.2; v/v/v) at a flow rate of 3 mL/min at a temperature of 75 °C and pressure of 120 bar for 30 min. UE with ethanol–water 26/74 (v/v) lasted for 10 min at 70 °C. Both methods differed in solvent consumption and sample throughput, while providing a comparable total phenolic content of 2442 µg/g with an RSD < 10% and 2226 µg/g with RSD < 6%, for GXLE and UE, respectively. Both methods were used in determining the phenolic compounds in five apple cultivars, ‘Angold’, ‘Artiga’, ‘Golden Delicious’, ‘Meteor’, and ‘Topaz’. Phenolic profiles were plotted with chlorogenic acid, catechin, epicatechin, hirsutrin, phloridzin, and guaiaverin as the main components. Statistical evaluation, including pair t-test, Bland–Altman test, and linear regression did not reveal any differences between UE and GXLE results.

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