Phenolic compounds from virgin olive oil obtained by natural deep eutectic solvent (NADES): effect of the extraction and recovery conditions

Environmentally friendly natural deep eutectic solvents (NADES) have been shown to efficiently extract a wide range of phenolic compounds from virgin olive oil (VOO). The objective of this work was to optimize the yield of olive oil phenols extracted by NADES based on xylitol/choline choride (Xyl/ChCl). Different extraction and recovery conditions were investigated, including the effect of different extraction operating parameters (temperature, time, VOO:NADES ratio) and subsequent recovery conditions (XAD resin height, wash-water and eluent volume and pH). The highest concentration of phenols (555.36 mg/kg VOO) was obtained from extraction at 40 °C for 1 h, with a 1:1 ratio, using an adsorption resin XAD-16 with bed height of 10 cm, 250 mL acidified wash-water and 300 mL EtOH 100% as eluent. No statistically significant loss of the sum of phenolic compounds was observed when compared with the concentration values obtained by direct analysis in HPLC without the elimination of NADES. Additionally, a sequential desorption with different concentration of ethanol was used to determine the effect of the solvent concentration on polyphenol yield. Polar compounds, such as hydroxytyrosol and tyrosol, were recovered at 81.7% and 83.6%, respectively with 50 and 80% ethanol; however, 100% ethanol was required for the complete elution of oleacein (3,4-DHPEA-EDA) and oleocanthal (p-HPEA-EDA). In this paper we present an effective process for the extraction of polyphenols from VOO by NADES for direct analysis in HPLC and for the recovery and concentration of polyphenols by removing the solvent (NADES) with no losses of yield and solvent recycling.