Optimisation of olive oil phenol extraction conditions using a high-power probe ultrasonication

A new method of ultrasound probe assisted liquid–liquid extraction (US-LLE) combined with a freeze-based fat precipitation clean-up and HPLC–DAD-FLD-MS detection is described for extra virgin olive oil (EVOO) phenol analysis. Three extraction variables (solvent type; 100%, 80%, 50% methanol, sonication time; 5, 10, 20 min, extraction steps; 1–5) and two clean-up methods (n-hexane washing vs. low temperature fat precipitation) were studied and optimised with aim to maximise extracts’ phenol recoveries. A three-step extraction of 10 min with pure methanol (5 mL) resulted in the highest phenol content of freeze-based defatted extracts (667 μg GAE g−1) from 10 g of EVOO, providing much higher efficiency (up to 68%) and repeatability (up to 51%) vs. its non-sonicated counterpart (LLE-agitation) and n-hexane washing. In addition, the overall method provided high linearity (r2 ⩾ 0.97), precision (RSD: 0.4–9.3%) and sensitivity with LODs/LOQs ranging from 0.03 to 0.16 μg g−1 and 0.10–0.51 μg g−1 of EVOO, respectively.