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Optimisation of olive oil phenol extraction conditions using a high-power probe ultrasonication
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摘要
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鈥?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 渭g GAE g鈭?) 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 猢?#xA0;0.97), precision (RSD: 0.4-9.3%) and sensitivity with LODs/LOQs ranging from 0.03 to 0.16 渭g g鈭? and 0.10-0.51 渭g g鈭? of EVOO, respectively.

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