The conversion of plant byproducts, which are phenolic-rich substrates, to valuable co-products by implementing non-conventional extraction techniques is the need of the hour. In the current study, ultrasound- (UAE) and microwave-assisted extraction (MAE) were applied for the recovery of polyphenols from peach byproducts. Two-level screening and Box–Behnken design were adopted to optimize extraction efficiency in terms of total phenolic content (TPC). Methanol:water 4:1% v/v was the extraction solvent. The optimal conditions of UAE were 15 min, 8 s ON-5 s OFF, and 35 mL g−1, while MAE was maximized at 20 min, 58 °C, and 16 mL g−1. Regarding the extracts’ TPC and antioxidant activity, MAE emerged as the method of choice, whilst their antiradical activity was similar in both techniques. Furthermore, a liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated to determine chlorogenic acid and naringenin in byproducts’ extracts. 4-Chloro-4′-hydroxybenzophenone is proposed as a new internal standard in LC-MS/MS analysis in foods and byproducts. Chlorogenic acid was extracted in higher yields when UAE was used, while MAE favored the extraction of the flavonoid compound, naringenin. To conclude, non-conventional extraction could be considered as an efficient and fast alternative for the recovery of bioactive compounds from plant matrices.
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