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The in-line coupling of the pressurized liquid extraction with a solid-phase adsorbent and a UV–Vis detector for the simultaneous extraction and separation of bioactive compounds from yerba mate (PLE-SPE-UV) was carried out in two stages. In the first stage, water was used as a solvent, while in the second stage, ethanol was used. For the optimization of the method, different adsorbents (Sepra C18-E, Isolute C18-EC, and Strata-X C18), temperatures (40–80 °C), solvent flow-rate (1–3 mL/min), and pH (4.0 and 8.0) were evaluated. By using a UV–Vis detector on-line, it is possible to monitor the process in real-time. The developed method allowed obtaining similar or higher recoveries of all the compounds classes than other methods, such as ultrasound-assisted extraction, stirring, maceration, and pressurized liquid extraction alone, in addition to separating them into fractions. The developed method could be used as sample preparation for the analysis of different compounds classes from mate.

Pomegranate (Punica granatum L.) has been used in traditional herbal medicine by several cultures as an anti‐inflammatory, antioxidant, antihyperglycemic, and for treatment and prevention of cancer and other diseases. Different parts of the fruit, extraction methods, and solvents can define the chemical profile of the obtained extracts and their biological activities. This study aimed to characterize the chemical profile of peel extracts collected using different extraction solvents and their biological effects on the cell cycle and apoptosis of THP‐1 leukemic cells. Aqueous extract presented the highest content of punicalagins (α pun = 562.26 ± 47.14 mg/L and β pun = 1,251.13 ± 22.21 mg/L) and the lowest content of ellagic acid (66.38 ± 0.21 mg/L), and it promoted a significant impairment of the cell cycle S phase. In fact, punicalagin‐enriched fraction, but not an ellagic acid‐enriched fraction, caused an S phase cell cycle arrest. All extracts increased the number of apoptotic cells. Punicalagin‐enriched fraction increased the percentage of cells with fragmented DNA, which was intensified by ellagic acid combination. The treatment combining punicalagin and ellagic acid fractions increased the apoptotic cleaved PARP1 protein and reduced the activation of the growth‐related mTOR pathway. Thus, these results evidence that solvent choice is critical for the phenolic compounds profile of pomegranate peel extracts and their biological activities., The main aim of this study was to assess and compare the differences in the chemical profile of pomegranate peel extracts obtained using different extraction solvents and how does it affect their biological properties.