Ultrasound-assisted extraction of polyphenols from pine needles (Pinus elliottii): Comprehensive insights from RSM optimization, antioxidant activity, UHPLC-Q-Exactive Orbitrap MS/MS analysis and kinetic model

Abstract

Extracting polyphenolic bioactive compounds from Pinus elliottii needles, a forestry residue, promises economic and environmental benefits, however, relevant experimental data are lacking. Herein, a comprehensive investigation of the polyphenolic composition of pine needles (PNs) was carried out. Ultrasound-Assisted Extraction (UAE) was applied to extract the polyphenolic compounds of pine needles. The optimal conditions of extracts were determined by Response Surface Methodology (RSM). The maximum total phenolic content (TPC) of 40.37 mg GAE/g PNs was achieved with solid-liquid ratio of 1:20, 60 % ethanol, and 350 W for 25 min at 45 °C. Polyphenolic extracts showed antioxidant activity in scavenging free radicals and reducing power (DPPH, IC₅₀ 41.05 μg/mL; FRAP 1.09 mM Fe²⁺/g PNs; ABTS, IC₅₀ 214.07 μg/mL). Furthermore, the second-order kinetic model was also constructed to describe the mechanism of the UAE process, with the extraction activation energy estimated at 12.26 kJ/mol. In addition, 37 compounds in PNs were first identified by UHPLC-Q-Exactive Orbitrap MS/MS, including flavonoids and phenolic acids. The results suggest that Ultrasound-Assisted is an effective method for the extraction of natural polyphenolic compounds from pine needles and this study could serve as a foundation for utilizing phenolics derived from PNs in the food and pharmaceutical industries.

Keywords: Antioxidant activity; Kinetic Model; Pinus elliottii needles; Response Surface Methodology; UHPLC-Q-Exactive Orbitrap MS/MS; Ultrasound-Assisted Extraction.