Ana-Maria Drăghici-Popa

Selecting factors that significantly affect the extraction process and optimizing them are essential to obtain high extraction efficiency. This study aimed at optimizing the ultrasonic-assisted extraction (UAE) of polyphenols from Romanian blackthorn fruits using aqueous solutions of ethanol as green extraction solvents. Six process factors, including solvent/plant material ratio (R_LS = 4.95–15.1 cm³/g), ethanol concentration in the extraction solvent (c_et = 16.4–83.6%), extraction temperature (t = 30–70 °C), pH of the solvent (pH = 2–7), amplitude of the ultrasonic probe (A = 30–70%), and extraction time (τ = 5–15 min), were screened and optimized based on a Plackett–Burman design (PBD) and a central composite design (CCD). Statistical analysis indicated that R_LS, c_et, and t significantly affected the process response variables in terms of total phenolic content (TPC), total anthocyanin content (TAC), and antioxidant capacity (AC). Under optimal conditions (R_LS,opt = 15.1 cm³/g, c_et,opt = 33.2%, t_opt = 66.8 °C, pH_opt = 7, A_opt = 50%, and τ_opt = 10 min), the following levels of response variables were experimentally determined: TPC_opt = 14.45 ± 0.718 mg GAE/g DM, TAC_opt = 0.405 ± 0.057 mg C3GE/g DM, and AC_opt = 16.75 ± 1.144 mg TE/g DM. Six phenolic compounds were identified in the extract obtained at optimal levels of process factors, i.e., rutin (7.12 ± 0.06 mg/100 g DM), protocatechuic acid (6.83 ± 0.01 mg/100 g DM), neochlorogenic acid (4.88 ± 0.01 mg/100 g DM), vanillic acid (3.70 ± 0.01 mg/100 g DM), chlorogenic acid (1.93 ± 0.02 mg/100 g DM), and caffeic acid (1.51 ± 0.01 mg/100 g DM).

Grape marc is a by-product resulting from the winemaking industry that still contains beneficial compounds that can be valorized. Thus, we report here the possibility of using polyphenolic extracts of grape marc origin to obtain sun protection creams. The extractions were performed in ethanol and acetone solutions using pomace from different grape varieties (Merlot, Bläufrankisch, Fetească Neagră, Isabella) as a raw material. The obtained extracts were analyzed in order to determine the total phenolic content, the antioxidant activity, and the sun protection factor (SPF) via Mansur spectrophotometric assay. The best results were achieved using 70% ethanol in water as a solvent. The extracts with the highest potential photoprotective effects are from the Merlot variety (SPF_{spectrophotometric} = 7.83 ± 0.76). The sunscreens were prepared using the 70% ethanolic extract of the Merlot variety evaporated to dryness, redissolved in either distilled water or ethanol. The SPF estimated in vitro via the COLIPA method showed values of 14.07 ± 1.50 and 11.46 ± 1.32 for the aqueous and ethanolic extracts, respectively, when working with a cream to polyphenolic extract a ratio of 1/1 (w/w). At the same time, the use of aqueous polyphenolic extracts ensures the better stability of creams compared with the ethanolic ones.

This study aimed at establishing the optimal conditions for the classic extraction of phenolic compounds from Prunus spinosa L. fruits. The effects of different parameters, i.e., ethanol concentration in the extraction solvent (mixture of ethanol and water), operation temperature, and extraction time, on process responses were evaluated. Total phenolic content (TPC), total anthocyanin content (TAC), antioxidant capacity (AC), and contents of protocatechuic acid (PA), caffeic acid (CA), vanillic acid (VA), rutin hydrate (RH), and quercetin (Q) of fruit extracts were selected as process responses. A synergistic effect of obtaining high values of TPC, TAC, AC, PA, and VA was achieved for the extraction in 50% ethanol at 60 °C for 30 min. At a higher level of process temperature, the extraction of protocatechuic acid and vanillic acid was enhanced, but the flavonoids, i.e., rutin hydrate and quercetin, were degraded. A lower temperature should be used to obtain a higher amount of flavonoids. TPC, TAC, AC, and phenolic acid contents (PA, CA, and VA) in the extract samples obtained at an ethanol concentration of 50–100%, a temperature of 30–60 °C, and an extraction time of 30 min were strongly directly correlated.