One-step sustainable extraction of Silymarin compounds of wild Algerian milk thistle (Silybum marianum) seeds using Gas Expanded Liquids

J Chromatogr A. 2022 Jul 19:1675:463147. doi: 10.1016/j.chroma.2022.463147. Epub 2022 May 18.

Abstract

This work reports the application of Gas Expanded Liquid (GXL) extraction to concentrate the flavonolignan fraction (silymarin) and taxifolin from Silybum marianum seeds, which have proven to be highly valuable health-promoting compounds. GXL using green solvents was used to isolate silymarin with the objective of replacing conventional methods. In one hand, the effect of different compositions of solvents, aqueous ethanol (20%, 50% or 80% (v/v)) at different CO2/liquid (25, 50 and 75%) ratios, on the GXL extraction was investigated. The obtained extracts have been chemically and functionally characterized by means of UHPLC-ESI-MS/MS (triple quadrupole) and in-vitro assays such as anti-inflammatory, anti-cholinergic and antioxidant. Results revealed that the operating conditions influenced the extraction yield, the total phenolic content and the presence of the target compounds. The best obtained yield was 55.97% using a ternary mixture of solvents composed of CO2:EtOH:H2O (25:60:15) at 40 °C and 9 MPa in 160 min. Furthermore, the results showed that obtained extracts had significant antioxidant and anti-inflammatory activities (with best IC50 value of 8.80 µg/mL and 28.52 µg/mL, respectively) but a moderate anti-cholinesterase activity (with best IC50 value of 125.09 µg/mL). Otherwise, the concentration of silymarin compounds in extract can go up to 59.6% using the present one-step extraction method without further purification, being silybinA+B the predominant identified compound, achieving value of 545.73 (mg silymarin/g of extract). The obtained results demonstrate the exceptional potential of GXL to extract high-added values molecules under sustainable conditions from different matrices.

Keywords: Gas-expanded liquid extraction; Green solvents; Neuroprotective effect; Silybum marianum; UHPLC-ESI-MS/MS.

MeSH terms

  • Algeria
  • Antioxidants / analysis
  • Carbon Dioxide / analysis
  • Chromatography, High Pressure Liquid / methods
  • Ethanol / analysis
  • Flavonoids / analysis
  • Plant Extracts / chemistry
  • Seeds / chemistry
  • Silybum marianum* / chemistry
  • Silymarin*
  • Solvents / chemistry
  • Tandem Mass Spectrometry

Substances

  • Antioxidants
  • Flavonoids
  • Plant Extracts
  • Silymarin
  • Solvents
  • Carbon Dioxide
  • Ethanol