Stepwise Elution of a Three‐phase Solvent System in Centrifugal Partition Extraction: A New Strategy for the Fractionation and Phytochemical Screening of a Crude Bark Extract

Abstract

Centrifugal partition extraction in the elution mode using a three-phase solvent system can thus be proposed as an efficient and cost-effective alternative for a rapid fractionation of crude bark extracts and for an effective screening of potentially active secondary metabolites.

Bio-Guided Isolation of Methanol-Soluble Metabolites of Common Spruce (Picea abies) Bark by-Products and Investigation of Their Dermo-Cosmetic Properties

“…The column design used for this work, with only 231 partition cells (FCPE300 ® ), offers the possibility to rapidly fractionate multi-gram amounts of natural mixtures and thus to collect fractions in sufficient quantities for further chemical analyses and biological assays. In addition, the use of a triphasic solvent system composed of n-heptane, MtBE, CH 3 CN, and water was already reported as an efficient method to fractionate natural compounds from barks in a wide range of polarity [13].…”

“…Figure 2 shows the HCA correlation heat map. After entering the values of each chemical shift belonging to the same cluster into the local database containing 13 C-NMR data of natural compounds including known metabolites from Picea abies, nine compounds were directly identified, including one diterpene, dehydroabietic acid (1), three flavonoids, (+)-catechin (5), taxifolin (4) and taxifolin-3 -O-glucoside (9), two stilbene glycosides, E-astringin (8) and E-isorhapontin (7), one lignan, pinoresinol (3), one phenolic derivative, 3,4-dimethoxyphenyl-β-D-glucopyranoside (13), and saccharose (14) (Figure 2A). The chemical structures of identified compounds were confirmed by HRMS analysis.…”

“…The major compounds contained in the CPC fractions were firstly identified by using a recently developed 13 C-NMR-based dereplication procedure. All CPC fractions (from I to XIX) were analyzed by 13 C-NMR spectroscopy.…”

“…All CPC fractions (from I to XIX) were analyzed by 13 C-NMR spectroscopy. Automatic peak picking and alignment of 13 C-NMR signals across spectra of the fraction series resulted in a table with 19 columns (one per fraction) and 571 raws (one per chemical shift bin containing at least one signal in at least one fraction).…”

“…All CPC fractions (from I to XIX) were analyzed by 13 C-NMR spectroscopy. Automatic peak picking and alignment of 13 C-NMR signals across spectra of the fraction series resulted in a table with 19 columns (one per fraction) and 571 raws (one per chemical shift bin containing at least one signal in at least one fraction). By applying hierarchical clustering analysis on the lines of this dataset, statistical correlations between 13 C-NMR resonances belonging to individual molecular structures within the fractions were readily visualized as well-defined chemical shift clusters colored in yellow in front of the corresponding dendrograms.…”