Silica gel 100 c18 reversed phase

UV IKON 940 spectrophotometer was used to measure UV spectra. A Bruker Apex III Fourier-transform ion cyclotron resonance (FTICR) mass spectrometer (Bruker Daltonics, Billerica, USA) including an Infinity™ cell and a 7.0 Tesla superconducting magnet (Bruker, Karlsruhe, Germany) was used to perform mass spectrometric studies. A Bruker DRX-600 MHz Ultrashield spectrometer (Bruker BioSpin, Billerica, MA, USA) was utilized to measure NMR spectra. Chromatographic separation of the active compounds was performed on Silica gel 60 (70-230 mesh, Merck, Darmstadt, Germany), Silica gel 100 C₁₈-Reversed phase (0.04–0.063 mm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Pharmacia Fine Chemicals Inc., Uppsala, Sweden). Monitoring of the isolation process was carried out on TLC plates with Silica gel 60 F₂₅₄ (Merck, Darmstadt, Germany).

UV spectra were recorded in MeOH using a UV IKON940 spectrophotometer.1D and 2D NMR spectra (chemical shifts in ppm and coupling constants in Hz) were recorded on a Bruker DRX-600 MHz Ultrashield spectrometer (Bruker BioSpin, Billerica, MA, USA) using DMSO-d6 as solvent, with TMS as the internal reference. Column chromatographic separations were performed on silica gel 60 (70–230 mesh, Merck, Darmstadt, Germany), Silica gel 100C₁₈-Reversed phase (0.04–0.063 mm, Merck, Darmstadt, Germany) and Sephadex LH-20(Pharmacia Fine Chemicals Inc., Uppsala, Sweden). TLC analysis was performed on pre-coated TLC plates with silica gel 60 F₂₅₄(Merck, Darmstadt, Germany). Purification of the isolated compounds was performed on a preparative HPLC Agilent1200 equipped with a multi-wavelength detector and ZorbaxSB-C18 column (9.4 × 250 mm).