640 ir ftir spectrophotometer

Organogel samples were placed directly on the attenuated total reflection (ATR) crystal. FTIR spectra of the organogels were measured at 4 cm⁻¹ resolution from 650 to 4000 cm⁻¹ using a Varian 640-IR FTIR spectrophotometer (Varian Medical System, Palo Alto, CA, USA). Each spectrum was composed of 32 scans at room temperature (25 °C) [8 (link)].

UV and IR spectra were recorded on a Varian Cary 50 UV-Vis and Varian 640-IR FT-IR spectrophotometer, respectively. Optical rotations were measured on a Rudolph Autopol^® IV automatic polarimeter. NMR spectra were determined on a Bruker 500 MHz NMR spectrometer at 500 MHz for ¹H and 125 MHz for ¹³C-NMR (internal standard: TMS). Negative-ion mode ESI-Q-Orbitrap MS were obtained on a Thermo UltiMate 3000 UHPLC instrument (Thermo, Waltham, MA, USA).
Column chromatographies (CC) were performed on macroporous resin D101 (Haiguang Chemical Co., Ltd., Tianjin, China), silica gel (48–75 μm, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China), ODS (40–63 μm, YMC Co., Ltd., Tokyo, Japan), and Sephadex LH-20 (Ge Healthcare Bio-Sciences, Uppsala, Sweden). Preparative high performance liquid chromatography (pHPLC) column, Cosmosil 5C₁₈-MS-II (20 mm i.d. × 250 mm, Nakalai Tesque, Inc., Tokyo, Japan) were used to separate the constituents.

IR spectra were measured on a Varian 640-IRFT-IR spectrophotometer. NMR spectra were run on a 300 MHz Varian Magnet Oxford YH300 Console Mercury Plus 300 (¹³C) and Bruker Avance III 600 MHz (¹H, COSY, HMBC, HSQC). The chemical shift (δ) values are in ppm (parts per million) referenced with TMS (tetramethylsilane). High-resolution mass spectra were obtained using an AB SCIEX TripleTOF 5600+ mass spectrometer in the positive mode by direct infusion. Diol SPE fractionation of the extract was performed in DIO Spe-ed SPE cartridges (Applied Separations, Allentown, PA, USA) using hexane/CH₂Cl₂ (9:1—A), CH₂Cl₂/EtOAc (20:1—B), EtOAc (C), EtOAc/MeOH (5:1—D) and MeOH (E). Silica gel 60 (0.04 mm—0.063 mm, 230–400 mesh) using hexane with 3% EtOAc increasing polarity until 100% MeOH and Sephadex LH-20(CH₂Cl₂/4MeOH 1:1) were used for column chromatography. Silica gel plates were used for TLC. For PTLC, preparative layer with UV₂₅₄, 500 microns were used with hexane/CH₂Cl₂ (4:6).