Synergy fusion c18

A Bruker DRX-600 NMR spectrometer, operating at 599.19 MHz for ¹H and 150.858 MHz for ¹³C, using the TopSpin 3.2 software package, was used for the NMR experiments in CD₃OD. The chemical shifts are expressed in δ (parts per million), referring to the solvent peaks δ_H 3.31 and δ_C 49.05 for CD₃OD, with coupling constants, J, in Hertz. Conventional pulse sequences have been used for ¹H-¹H DQF-COSY, ¹H-¹³C HSQC, and HMBC experiments [50 (link)]. ESI-MS experiments [51 (link)] were conducted using a Finnigan LC-Q Deca spectrometer (Thermoquest, San Jose, CA, USA), which was equipped with Xcalibur 3.1 software (Thermoquest, San Jose, CA, USA). Molecular exclusion chromatography was performed on Sephadex LH-20. HPLC separations were performed with a Waters 515 series pump system, equipped with a Waters R401 refractive index detector and a Rheodyne injector (100 μL loop), using Synergy Fusion C₁₈ (250 × 10 mm i.d., 4 μm, Phenomenex, Torrance, CA, USA), at a flow rate of 2 mL/min. Thin-layer chromatography (TLC) was performed with silica gel plates 60F-254 (Delchimica, Naples, Italy) and cerium sulphate spray reagent, and a UV lamp (254 and 366 nm) was used to visualize the spots. Quantitative analysis of the extract was performed with Agilent 1100 HPLC with G1312A Binary Pump, G1315B Diode Array Detector (DAD), and G1328B Injector (Agilent Technologies, Santa Clara, CA, ISA).