1260 infinity quaternary lc apparatus

Optical rotations were measured using a Jasco P-2000 polarimeter at the sodium D line. ECD spectra were recorded using a Jasco-715 (Jasco Europe, Carpi, Italy) spectropolarimeter. NMR spectra were determined on Varian Unity Inova (Varian ,Palo Alto, CA, USA)pectrometers at 700 MHz and 500 MHz; chemical shifts were referenced to the residual solvent signal (CD₃OD: δ_H 3.31, δ_C 49.30). For an accurate measurement of the coupling constants, the one-dimensional ¹H-NMR spectra were transformed at 64-K points (digital resolution: 0.09 Hz). The HSQC spectra were optimized for ¹J_CH = 142 Hz; the ¹³C and ³¹P HMBC experiments for ^2,3J_CH = 8.3 Hz and ³J_PH = 8 Hz, respectively. High-resolution ESI-MS and HR-ESI-HPLC experiments were performed on a Thermo LTQ Orbitrap XL mass spectrometer coupled to a Thermo U3000 HPLC system. Fatty acid methyl esters (FAMEs) were analyzed by GC/MS (Agilent, Cernusco sul Naviglio (Mi), Italy, 6850 series II/5973 Network MSD) on an HP-5MS capillary column (Agilent, 5% Phenyl Methyl Siloxane) (30 m, 0.25 mm φ, 0.25 μm). Helium was used as a carrier gas, injection was in split mode, and the program was as follows: hold 150 °C for 15 min, heat to 300 °C with 5 °C/min, hold 300 °C for 10 min. High performance liquid chromatography (HPLC) separations were achieved on an Agilent 1260 Infinity Quaternary LC apparatus equipped with a Diode-Array Detector (DAD).