Lcq advantage max mass spectrometer

Optical rotations were measured on a JASCO P-2000 polarimeter, UV/Vis data were obtained using a Beckman DU800 spectrophotometer, and IR spectra were recorded on a Nicolet 100 FT-IR spectrometer. NMR data were obtained on a JEOL ECZ 500 NMR spectrometer equipped with a 3 mm inverse probe (H3X), the 1,1-ADEQUATE experiment was performed on a Bruker AVANCE III 600 MHz NMR with a 1.7 mm dual tune TCI cryoprobe. NMR data were recorded in either DMSO-d₆ or methanol-d₄ and adjusted to the residual solvent peak (DMSO-d₆ δ_H 2.50, δ_C 39.52; methanol-d₄ δ_H 3.31, δ_C 49.00). For HPLC-MS analysis, a Thermo Finnigan Surveyor HPLC system with a Phenomenex Kinetex 5 μm C18 100 × 4.6 mm column coupled to a Thermo-Finnigan LCQ Advantage Max Mass Spectrometer was used. Samples were analyzed using a linear gradient with (A) H2O + 0.1% FA to (B) CH₃CN + 0.1% FA at a flow rate of 0.6 ml/min and UV detection at 220 nm, 254 nm and 280 nm. For HR-ESI-MS analysis, an Agilent 6530 Accurate Mass QTOF mass spectrometer was used in the positive ion mode. Semi-preparative HPLC was performed on a Thermo Fisher Scientific HPLC system with a Thermo Dionex UltiMate 3000 pump, RS autosampler, RS diode array detector, and automated fraction collector. All solvents were HPLC grade except for H₂O, which was purified by a Millipore Milli-Q system before use.

Low-resolution LC-MS/MS analysis was done on a Thermo Finnigan LCQ Advantage Max mass spectrometer coupled to an HP1050 HPLC. A gradient of 10–100% methanol with 0.02% formic acid over 25 minutes was used for separation. The ESI conditions were set with the source voltage at 5 kV and capillary temperature at 250°C. The detection window was set from 200 to 2000 Da, collision energy was at 35%, isolation width was 3 m/z, with three data dependent MS² events per MS¹ and dynamic exclusion. High resolution LC-MS/MS data was collected on a Bruker impact II qTOF in positive mode with the detection window set from 50 to 1500 Da, on a UPLC gradient of 10–100% acetonitrile with 0.02% formic acid over 17 minutes. The ESI conditions were set with the capillary voltage at 4.5 kV. The detection window was set from 50 to 1500 Da and the top three precursor ions from each MS¹ scan were subjected to collision energies of 12 eV, 48eV, and 60eV for a total of nine data dependent MS² events per MS¹ with dynamic exclusion.