991 photodiode array detector

Thin layer chromatography (TLC) was performed on precoated silica gel 60 F254 plates (Merck, Darmstadt, Germany) and spot detection was carried out by UV light or by charring with a ninhydrin solution. HPLC analysis was performed on a Waters 600E multisolvent delivery system (Milford, MA, USA), combined with Waters 991 photodiode array detector, using the following methods: (A) column: Nucleosil C8, 7 μm, 125 × 4 mm; flow rate: 1 mL/min; gradient: from 50 to 100% acetonitrile in water within 30 min; (B): column: Zorbax SB-C18, 3.5 μm; 2.1 × 30 nm; gradient: from 50% to 100% acetonitrile in water within 15 min, 100% acetonitrile within 15 min or from 20% to 100% acetonitrile in water within 30 min or from 20% to 100% acetonitrile in water within 30 min; flow rate: 0.4 mL/min; (C): Lichrospher RP-8 (4 × 150 mm, 5 μm); gradient: from 20% to 100% acetonitrile in water within 30 min; flow rate: 1 mL/min. All chromatograms were detected at 265 nm. ES-MS spectra were recorded on a Micromass Platform L.C. (Manchester, UK) at 30 V.

Thin layer chromatography (TLC) was performed on precoated silica gel 60 F₂₅₄ plates (Merck, Darmstadt, Germany) and spot detection was carried out using UV light and/or by charring with a ninhydrin solution. High Performance Liquid Chromatography (HPLC) analysis was performed on a Waters 2695 multisolvent delivery system (Milford, MA, USA), combined with a Waters 991 photodiode array detector. The following columns were used: (A) Lichrosphere RP-8, 5 μm, 125–4 mm; (B) Zorbax SB-C18, 3.5 μm, 30–2.1 mm; (C) Column: Lichrosphere RP-18, 5 μm, 125–4 mm; (D) YMC-Triart C18, 12 nm, S-5 µm, 250–4.6 mm. ESI-MS spectra were recorded on a Waters Micromass ZQ 4000 mass detector (positive mode), controlled using MassLynx 4.1 software (Milford, MA, USA), by direct infusion using a syringe pump at a flow rate of 5 mL/min. Cone voltage was set at 30 V and scan time at 1 s, with the interscan delay at 0.1 s. NMR spectra were recorded on a Brucker DPX 600 MHz instrument (Peoria, IL, USA). The sample spectra were recorded at 25 °C. Chemical shifts (δ) were referenced to the corresponding solvent peaks and are reported in parts per million (ppm). Coupling constants (J) are given in Hertz. Multiplicities are abbreviated as: s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), or combinations thereof.

Thin layer chromatography (TLC) was performed on precoated silica gel 60 F254 plates (Merck, Darmstadt, Germany) and spot detection was carried out by UV light, or by charring with a ninhydrin solution. HPLC analysis was performed on a Waters 600E multisolvent delivery system (Milford, MA, USA), combined with Waters 991 photodiode array detector, using a Nucleosil C8 (4 mm × 125 mm, 7 μm) and a linear gradient from 50 to 100% acetonitrile (containing 0.1% TFA) in water (containing 0.1% TFA) within 30 min at a flow rate of 1 mL/min or Lichroshere RP-8 (4 mm × 150 mm, 5 μm) and a linear gradient from 20 to 100% acetonitrile (containing 0.1% TFA) in water (containing 0.1% TFA) within 30 min at a flow rate of 1 mL/min. Chromatograms were detected at 265 nm. ES-MS spectra were recorded on a Micromass Platform L.C. (Manchester, UK) at 30 V.