1D and 2D NMR spectra were acquired in a Bruker UltrashieldTM Plus 600MHz NMR. MS analysis of the obtained compounds was performed with an LTQ ThermoScientific Orbitrap and an Agilent QQQ 6460. All solvents used during the experimental procedure were of analytical grade or redistilled. Additionally, the solvents used for Liquid Chromatography were HPLC grade and purified by filtration through ion- and carbon-exchange resins. The stationary phase for low pressure CC was silicon dioxide (Silica gel 40–63μm/Silica flash). Aluminum and glass plates, coated with silicon dioxide (Silica gel 60 F254) were used for TLC and preparative TLC, respectively, and the obtained chromatograms were observed in a CAMAG TLC Visualizer at 254 and 366 nm. For the HPLC analysis, a THERMO Finnigan Spectra System was used, coupled with a PDA UV Detector. The column used was a Lichrosorb RP-18 with dimensions of 5 μm and 250×4 mm.
Finnigan spectra system
Manufactured by Thermo Fisher Scientific
Sourced in United States
The Finnigan Spectra System is a laboratory instrument designed for spectroscopic analysis. It is capable of performing various spectroscopic techniques, such as mass spectrometry and nuclear magnetic resonance spectroscopy, to identify and quantify chemical compounds.
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Lab products found in correlation
3 protocols using finnigan spectra system
1
Analytical Techniques for Compound Characterization
2
Ascorbic Acid Quantification in Pepper Fruit
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For ascorbic acid, the pericarp tissue of pepper fruit was chopped into small pieces with a ceramic knife, and 2.5 g crushed pericarp tissue was immediately mixed with 5 mL 2% metaphosphoric acid and ground thoroughly in a ceramic mortar, as reported by Mikulic-Petkovsek et al. [68 (link)]. The samples were left on a shaker for 30 min and then centrifuged at 9000× g rpm for 7 min at 4 °C (5801R; Eppendorf, Hamburg, Germany). The supernatants were filtered through cellulose filters (Chromafil A-20/25; Macherey-Nagel, Dueren, Hamburg, Germany), transferred to vials, and analyzed by HPLC (Finnigan spectra system; Thermo Scientific, Waltham, MA, USA), as previously reported [69 (link)]. The ascorbic acid concentrations were determined using the calibration curves established using an appropriate external standard, and the data are expressed as mg·(100 g)–1 FW.
3
Quantitative Oleuropein Analysis in Rabbit Plasma
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All solvents used were of liquid chromatography-mass spectrometry (LC-MS) grade and have been purchased from Fluka/Riedel-de Haën (Buchs, Switzerland). Purified oleuropein from olive leaves [95% purity assessed using analytical reversed phased (RP)-high-performance liquid chromatography (HPLC) employing a Thermo Finnigan Spectra system (column: LiChrosorb RP-18, 250 × 4.0 mm, 5 µm, elution solvent: H2O: acetonitrile gradient, flow:1 mL/min, UV-detection: 254 nm)] was used in this study.
Plasma levels of oleuropein were analyzed using a methodology developed in our laboratory, modified and partially validated for the analysis of rabbit plasma. Briefly an ultra-high-performance liquid chromatography (UHPLC) with high-resolution mass spectrometry (HRMS) has been employed for the analysis of the circulating levels of the oleuropein in rabbit plasma, with the samples being pre-treated by solid phase extraction [17] (link).
Plasma levels of oleuropein were analyzed using a methodology developed in our laboratory, modified and partially validated for the analysis of rabbit plasma. Briefly an ultra-high-performance liquid chromatography (UHPLC) with high-resolution mass spectrometry (HRMS) has been employed for the analysis of the circulating levels of the oleuropein in rabbit plasma, with the samples being pre-treated by solid phase extraction [17] (link).
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