Lct premier xe mass spectrometer

The four ethanol extracts from glanded and glandless cottonseed were analyzed by HPLC-UV-MS on a Waters Alliance (2695), PDA detector (996), and a Waters LCT Premier-XE mass spectrometer (ToF) with an electrospray ionization (ESI) source. UV was detected at 210–600 nm. MS was detected at 200–1000 m/z. ESI conditions were: positive mode: 3500 V capillary voltage, 70 V cone voltage, 350 °C desolvation temperature, 105 °C source temperature, 450 l/min desolvation gas, 50 l/min cone gas; negative mode: 3000 V capillary voltage. A Synergy Hydro RP 4 µm 3.0 × 150 mm column (Phenomenex, Torrance, CA) was used with a gradient of acetonitrile/0.1% formic acid from 0.5% to 10% acetonitrile over 2 min, followed by a gradient to 19% over 9 min, to 37% over 3 min, and to 80% over 3 min. Equilibration at initial conditions was for 10 min between runs. Flow rate was 0.3 ml/min and column temperature was 30 °C. A 75 μl injection of a 100% DMSO solution of the extract was analyzed. Gossypol standard in DMSO was prepared at 2 pg/µl and LPS standard in water was prepared at 100 ng/µl. A standard curve was determined for gossypol for quantification based on peak area of its m/z 517.22 ± 0.03 in the negative ESI chromatogram.

All reagents and chemicals were brought from Sigma-Aldrich (Schnelldorf, Germany) and Alfa Aesar (Ward Hill, MA, USA). The Melting points were collected by utilizing the SMP-II Digital Melting Point instrument. Nuclear magnetic resonance spectroscopy (NMR) for ¹H and ¹³C atoms were conducted on a Bruker instrument (500 MHz-Avance III High-Performance Digital) at the Faculty of Science, University of Jordan, Jordan. High-resolution mass spectroscopy was performed by utilizing a Waters LCT Premier XE Mass Spectrometer at Pharmacy Faculty, Gazi University, Ankara, Turkey.

All used chemical reagents and starting materials were ordered from Alfa Aesar (UK) and Sigma-Aldrich (Germany). All used cancer, and normal cell lines were ordered from ATCC. The SMP-II Digital Melting Point Apparatus was used without correcting to find the melting points (M.P.) of all final compounds. ¹H-NMR and ¹³C-NMR spectra were recorded by using DMSO-d₆ as the solvent and were conducted by the Bruker 500 J MHz-Avance III High-Performance Digital FT-NMR spectrometer at the Chemistry department, Science Faculty, in the University of Jordan, Amman-Jordan. However, the chemical shifts were recorded accordingly as δ (ppm). The used mass instrument was the High-resolution mass spectrometer (HRMS) at the Phramceuteical chemistry department, Pharmacy Faculty in Gazi University, Ankara-Turkey, this instrument uses the Waters LCT Premier XE Mass Spectrometer which is coupled to an AQUITY Ultra Performance Liquid Chromatography (UP-LC) system (Waters Corporation, Milford, MA, USA) [50 (link)].