Uplc rs ultimate 3000 q exactive hybrid quadrupole orbitrap mass spectrometer

Thin layer chromatographic analyses were performed using TLC silica gel, pore size 60 Å 60, F₂₅₄ on aluminum sheets (Merck Millipore, Darmstadt, Germany). For column chromatographic analyses (CC.), various stationary phases were used, including silica gel, pore size 60 Å 60, mesh 70–230 (Merck Millipore, Darmstadt, Germany), and reversed-phase octadecyl (RP-C18) silica gel (Merck Millipore, Darmstadt, Germany). Various mobile phases were composed of reagent-grade solvents (Loba Chemie Pvt. Ltd., Mumbai, India). Then, 1- and 2-D NMR spectra were recorded on a Bruker UltraShield Plus 500 MHz spectrometer (Rheinstetten, Germany), with CD₃OD as the solvent. Chemical shifts (δ) were obtained in part per million (ppm) and the coupling constants (J) were measured in hertz (Hz). Electrospray ionization mass spectrometry (ESI-MS) was obtained using a Thermo Scientific UPLC RS Ultimate 3000-Q Exactive hybrid quadrupole-Orbitrap mass spectrometer (Waltham, MA, USA).

IR spectrum was acquired using a JASCO 320-A spectrometer (JASCO International Co., Ltd., Easton, MD, USA). Normal and reversed-phase silica gels (Merck, Darmstadt, Germany) were used for column chromatography (CC) and thin-layer chromatography (TLC). The compounds were visualized on TLC by spraying with 15% H₂SO₄/ethanol, followed by heating.
NMR spectroscopy was performed using deuterated solvents in an UltraShield Plus 500 (Bruker, Billerica, MA, USA) spectrometer operating at 500 MHz for ¹H and 125 MHz for ¹³C at the College of Pharmacy, Prince Sattam Bin Abdulaziz University. The two-dimensional NMR analyses (COSY, HSQC, and HMBC) were conducted using the standard Bruker pulse program. Chemical shift values are reported in δ (ppm) relative to an internal standard (TMS), and coupling constants (J) are reported in Hertz (Hz).
HRMS was performed using a Thermo Scientific UPLC RS Ultimate 3000 Q Exactive Hybrid Quadrupole-Orbitrap Mass Spectrometer (Mundelein, IL, USA) combined with high-performance quadrupole precursor selection with high resolution, accurate-mass (HR/AM) Orbitrap™ detection. The instrument was located at Prince Sattam Bin Abdulaziz University, College of Pharmacy. The detection was performed in negative and positive modes, and the experiment run time was 1 min using nitrogen as the supplementary gas with a scan range from 160–1500 m/z.