The 1H and 13C NMR spectra of the compounds were recorded on a Bruker Avance 300 NMR spectrometer operating at 7.05 Tesla magnetic field, controlled by TopSpin 1.3 software package, equipped with 5 mm 1H/13C dual inverse Z-grad probehead, and in DMSO‑d6 solution at 30 °C. The chemical shifts are referred to tetramethylsilane (δTMS = 0 ppm). The chemical structures of the compounds were proven based on two dimensional zqs-TOCSY [20 ], zqs-easy-ROESY [[20] , [21] (link), [22] (link)], multiplicity-edited HSQC as well as HMBC spectra. The LC-MS analyses were performed with Waters liquid chromatograph - mass spectrometer (mass detector, Waters SQD; UV detector, Waters 996 DAD; separation module, Waters Alliance 2795; column, Waters XBridge C18 50 × 4.6 mm 3.5 μm; and the gradient used with solvent-1, water (Mili-Q) containing 0.1% formic acid (Riedel- DeHaen, extra-pure), and solvent-2, acetonitrile (Riedel- DeHaen). The flow-rate was 2 ml/min with 5 μg sample. The MS parameters were used as: Ionisation, ES+/ES-; source block temperature, 110 °C; desolvation temperature, 250 °C; desolvation gas, 500 L/h; cone gas, 80L/h; capillary voltage, 3000 V; cone voltage, 30 V; extractor voltage, 6 V; Rf lens Voltage, 0.1 V; Scan: 80–1000 m/z in 1 s; and Inter-scan delay, 0.1 s.
Waters sqd
Manufactured by Waters Corporation
Sourced in United States
The Waters SQD is a single quadrupole mass spectrometer designed for a range of analytical applications. It provides reliable, accurate, and sensitive detection of small molecules. The SQD offers robust performance and easy-to-use software for efficient operation.
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Lab products found in correlation
2 protocols using waters sqd
1
Structural Elucidation of Compounds by NMR and LC-MS
2
Preparative HSCCC Automated Separation
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Preparative HSCCC was realized on the model OptiChrome™- a double-action column semi-preparation HSCCC (Counter-Current Technology Co., Ltd., Jiangsu, China). The instrument was a fully automated system consisting of a 2 polytetrafluoroethylene (PTFE) preparative coils (i.d of tube, 1.59 mm; revolution radius, 80 cm; range of β 0.50–0.80; total volume, 360 mL) and a 20 mL sample loop. Separating effect could be predicted by a FastChrome-30 analytical HSCCC (Counter-Current Technology Co., Ltd., Jiangsu, China) with a PTFE preparative coils (total volume, 25 mL; range of β, 0.56–0.91), a 1 mL sample loop. The HSCCC system was equipped with a model ultraviolet (UV)-3000 detector (Beijing Chuang Xin Tong Heng Science and Technology Co., Ltd), a model CXTH3000 workstation. The analytical HPLC equipment was measured on an Agilent 1260 system (Agilent Technologies Inc., USA). NMR spectra were obtained on a Bruker500 MHz DD2 NMR spectrometer (Bruker, Swiss); and the electrospray ionization (ESI)-MS was operated on Waters SQD (Waters, USA).
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