Amazon sl ion trap mass spectrometry

The HPLC system was performed using a Thermo Scientific™ Acclaim™ C18 column (2.1 × 100 mm, 2.2 μm, 0.2 ml min⁻¹) with gradient elution. UV spectra were recorded on a DAD detector with wavelength ranging from 190 to 400 nm. The MS was measured on a Bruker amazon SL Ion Trap mass spectrometry (Bruker Corporation) using the standard ESI source. Mass spectra were acquired in centroid mode ranging from 100 to 1500 m/z with positive‐mode electrospray ionization and auto MS² fragmentation. HPLC parameters were as follows: solvent A, H₂O with 0.2% (v/v) TFA; solvent B, 0.1% (v/v) TFA in acetonitrile (ACN); gradient at a constant flow rate of 0.2 ml min⁻¹, 0–5 min, 5% (v/v) B; 5–45 min, 5%–95% (v/v) B; 45–50 min, 95% (v/v) B; or 0–5 min, 5% (v/v) B; 5–25 min, 5%–95% (v/v) B; 25–30 min, 95% (v/v) B detection by UV spectroscopy at 190–400 nm.

1260 HPLC (Agilent Technologies Co., Ltd, MA); AmaZon SL ion trap mass spectrometry (Bruker Daltonik GmbH Co., Ltd, Bremen); 5C18-PAQ (4.6 (ID) × 250 (mm)) chromatography column (Cosmosil, Japan); incubator (QYC-2102C, CIMO Instrument Manufacturing Co., Ltd. Shanghai, China); microplate reader (DNM-9606, Perlong Medical Equipment Co., Ltd. Beijing, China); D8 Advance XRD characterisation (Bruker, Germany); JSM-7610F scanning electron microscope (JEOL Ltd. Japan); MPMS3 Magnetic properties (Quantum Design); VERTEX 70 infrared spectra (Bruker, Germany); JEM-2100 transmission electron microscope (JEOL Ltd. Japan).

Optical rotations were acquired by an Anton Paar MCP 200 polarimeter at 20°C. UV data were recorded using a UV‐2550 spectrophotometer (Shimadzu, Japan). IR spectra were measured on a Nicolet iN 10 Micro FTIR spectrometer. ¹H and ¹³C NMR, DEPT, and 2D NMR spectra were recorded on a Bruker AvanceIII 600 MHz with TCI cryoprobe using TMS as an internal standard. HRESIMS spectra were measured on a Bruker Impact HD microTOF Q III mass spectrometer (BrukerDaltonics, Bremen, Germany) using the standard ESI source. HPLC‐MS was operated using a Thermo Scientific Dionex Ultimate 3000 system coupled with the Bruker amazon SL Ion Trap mass spectrometry (Bruker Corporation, Bremen, Germany), controlled by Hystar v3.2 and Chromeleon Xpress software. A Thermo Scientific™ Acclaim™ C18 column (2.1 × 100 mm, 2.2 μm) was used. The mobile phase consisted of H₂O containing 0.1% (v/v) FA and ACN. Semipreparative HPLC was performed using an ODS column [Bruker ZORBAX SB‐C18, 250 × 10 mm, 5 μm, 2 ml min⁻¹]. TLC and column chromatography (CC) were performed on plates precoated with silica gel GF254 (10–40 μm) and over silica gel (200–300 mesh, Qingdao Marine Chemical Factory, Qingdao, Shandong, China) and Sephadex LH‐20 (GE Healthcare, Pittsburgh, PA, USA) respectively.