6529b q tof mass instrument

Optical rotations were measured on a JASCO P-1020 automatic digital polarimeter at room temperature. IR spectra were recorded on a Bruker Tensor 27 spectrometer using KBr pellets. UV spectra were recorded on a Shimadzu UV-2450 spectrophotometer (Shimadzu, Tokyo, Japan). High-resolution electrospray ionization mass spectrometry (HRESIMS) was obtained on an Agilent 6529B Q-TOF mass instrument using electrospray ionization. The 1D and 2D nuclear magnetic resonance (NMR) spectra were obtained on Bruker AVANCE III 500 MHz or Bruker AVIIIHD 600 MHz spectrometers in CDCl₃ with TMS as an internal standard. Analytical HPLC was conducted on an Agilent 1260 infinity system equipped with a DAD-UV detector. Preparative HPLC was carried out using a Shimadzu LC-6A system (Shimadzu, Tokyo, Japan) equipped with a Shim-pack RP-C₁₈ column (20 × 200 mm, i.d. 10 μm, Shimadzu, Tokyo, Japan) with a flow rate of 10.0 mL/min, detected by a binary channel UV detector. Silica gel (200–300 mesh, Qingdao Haiyang Chemical Co. Ltd., China), MCI (Mitsubishi, Japan), and RP-C₁₈ silica (40–63 μm, FuJi, Japan) were used for column chromatography.

The optical rotations were measured on a JASCO P-1020 polarimeter at room temperature. The melting points were measured using an X-4 digital display micromelting apparatus and are uncorrected. The IR spectra were recorded on a Bruker Tensor 27 spectrometer using KBr pellets. The 1D- and 2D-NMR spectra were measured on a Bruker AVIII-500 NMR instrument (¹H: 500 MHz, ¹³C: 125 MHz) using TMS as the internal standards. HRESIMS was performed on an Agilent 6529B Q-TOF mass instrument using electrospray ionization. All of the solvents used were of analytical grade (Jiangsu Hanbang Science and Technology. Co., Ltd.). Silica gel (200–300 mesh, Qingdao Haiyang Chemical Co., Ltd, China), Sephadex LH-20 (Pharmacia, Sweden), MCI (Mitsubishi, Japan) and RP-C18 silica (40–63 μm, Fuji, Japan) were used for the column chromatography. Preparative HPLC was conducted using an Agilent 1260 Series instrument with a Shim-Pak RP-C18 column (20 × 200 mm), at a flow rate of 10.0 mL/min, and detection by a binary channel UV detector. The fractions obtained from CC were monitored by TLC with precoated Silica gel GF₂₅₄ (Qingdao Haiyang Chemical Co., Ltd, China) plates.