Agilent 6529b q tof instrument

Optical rotations were measured using a JASCO P-1020 polarimeter (JASCO Corporation, Tokyo, Japan) in MeOH at 25 °C. UV spectra were recorded on a Shimadzu UV-1800 spectrophotometer (Shimadzu Corporation, Tokyo, Japan) in MeOH. ECD spectra were obtained by Chirascan circular dichroism spectrometers (Applied Photophysics Ltd., Leatherhead, UK). Both 1D and 2D NMR spectra were recorded on a Bruker AVIII-600 NMR spectrometer, using TMS as an internal standard. High-resolution electrospray ionization (HR-ESI-MS) was carried out with an Agilent 6529B Q-TOF instrument (Agilent Technologies, Santa Clara, CA, USA). Column chromatography was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China) and ODS (50 µm, YMC, Kyoto, Japan) on a Flash Chromatograph System (SepaBen machine, Santai Technologies, Changzhou, China). Preparative high-performance liquid chromatography (Pre-HPLC) was performed on a Shimadzu LC-20 system (Shimadzu, Tokyo, Japan) equipped with a Shim-pack RP-C18 column (20 × 250 mm i.d., 10 µm, Shimadzu, Tokyo, Japan) with a flow rate at 10 mL/min at 25 °C.

Optical rotations were determined using a JASCO P-1020 polarimeter (JASCO Corporation, Tokyo, Japan). The NMR spectra were recorded in CDCl₃ on a Bruker AVIII-500 spectrometer (Bruker, Bremen, Germany), using TMS as an internal standard. High-resolution electrospray ionization (HRESIMS) was recorded on an Agilent 6529B Q-TOF instrument (Agilent Technologies, Santa Clara, CA, USA). Column chromatography was performed using Silica gel (200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China), a Sephadex LH-20 (Merck, Darmstadt, Germany) and ODS (50 µm, YMC, Kyoto, Japan). TLC was performed using Silica gel GF₂₅₄ (Marine Chemical Industry Factory, Qingdao, China) and was detected by spraying with 5% H₂SO₄−EtOH.

Optical rotations were measured using a JASCO P-1020 polarimeter (JASCO Corporation, Tokyo, Japan) in MeOH at 25 °C. UV spectra were obtained with a Shimadzu UV-1800 spectrophotometer (Shimadzu Corporation, Tokyo, Japan). High-resolution electrospray ionization (HRESIMS) were recorded on an Agilent 6529B Q-TOF instrument (Agilent Technologies, Santa Clara, CA, USA). ECD spectra were carried out with Chirascan circular dichroism spectrometers (Applied Photophysics Ltd., Leatherhead, UK). Both 1D and 2D NMR spectra were measured with a Bruker AVⅢ-500 NMR spectrometer with tetramethylsilane (TMS) as an internal standard (Bruker, Karlsruhe, Germany). Preparative high-performance liquid chromatography (Pre-HPLC) was performed, utilizing a Shimadzu LC-20 system (Shimadzu, Tokyo, Japan), equipped with a Shim-pack RP-C₁₈ column (20 × 250 mm i.d., 10 μm, Shimadzu, Tokyo, Japan) with a flow rate at 10 mL/min at 25 °C, recorded by a binary channel UV detector at 210 nm and 254 nm. Column chromatography (CC) was performed with silica gel (200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China) and ODS (50 μm, YMC, Kyoto, Japan). Thin-layer chromatography (TLC) was performed, using precoated silica gel GF254 plates (Qingdao Marine Chemical Inc., Qingdao, China).