1290 uplc 6540 q tof mass spectrometer

Optical rotations were measured with a Jasco P-1020 polarimeter. UV spectra were obtained using a Shimadzu UV-2401 PC spectrophotometer. IR spectra were obtained with a Bruker FT-IR Tensor 27 spectrometer using KBr pellets. 1D and 2D NMR spectra in CDCl₃ were recorded on an AVANCE III 500 and 600 MHz spectrometers. HREIMS spectra were recorded on an Agilent 1290 UPLC/6540 Q-TOF mass spectrometer. ECD spectra were recorded on an Applied Photophysics spectropolarimeter. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, China) and RP-18 gel (20–45 µm, Fuji Silysia Chemical Ltd., Tokyo, Japan). Semi-preparative HPLC were performed on an Agilent 1260 instrument with a ZORBAX SB-C18 column (9.4 × 250 mm, 5 μm) or an Agilent 1100 instrument with a CHIRALPAK IC column (10 × 250 mm, 5 μm). TLC (GF₂₅₄, Qingdao Haiyang Chemical Co., Ltd. Qingdao, China or RP-18 F₂₅₄, Merck, Darmstadt, Germany) was used to monitor the fractions. Spots were detected by a UV light (254 nm) and followed by dipping in 10% H₂SO₄ in EtOH and heating at 110 °C.

Optical rotations were measured on a Jasco P-1020 polarimeter. UV spectra were recorded on a Shimadzu UV2401 PC spectrophotometer. IR spectra were determined on Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr discs. ECD spectra were recorded on an Applied Photophysics spectropolarimeter. 1D and 2D NMR spectra were recorded on Bruker AV 600 or 800 MHz spectrometers using TMS as an internal standard. Chemical shifts (δ) were expressed in ppm with reference to the solvent signals, and coupling constant (J) values were reported in Hz. HRESIMS data were measured using an Agilent 1290 UPLC/6540 Q-TOF mass spectrometer. Sephadex LH-20 (GE Healthcare, Uppsala, Sweden), Si gel (200–300 mesh, Qingdao Marine Chemical Co., Qingdao, People’s Republic of China), and RP-18 (50 μm, Merck, Germany) were used for column chromatography (CC). Semi-preparative HPLC was performed on an Agilent 1260 instrument with a ZORBAX SB-C18 column (9.4 × 250 mm, 5 μm). Fractions were monitored by Si gel GF₂₅₄ (Qingdao Marine Chemical Co., China) or RP-18 F₂₅₄ (Merck, Darmstadt, Germany) plates. Spots were visualized under UV light and by spraying with 10% H₂SO₄ in EtOH followed by heating.

Optical rotations were measured with a Jasco P-1020 automatic polarimeter. CD spectra were obtained on the Applied Photophysics circular dichroism spectrometer (Applied Photophysics, Leatherhead, Surrey, UK). High-resolution MS data were measured on an Agilent 1290 UPLC/6540 Q-TOF mass spectrometer in positive mode. IR spectra were determined on a NICOLET iS107 Mid-infrared spectrometer. NMR spectra were measured on Bruker AVANCE III 500 MHz and AV 600 MHz NMR spectrometers with TMS as the internal standard. An Agilent 1260 series instrument equipped with a SunFire-C₁₈ column (5 μm, 10 mm × 250 mm) and XSelect HSS T3(5 μm, 10 mm × 150 mm) were used for high-performance liquid chromatography (HPLC). Silica gel (100 − 200, 200 − 300, 300 − 400) mesh (Qingdao Marine Chemical, Inc), NH MB 100–40/75 Silica gel (FUJI SILYSIA CHEMICAL LTD), Lichroprep RP-18 (40 − 63 μm, Fuji), and Sephadex LH-20 (20 − 150 μm, Pharmacia) was used for CC.