6200 q tof ms system

Melting points were obtained on an X-4 micro melting point apparatus. Optical rotations were measured with a Horiba SEPA-300 polarimeter. IR spectra were obtained with a Tenor 27 spectrophotometer using KBr pellets. 1D and 2D spectra were run on a Bruker Avance III 600 MHz spectrometer with TMS as an internal standard. Chemical shifts (δ) were expressed in ppm with reference to the solvent signals. Mass spectra were recorded on an Agilent 6200 Q-TOF MS system. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, People’s Republic of China), RP-18 gel (20–45 µm, Fuji Silysia Chemical Ltd., Japan), and Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Sweden). Medium Pressure Liquid Chromatography (MPLC) was performed on a Büchi Sepacore System equipping with pump manager C-615, pump modules C-605 and fraction collector C-660 (Büchi Labortechnik AG, Flawil, Switzerland), and columns packed with RP-18 gel. Preparative High Performance Liquid Chromatography (prep-HPLC) was performed on an Agilent 1260 liquid chromatography system equipped with Zorbax SB-C18 columns (5 μm, 9.4 mm × 150 mm or 21.2 mm × 150 mm) and a DAD detector. Fractions were monitored by TLC (GF 254, Qingdao Haiyang Chemical Co., Ltd. Qingdao), and spots were visualized by heating silica gel plates sprayed with 10% H₂SO₄ in EtOH.

Optical rotations were recorded on a JASCO P-1020 digital polarimeter. IR spectra were obtained on Bruker Tensor-27 infrared spectrophotometer with KBr pellets. ESI-MS spectra were recorded on a Bruker HCT/Esquire spectrometer. HR-ESI-MS were obtained on an Agilent 6200 Q-TOF MS system. 1D and 2D NMR spectra were obtained on a Bruker Avance III 600 MHz spectrometer in C₅D₅N; chemical shifts are given in δ (ppm), and coupling constants are reported in Hz. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Puke Chemical Co. Ltd., China) and Rp-18 gel (40–63 μm, Merck, Darmstadt, Germany). GC analysis was performed on a HP5890 gas chromatograph equipped with an H₂ flame ionization detector. Semi-preparative HPLC was run on Agilent 1100 liquid chromatograph equipped with a Zorbax SB-C18 column (5 μm, 25 cm × 9.4 mm) and a diode array detector (DAD). TLC was performed on HSGF₂₅₄ (0.2 mm, Qingdao Puke Chemical Co. Ltd., China). Fractions were monitored by TLC and spots were visualized by heating silica gel plates sprayed with 10 % H₂SO₄ in EtOH.