Merck hibar si 60 column

The values of optical rotation of the metabolites were determined with a JASCO P-1020 polarimeter (JASCO Corporation, Tokyo, Japan). Infrared absorptions were recorded using a JASCO FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan). ¹H and ¹³C NMR spectra were obtained on a Varian 400MR FT-NMR (or Varian Unity INOVA500 FT-NMR) instrument (Varian Inc., Palo Alto, CA, USA) at 400 MHz (or 500 MHz) and 100 MHz (or 125 MHz), respectively, in CDCl₃ or C₆D₆. The data of LRESIMS and HRESIMS were measured using a Bruker APEX II (Bruker, Bremen, Germany) mass spectrometer. Silica gel (230–400 mesh) was used as adsorbent for column chromatography. TLC analyses were performed using precoated silica gel plates (Kieselgel 60 F-254, 0.2 mm) (Merck, Darmstadt, Germany). Further purification of impure fractions or compounds were performed by high-performance liquid chromatography on a Hitachi L-7100 HPLC instrument (Hitachi Ltd., Tokyo, Japan) with a Merck Hibar Si-60 column (250 mm × 21 mm, 7 μm; Merck, Darmstadt, Germany) and on a Hitachi L-2455 HPLC apparatus (Hitachi, Tokyo, Japan) with a Supelco C18 column (250 mm × 21.2 mm, 5 μm; Supelco, Bellefonte, PA, USA).

Values of the specific optical rotation of the isolates were measured with a JASCO P-1020 polarimeter (JASCO Corporation, Tokyo, Japan). Infrared spectra were recorded using a JASCO FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan). The CD spectrum was recorded on a Jasco J-815 circular dichroism (CD) spectropolarimeter (JASCO, Tokyo, Japan) in MeOH. ¹H- and ¹³C-NMR spectra were acquired on a Varian 400MR FT-NMR (or Varian Unity INOVA500 FT-NMR) instrument (Varian Inc., Palo Alto, CA, USA) at 400 MHz (or 500 MHz) and 100 MHz (or 125 MHz), respectively, in CDCl₃ or C₆D₆. LR-ESI-MS and HR-ESI-MS experiments were carried out using a Bruker APEX II (Bruker, Bremen, Germany) mass spectrometer. Silica gel (230–400 mesh) was used as the adsorbent for normal-phase column chromatography. Thin-layer chromatography (TLC) analyses were performed with precoated silica gel plates (Kieselgel 60 F-254, 0.2 mm, Merck, Darmstadt, Germany). Further purification of impure fractions or compounds was further achieved by high-performance liquid chromatography on a Hitachi L-7100 HPLC instrument (Hitachi Ltd., Tokyo, Japan) with a Merck Hibar Si-60 column (250 mm × 21 mm, 7 μm; Merck, Darmstadt, Germany) and on a Hitachi L-2455 HPLC apparatus (Hitachi, Tokyo, Japan) with a Supelco C18 column (250 mm × 21.2 mm, 5 μm; Supelco, Bellefonte, PA, USA).