Optical rotations were measured on a PE model 343 polarimeter (PerkinElmer, Waltham, MA, USA). CD spectra were recorded on a
JASCO-815 CD spectrometer (JASCO, Tokyo, Japan). IR spectra were recorded on a Nicolet 5700 FT-IR microscope instrument (Thermo Fisher Scientific, Waltham, MA, USA). NMR spectra were obtained on
INOVA-500 (Varian, Palo Alto, CA, USA) and Bruker AV600-III (Bruker, Billerica, MA, USA) spectrometers, in C
5D
5N with solvent peaks used as references. ESIMS were measured on an
Agilent 1100 Series LC/MSD Trap mass spectrometer (Agilent, Santa Clara, CA, USA). HR-ESIMS data were measured using an
Agilent 6520 Accurate-Mass Q-TOF LC/MS spectrometer (Agilent). Preparative HPLC was performed on a Shimadazu LC-6AD instrument with SPD-20A and RID-10A detectors (Shimadazu, Kyoto, Japan) using an
YMC Pack ODS-A column (250 mm × 20 mm, 5 μm, YMC, Kyoto, Japan). Macroporous resin (D101 type, the Chemical Plant of NanKai University, Tianjin, China),
Si gel (160–200 and 200–300 mesh, Qingdao Marine Chemical Factory, China) was used for column chromatography (CC). TLC was carried out with glass precoated
Si gel GF
254 plates (Qingdao Marine Chemical Factory). Spots were visualized under UV light or by spraying with 10% H
2SO
4 in EtOH/H
2O (95:5,
v/
v) followed by heating.
Li Y., Zhu Y., Zhang Z., Li L., Liu Y., Qu J., Ma S, & Yu S. (2019). Antinociceptive grayanane-derived diterpenoids from flowers of Rhododendron molle. Acta Pharmaceutica Sinica. B, 10(6), 1073-1082.