Study on preparation of reference products of phorbol diesters
Objective To study the preparation method and quality standard of the reference product of phorbol diesters(TPA),and to provide the basis for the quality control of raw materials and related preparations of phorbol diesters.Methods The methanol-water extract of croton oil was separated and purified by silica gel column preparation chromatography and reversed-phase preparation chromatography.The purity and content of the reference product of phorbol diesters were checked by high performance liquid chromatography(HPLC)and gas chromatography,and the chromatogram and structure were analyzed by ultraviolet spectroscopy(UV),infrared spectroscopy(IR),mass spectrometry(MS),Hydrogenium-1 nuclear magnetic resonance spectroscopy(1H-NMR),Carbon-13 nuclear magnetic resonance(13C-NMR)and other methods.The molecular formula was confirmed as C36H56O8.Results The maximum UV absorption wavelength of the purified reference product was 232 nm,the MS result was high-resolution electrospray ionization mass spectrometry(HESI-MS)m/z 615.4120(M-H),and the purity was>99.5%by HPLC.Conclusion The preparation method is scientific and effective,and the purity of the prepared reference product meets the relevant requirements of traditional Chinese medicine chemical reference products,and can be used as chemical reference products for the quality control of phorbol diesters raw materials and related preparations.
Croton tigliumPhorbol diestersChemical referenceReversed-phase preparative chromatographyStructural identificationContent determinationPurityQuality control
万方数据
维普
