ABSTRACT
To establish HPLC-MS/MS method for simultaneous determination of daphnetin, daphnoretin, and daphneticin in rat plasma after oral and intravenous administration of Daphne giraldii extract, and then use them in the calculation of pharmacokinetic parameters. Six sprague-dawley rats received intragastric administration of D. giraldii extract (daphnetin, daphnoretin and daphneticin were 88.40, 3.24 and 4.28 mg•kg⁻¹, respectively). Their drug plasma concentration was determined by LC-MS/MS with schisandrin as an internal standard to draw plasma concentration-time curve. The pharmacokinetic parameters were calculated by Kinetica 4.4. The results showed that the linear range was 5-1 000 μg•L⁻¹ for daphnetin, daphnoretin and daphneticin, and the method ological test showed conformance to the requirements.The intraday and inter-day variable coefficients (RSD) were both less than 15.0%, indicating that both of legitimate precise and accuracy were consistent with the analysis requirements of biological samples. For daphnetin, the pharmacokinetic parameters Tmax, Cmax, AUC0-t, T1/2 and MRT were 4 h, 858.96 μg•L⁻¹, 10 566.4 μg•L⁻¹•h, 5.19 h and 9.43 h, respectively. For daphnoretin, the pharmacokinetic parameters Tmax, Cmax, AUC0-t, T1/2 and MRT were 2.92 h, 178.00 μg•L⁻¹, 905.89 μg•L⁻¹•h, 3.50 h and 6.95 h, respectively. For daphneticin, the pharmacokinetic parameters Tmax, Cmax, AUC0-t, T1/2 and MRT were 2 h, 36.67 μg•L⁻¹, 355.11 μg•L⁻¹•h, 4.95 h and 8.27 h, respectively. The LC-MS/MS analysis method established in this study was proved to be so accurate and sensitive that it can be applied to the pharmacokinetic study of daphnetin, daphnoretin and daphneticin.
ABSTRACT
Object To isolate and identify the biflavonoids from the stem bark of Daphne giraldii Nitsche. Methods The flavonoids were isolated and purified by column chromatography on silica gel and Sephadex LH-20. Their structures were determined by spectroscopic methods, including IR, 1HNMR, 13 CNMR, HMBC and FAB-MS.Results Four biflavonoids daphnodorins A-D 1 (Ⅰ-Ⅳ) were isolated from the stem bark of D. giraldii. Conclusion The above four biflavonoids were isolated from the title plant only.
ABSTRACT
Objective To study the chemical constituents from the stem bark of Daphne giraldii. MethodsThe chemical constituents in the alcoholic extract from the stem bark of D. giraldii were isola-ted and purified using liquid/liquid extraction and silica gel column chromatography. The structures of the isolated compounds were determined on the basis of NMR, and mass spectra. ResultsSeven compounds were isolated from the alcohol extract. Their structures were identified as E-octadecyl caffeinate (Ⅰ), (+)-nortrachelogenin (Ⅱ), daphnoretin (Ⅲ), daphneticin (Ⅳ), 7, 8-dihydroxy coumarin (Ⅴ), 7-hydroxy coumarin (Ⅵ), and luteolin (Ⅶ) on the basis of 1H-NMR, 13C-NMR, and MS. ConclusionCompound Ⅰ is a new one. Compounds Ⅱ, Ⅳ, and Ⅶ are isolated from the title plant for the first time.