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1.
International Journal of Traditional Chinese Medicine ; (6): 854-860, 2018.
Artículo en Chino | WPRIM | ID: wpr-693683

RESUMEN

Objective To establish a HPLC-MS/MS method for comprehensive monitor and control of the raw material feeding (Gentiana scabra,Katsumade Galangal Seed and dried tangerine peel),and determination of Gentiopicroside,Alpinetin,Cardamonin and Hesperidin in Compound gentian tincture.Methods The separation was performed on an Inertsil ODS-3 (4.6 mm× 150 mm,5 μm) analytical column with the mobile phase consisting of acetonitrile-0.1% formic acid solution by gradient elution program,and the column temperature was 40 ℃.Active ingredients were separated by HPLC.The Electrospray Ionization Mass (ESI) source was applied and operated in the negative ion mode,and reactions ion monitoring mode (MRM) for quantitative analysis were selected.Results Through the analysis of the samples with mixed extract the same characteristic peak in MS was found to determine the proprietary Chinese medicine according to the prescription feeding process.The calibration curve of Gentiopicroside,Alpinetin,Cardamonin and Hesperidin were linear:103.26-619.56 μg (r=0.999 0),109.50-657.00 μg (r=0.999 5),105.50-633.00 μg (r=0.996 9),105.02-630.12 μg (r=0.999 5).The precision was Gentiopicroside 0.81%,Alpinetin 0.48%,Cardamonin 0.61% and Hesperidin 1.55% respectively.The average recovery rate were Gentiopicroside 95.08%,Alpinetin 93.28%,Cardamonin 94.78% and Hesperidin 95.04% respectively.Conclusions The method was proved to be simple,accurate,reliable,high sensitivity and can be used for determination and control of the raw material feeding (Gentiana scabra,Katsumade Galangal Seed and dried tangerine peel).

2.
Chinese Traditional and Herbal Drugs ; (24): 687-690, 2011.
Artículo en Chino | WPRIM | ID: wpr-855626

RESUMEN

Objective: The aim of the study was to establish a high speed counter-current chromatography (HSCCC) method for the isolation and purification of alpinetin and cardamomin from Alpinia katsumadai. Methods: Two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (5 : 5 : 7 : 3) was used. The flow rate of the mobile phase was 2.0 mL/min, the revolution speed was 800 r/min, the separation temperature was controlled at 25 °C, the reservation ratio of the stationary phase was 50%, and the detection wavelength was 300 nm. Results: Alpinetin (17.2 mg) and cardamomin (25.1 mg) could be obtained from 100 mg of the crude extract in one-step separation by the method. The purities of them were 98.1% and 99.2%, respectively, as determined by HPLC and their chemical structures were identified by 1H-NMR and 13C-NMR. Conclusion: The traditional method, column elution, could not eliminate irreversible adsorption, while the HSCCC method used for the isolation and purification of alpinetin and cardamomin from A. katsumadai has many advantages, such as facility, high efficiency, and high recovery as well.

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