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OBJECTIVE:To optimize the purification technology of total flavones from Ampelopsis grossedentala with macro-porous resins. METHODS:4 kinds of macroporous resins for the purification of total flavones from A. grossedentala were screened by using drug-loading amount,desorption rate,recovery and purification rate as indicators. Single factor test and central composite design-response surface methodology were used to optimized eluant mass fraction,adsorption time,flow rate of eluant,eluant pH and other factors of purification technology,and validation test was also conducted. RESULTS:D-101 macroporous resin was the best. The optimal condition was as follows as the concentration of sample solution 2 mg(by extract weight)/ml,the volume of sam-ple solution 1.1 BV,ethanol 86.0%,adsorption time 36.7 min,flow rate of eluant 3.81 BV/h,pH 7. In validation test,mass frac-tion of total flavones increased from 66.83% to 85.00% in validation test(RSD=0.15%,n=3),and were close to predicted val-ue(85.08%). CONCLUSIONS:Central composite design-response surface methodology is feasible and stable for the optimization of purification technology of total flavones from A. grossedentala with macroporous resins.
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Objective:The fingerprint chromatograms were established for quality evaluation of Sedum aizoon L.collected from different habitats by HPLC.Methods:The analysis was performed on a Diamonsil C18 column(4.6mm? 250mm,5?m)with acetonitrile-water(acidified to 0.5%with phosphoric acid)as mobile phase in a gradient mode at a flow rate of 1.0 mL/min,and at a column temperature of 25℃.The detection of wavelength was at 254 nm.Results:2lpeaks were selected as the common fingerprint peaks.The relative standard deviations for relative retention values and relative peak areas were less than 3%in the precision and repeated test.The similarity of l0 batches of samples were no less than 0.9.Conclusion:The method was reliable and can be helpful on the quality control of Sedum aizoon L.
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Objective:To establish a GC fingerprint analysis method for identification of volatile oil in ultramicro-powder of Houttuynia cordata from different habitats, then to control the quality sensitively.Methods: GC was used to analyze the volatile constituents of ultramicro-powder of Houttuynia cordata from 12 different habitats;SPDTM-1CapillaryColumn(30m?0.32mm?0.25?m),temperature programming and FID detector were applied.Results: The mutual mode of GC fingerprints was set up and the similar degrees to the volatile oil from of different habitats were compared.Conclusion:The GC fingerprints of volatile oil in ultramicro-powder can be used to identify the Houttuynia cordata from different habitats and evaluate its quality.
RESUMO
Objective: To discover and determine the content of kaempferol in Sedum aizoon L.for the first time.Methods: Waters HPLC-MS/MS,XTerra-MS C18 (5?m,2.1?150mm) and the mobile phase consisted of acetonitrile-water-formic(40∶60∶1) were applied to find kaempferol in Sedum aizoon L.;Daojin HPLC and the SHIM-PACK VP C18(250nm?4.6nm,10?m) column were used.The mobile phase consisted of methanol-0.4% phosphoric acid solutions(59:41) with the flow rate at 1.0ml/min and the UV detector wave-length were set at 370nm.Results: Compared with standard sample,the thing that kaempferol exists in Sedum aizoon L.was confirmed.The calibration curve was in good linearity over the range of 2.0-8.0?g,and regression equation was Y=40343X-11107(r=0.9998).The average recovery rate was 102.53%,with RSD =0.92%(n=6).Conclusion: The method is simple,accurate and reproducible so it can be used to determine and analyze the content of kaempferol in Sedum aizoon L.