Optimization of the Purification Technology of Total Flavones in Ampelopsis grossedentala with Macropo-rous Resins by Central Composite Design-Response Surface Methodology / 中国药房

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.

Studies on HPLC fingerprint of Herba Sedum aizoon L / 中华中医药杂志

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.

Determination and Analysis of Kaempferol in Sedum aizoon L.by HPLC-MS/MS / 中华中医药杂志

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.

Study on the GC fingerprints of volatile oil in ultramicro-powder of Houttuynia cordata / 中华中医药杂志

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.