ABSTRACT
OBJECTIVE：To establish a metho d for sim ultaneous determination of 8 flavonoid glycosides in Sedum bulbiferum . METHODS：HPLC method was adopted to determine the contents of kaempferol- 3-O-β-D-glucopyranoside-（1→2）-α-L-glucopy- ranoside-7-O-α-L-glucopyranoside（KGGR），kaempferol-3-O-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside（KGR），quercetin-3- O-α-L-rhamnose-7-O-α-L-rhamnoside（QRR），BulbiferumosideⅡ，kaempferol-3-O-（6-coumarinyl）-β-D-glucose-（1→2）-β-D-glu- cose-7-O-α-L-rhamnoside（KcGGR），kaempferol-3-O-（2-β-D-glucose）-α-L-rhamnose-7-O-α-L-rhamnoside（KGRR），kaempferol-3- O-α-L-rhamnoside-7-O-α-L-rhamnoside（KRR），kaempferol-3-O-（6″-acetyl-β-D-glucose）-7-O-α-L-rhamnoside（KaGR）in S. bulbi- ferum. The determination was performed on Waters CORTECS C 18 column with mobile consisted of acetonitrile - 0.1％ phosphoric acid water solution （gradient elution ）at the flow rate of 0.8 mL/min. The detection wavelength was set at 254 nm，and column temperature was 35 ℃. The sample size was 5 μL. RESULTS：The linear range of 8 constituents were 0.013-0.052，0.005-0.018， 0.008-0.031，0.010-0.042，0.009-0.038，0.008-0.030，0.009-0.037，0.032-0.130 μg，respectively（all r were not less than 0.999 0）. The limits of detection were 0.08，0.14，0.11，0.21，0.42，0.35，0.23，0.28 μg/mL，respectively. The limits of quantification were 0.25，0.47，0.38，0.69，1.40，1.17，0.77，0.93 μg/mL，respectively. RSDs of precision ，reproducibility and stability tests （24 h） were all lower than 3％（n＝6 or n＝7）. The average re coveries were 99.67％-104.20％（RSDs＝0.17％-1.59％，n＝6）. Average contents of above 8 constituents in 13 batches of samples were 0.893 8，0.312 6，0.490 8，0.964 9，0.751 2，0.502 2，0.606 2， 1.915 7 mg/g（n＝3）. CONCLUSIONS ： The method is simple， acourate and reproducible ， and can be used for simultaneous determination of 8 flavonoid glycosides in 才〔2016〕5677） S. bulbiferum .
ABSTRACT
OBJECTIVE:To establish the quality standard for Gaultheria yunnanensis. METHODS:TLC was adopted for quali-tative identification of samples. Moisture,total ash and acid-insoluble ash were determined. HPLC method was used to determine the content of methyl salicylate. The determination was performed on Eclipse XDB-C18 column with mobile phase consisted of meth-anol-water(62:38,V/V)at the flow rate of 1.0 mL/min. The detection wavelength was set at 307 nm,and column temperature was 30 ℃. The sample size was 10 μL. RESULTS:TLC spots of samples were clear and well separated. The moisture was 8.2%-10.8%,total ash was 0.9%-4.0% and acid-insoluble ash was 0.1%-0.9%. The linear range of methyl salicylate were 0.045-0.73μg(r=0.9999). RSDs of precision,stability and reproducibility tests were no more than 1.0%. The recoveries of meth-yl salicylate were 97.8%-104.3%(RSD=2.6%,n=9). CONCLUSIONS:The established standard can be used for quality control of G. yunnanensis.
ABSTRACT
OBJECTIVE:To establish HPLC fingerprints of Miao medicine Ardisia crenata.METHODS:HPLC method was adopted.The determination was performed on Diamonsil C18 column with mobile phase consiste of methanol-water (gradient elution) at the flow rate of 1.0 mL/min.The detection wavelength was 220 nm,and column temperature was maintained at 30 ℃.The sample size was 10 μL.Using 11-O-(3',4',5'-three-o-galloylhyperin)-bergeninum as reference,HPLC fingerprints of 16 batches of samples were determined.Common identification and similarity evaluation were performed by using TCM Chromatographic Fingerprint Similarity Evaluation Software (2012 edition).Cluster analysis of fmgerprrints was conducted.RESULTS:There were 6 common peaks in HPLC fingerprints of 16 batches of samples.The similarity among 8 batches was more than 0.9.The 16 batches of samples could be clustered into 4 categories.CONCLUSIONS:Established fingerprints can provide reference for identification and quality evaluation ofA.crenata.