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AIM To establish the UPLC fingerprints of Bushen Qiangshen Tablets (Epimedii Folium,Cuscutae Semen,Rosae Laevigatae Fructus,etc.).METHODS The analysis of 50％ ethanol extract of this drug was performed on a 40 ℃ thermostatic Agilent SB-C18 column (100 mm ×4.6 mm,2.7 μm),with the mobile phase comprising of acetonitrile-0.1％ phosphoric acid flowing at 0.5 mL/min in a gradient elution manner,and the detection wavelength was set at 215 nm.Then the fringerprints were evaluated by cluster analysis,principal components analysis and orthogonal partial least squares discriminant analysis.RESULTS There were twenty common peaks in the UPLC fingerprints of twelve batches of samples,nine of which (protocatechuic acid,salidroside,chlorogenic acid,hyperin,specnuezhenide,epimedin C,icariin,kaempferide and baohuoside Ⅰ) were identified,with the similarities of 0.843-0.970.Twelve batches of samples could be divided into three types,and four differential markers,including specnuezhenide and chlorogenic acid,were found out.CONCLUSION This simple and reliable method can be used for the quality control of Bushen Qiangshen Tablets.
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AIM To establish an HPLC method for the simultaneous content determination of narirutin,naringin,hesperidin,neohesperidin,honokiol and magnolol in Liuhe Dingzhong Pills (Aurantii Fructus,Citri reticulatae Pericarpium,Magnoliae officinalis Cortex,etc.).METHODS The analysis of 75％ methanol extract of this drug was performed on a 30 ℃ thermostatic Dikma Spursil C18 column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of acetonitrile-water flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelengths were set at 283 nm and 294 nm.RESULTS Six constituents showed good liner relationships within their own ranges (r≥0.999 3),whose average recoveries were 92.6％-103.7％ with the RSDs of 0.89％-2.87％.The contents of naringin and neohesperidin in three batches of samples showed obvious differences.CONCLUSION We should pay attention to the unstable quality of Liuhe Dingzhong Pills due to Aurantii Fructus.
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OBJECTIVE:To establish a method for the determination of Oleanolic acid and Ursolic acid isomers in Hedyotis corymbosa.METHODS: Capillary zone electrophoresis with high frequency conductivity detection was adopted.The separation of sample was performed on an uncoated fused silica capillary(55 cm?75 ?m ID) at an effective length of 50 cm.1.2 mmol?L-1 Triethylamine(TEA)-HCl(pH10.0) buffer containing 0.24 mmol?L-1 ?-cyclodextrin was selected for the running buffer solution.The voltage applied was 12.5 kV and the sample was injected by gravity for 10 s at a height of 20 cm.Brufen was used as internal standard.RESULTS: The linear ranges for Oleanolic acid and Ursolic acid were 3.9～39.0 ?g?mL-1(r=0.999 1) and 20.0～140.0 ?g?mL-1(r=0.999 0),respectively,and their average recovery rates were 96.5% and 96.0% respectively and RSD were 1.98% and 1.09%,respectively(n=6).CONCLUSION:It was proved that the method was simple,accurate,rapid and reproducible,and applicable for the quality control of Hedyotis corymbosa.
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Objective To determine the content of quercetin in Semen Hoveniae.Methods A RP-HPLC method was established.The chromatographic column was Synergi 4u Fusion-RP 80.The mobile phase was acetonitrile-0.5 %phosphoric acid(33 ∶67).The flow rate was 1.0 mL?min-1,the detection wavelength was at 360 nm,and the column temperature was 30 ℃.Results The average recovery of quercetin was 98.6 %,and RSD was 2.39 %(n=6).Conclusion The method is effective,simple and accurate,and can be used to determine the content of quercetin in Semen Hoveniae.
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Objective Using the contents of naphthaquinine and shikonin as the indices,the influences of ultrasonic extraction and soxhlet extraction on the active constituents in Arnebia euchroma(Royle)Johnst.were studied.Methods An orthogonal design was applied.Naphthaquinine content was determined by spectrophotometry and shikonin content by HPLC.The extraction rate of the two extracting methods was compared to optimize the process condition.Results By using the two extracting methods,particle size had an obvious effect on the extraction rate of naphthaquinine(the bigger particle,the higher extraction rate),but had no effect on the extraction rate of shikonin;the solvent of ethanol showed different effects on the extraction rate of active constituents by using the two extraction methods,the extraction rate being higher by ultrasonic extraction while lower by soxhlet extraction.Conclusion Ultrasonic extraction is efficient,and with energy and time saving in extracting active constituents of Arnebia euchroma(Royle)Johnst.,which is superior to soxhlet extraction.
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Objective To determine the content of trigonelline in Radix Mirabilis.Methods A RP -HPLC method was established.The chromatographic c olumn was Inertsil NH 2 Columns(250?4.6mm,5?m.).The mobile phase was acetonitrile -water(80∶20).The flow rate was 0.8mL?min -1 and the detection wavelength was at 265nm,and the column temperature was 30℃.Results The calibration curve was linear in t he range of 0.1872～0.9360?g .The aver-age recovery for trigonelline was 99.6%and RSD was 1.76%(n=6).Conclusion The method is simple and effec-tive and can be used to determine the c ontent of trigonelline in Radix Mirabilis.
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AIM: To determine the content of(+)-catechin and (-)-epicatechin and berberine hydrochloride in Wangying Capsule(Rhizoma Picrorhizae,Rhizoma Coptidis,Catechu,etc.). METHODS: A RP-HPLC method was established.The chromatographic column was Diamonsil-C_(18).The mobile phase was 0.04 mol/L citric acid-N,N-dimethylformamide-tetrahydrofuran(40∶8∶2) for determining(+)-catechin and(-)-epicatechin with the flow rate of 1.0 mL/min,and the detection wavelength of 280 nm.The mobile phase was acetonitrile-water(52∶48)(including 0.34% potassium dihydrogen phosphate and 0.17% sodium dodecyl sulfate) for determining berberine hydrochloride with the flow rate of 1.0 mL/min,and the detection wavelength of 265 nm. RESULTS: The average recoveries for(+)-catechin and(-)-epicatechin and berberine hydrochloride were 100.9% and 99.9% and 97.0%,precision of the method were 2.52% and 2.53% and 2.70%(RSD,n=6),respectively. CONCLUSION: The method can be used for quantitative determination of the preparation.
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OBJECTIVE:To establish a capillary zone electrophoresis with high frequency conductance method for the determination of ursolic acid in Radix et Rhizoma Clematidis.METHODS:The separation of sample was performed on an uncoated fused silica capillary(60 cm?75 ?m ID,effective length:56 cm) with 1.2 mmol?L-1 triethylamine-HCl(pH 10.60) and 0.24 mmol?L-1 ?-cyclodextrin as running buffer solution.The separation voltage was 12.5 kV and the gravity injection of sample was conducted for 10 s at a height of 20 cm.RESULTS:The calibration curve of ursolic acid was linear over the concentration range of 5.55～111.0 mg?mL-1(r=0.999 3) and the average recovery for ursolic acid was 96.0%(RSD=1.39%,n=6). CONCLUSION:The method was proved to be simple,accurate,rapid and reproducible,and suitable for the quantitative determination of ursolic acid in Radix et Rhizoma Clematidis.