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OBJECTIVE： To provide reference for the establishment of quality standard of Shenhuang liniment. METHODS： Qualitative identification of Sophora flavescens， Phellodendron chinense， Rhei Radix Et Rhizoma and Scutellaria baicalensis in Shenhuang liniment were carried out by TLC according to the method of 2015 edition of Chinese Pharmacopeia （part Ⅳ）. HPLC method was used to determine the contents of matrine and oxymatrine in Shenhuang liniment [Phenomenex Luna NH2 column， mobile phase consisting of acetonitrile-absolute ethanol-3％ phosphoric acid aqueous solution （80 ∶ 10 ∶ 10，V/V/V）， column temperature of 45 ℃， flow rate of 1.0 mL/min， detection wavelength of 220 nm， sample size of 5 μL]. RESULTS： Results of TLC showed that the corresponding spots of the same color were found in the corresponding positions of the chromatograms for test samples and reference substance/substance control； and the spots were clear， retardation factor was moderate， the separation degree was high， and the negative control had no interference. Results of HPLC showed that the linear range of matrine and oxymatrine were 203.60-1 221.60 ng（r＝0.999 4）and 210.08-840.30 ng（r＝0.999 7）， respectively. RSDs of precision， stability and reproducibility tests were all lower than 3.0％ （n＝6）. Average recovery rates were 96.03％ and 100.93％， and RSDs were 2.55％ and 2.69％（n＝9）. CONCLUSIONS： Established method is specific， accurate and reproducible， and can be used for quality control of Shenhuang liniment.
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OBJECTIVE:To establish UPLC fingerprint of Gehua formula granules. METHODS:UPLC method were adopted. The determination was performed on Zorbax Eclipse XDB-C18 column with mobile phase consisted of acetonitrile-water at the flow rate of 0.5 mL/min. The detection wavelength was set at 264 nm,column temperature was 25 ℃,and the sample size was 1 μL. Using tectorigenin as reference substance,UPLC chromatograms of 10 batches of Gehua formula granules were determined. The common peak identification and similarity evaluation were conducted by TCM Chromatogram Fingerprint Similarity Evaluation Sys-tem(2004 A edition). RESULTS:14 common peaks were identified in UPLC chromatograms of 10 batches of Gehua formula gran-ules and similarities were all higher than 0.90. UPLC chromatograms of 10 batches of samples were in good agreement with control fingerprint. CONCLUSIONS:Established UPLC fingerprint can provide reference for identification and quality evaluation of Gehua formula granules.
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AIM To establish the HPLC fingerprints of Cajanus cajan (L.) Millsp.leaves and to determine the contents of orientoside and luteolin.METHODS The analysis of 65％ methanol extract from C.cajan leaves was performed on a 25 ℃ thermostatic Agilent Zorbax SB-C18 column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of methanol-1％ acetic acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 260 nm.RESULTS There were twenty-one common peaks in ten batches of samples (S1-S10),whose similarities were more than 0.950,except for that of S3 (0.516).Orientoside and luteolin showed good linear relationships within the ranges of 0.089 5-3.960 μg and 0.015 5-0.408 μg,whose average recoveries were 99.43％ (RSD =1.32％) and 98.50％ (RSD =0.82％),respectively.The contents of two constituents in the samples from three growing areas (Guangdong,Yunnan and Hainan) showed obvious differences.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of C.cajan leaves.
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Objective:To establish a method for the separation and determination of ketoprofen enantiomer .Methods:A pre-col-umn derivation RP-HPLC method was used with L-alanine-β-naphthylamine ( L-Ala-β-NA) as the derivation reagent .The RP-HPLC conditions were as follows: a Hypersil ODS-2 column (250 mm ×4.6 mm,5 μm) was applied, the mobile phase was acetonitrile-0.025 mol· L-1 phosphate buffer solution (40∶60, v/v) and the flow rate was 1.0 ml· min-1 , the detection wavelength was set at 245 nm and the column temperature was 25℃.The injection volume was 10μl.Results:Base line separation was achieved for the sep-aration of enantiomer from ketoprofen , and the retention time for S-(+) -ketoprofen and the R-(-) -ketoprofen was 24.2 min and 26.0 min, respectively.Dexketoprofen within the range of 0.025-0.125 mg had a good linear relationship (r=0.998 1) and the aver-age recovery was 90.93%(RSD =4.10%, n=9 ).Conclusion:The method is simple, accurate and reliable, which can be applied in the separation and determination of ketoprofen .
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Objective:To develop a UPLC method for determining four glycosides in microctis folium.Methods:The UPLC deter-mination was performed on an Agilent SB -C18 (3.0 mm ×50 mm, 1.8 μm) colume with 0.05% acetonitrile -phosphate solution as the mobile phase.The detection wavelength was set at 320 nm.The flow rate was 0.3 ml· min-1.The column temperature was 25℃.Results:Narcissoside, isovitexin, kaempferol-3-rutinoside and isorhamnetin-3-O-glucoside all showed good linearity with the re-covery of 98.89%,99.03%, 97.00%and 97.41%, and RSD of 0.41%, 0.84%,0.44%and 0.80%, respectively (n=9).Con-clusion:The method is convenient with good stability , repeatability and sample recovery rate , which provides basis for the quality eval-uation and control of microctis folium.