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OBJECTIVE：To optimi ze and improve the quality standard for Keqing capsules. METHODS ：According to general rule 0502 method stated in 2015 edition of Chinese Pharmacopeia （part Ⅳ），TLC method was used to identify Reineckia carnea and Morus alba in Keqing capsules [the developing solvents were dichloromethane-ethyl acetate-formic acid （10 ∶ 4 ∶ 0.2，V/V/V） and ethyl acetate-carbinol-ammonia （12 ∶ 2 ∶ 1，V/V/V），respectively]. The contents of morphine and codeine phosphate in Keqing capsules were determined by HPLC. The determination was performed on XBridge C 18 column with mobile phase consisted of acetonitrile-0.01 mol/L potassium dihydrogen phosphate aqueous solution （pH value adjusted to 2.7 with 5％ phosphoric acid solution）（5 ∶ 95，V/V）at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm，and the column temperature was 35 ℃. The sample size was 10 µL. RESULTS ：In TLC of R. carnea and M. alba in samples ，same color spots were shown in the correspon ding positions of reference substance chromatogram without interference from negative control. The linear range of morphine and codeine phosphate were batches of Keqing capsules were 0.97-1.37，0.16-0.37 mg/g，respectively. CONCLUSIONS ：TLC identification method for R. carnea and M. alba ，as well as HPLC content determination method for morphine and codeine phosphate in Keqing capsules are established；the method is simple ，accurate and reliable with strong specificity ，which improves the quality standard of Keqing capsules.
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AIM To establish the quality standard for Cyclocarya paliurus (Batal.) ljinsk..METHODS The contents of water,ash and extract in twelve batches of samples were determined.TLC and HPLC were adopted in the qualitative identification and quantitative determination of quercetin and kaempferol,respectively,and phenol-sulfuric acid method was used for the polysaccharide content assessment.RESULTS The average contents of water,total ash,acid-insoluble ash,water-soluble extract and alcohol-soluble extract were 11.05％,5.81％,1.70％,11.25％ and 10.16％,respectively.The clear TLC spots demonstrated their strong specificity.Quercetin and kaempferol showed good linear relationships within the ranges of 0.004 953-0.022 29 mg/mL and 0.005 748-0.028 74 mg/mL (r =0.999 9),whose average recoveries were 97.1％ (RSD =2.59％) and 97.9％ (RSD =2.86％),respectively.Polysaccharide showed a good linear relationship within the range of 0.021 22-0.095 58 mg/mL,whose average recovery was 97.2％ (RSD =2.42％).The contents of three constituents in various batches of samples showed obvious differences.CONCLUSION In C.paliurus,the contents of water,total ash,acid-insoluble ash,water-soluble extract and ethanol-soluble extract should not be more than 13.0％,7.0％,2.0％,13.5％ and 12.0％,while those of quercetin,kaempferol and polysaccharide (calculated by dry product) should not be less than 0.040％,0.070％ and 0.60％,respectively.
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Objective To establish a methodological study pattern of quantitative analysis of multi-components by single marker ( QAMS) , and examine its feasibility and technical applicability in the quality control of compound preparation of traditional Chinese medicine-Jinhoujian spray. Methods Gas chromatographic method ( GC) was used and naphthalene served as the internal standard. Menthol was used as the reference substance. The relative correlation factors ( RCF) of 1,8-Cineole, camphor and borneol to menthol were calculated and established to carry out QAMS.The accuracy of this method was confirmed by comparison of internal standard method. Results The reproducibility of relative correction factor was perfect. The two methods did not show significant difference in 10 bathes of samples. Conclusion The QAMS method is feasible, credible, and can be used to determine active ingredients in Jinhoujian spray.
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OBJECTIVE:To establish an HPLC method for the determination of Diosgenin in Bixiefenqing pills.METHODS:The samples were separated on DiamonsilTM C18(200 mm?4.6 mm,5 ?m)column.The mobile phase consists of acetonitrile-water(92∶8) at a flow rate of 1.0 mL?min-1.The detecting wavelength was set at 203 nm and the column temperature was set at 35 ℃.RESULTS:The linear range of Diosgenin was 0.115 36～1.038 24 ?g(r=0.999 9).The average recovery was 98.71%(RSD=1.92%,n=9).CONCLUSION:The method was proved to be simple and accurate,and suitable for the identification and quality control of Bixiefenqing pills.
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Objective: To establish the determination method of gallic acid in Ninbitai Capsules.Methods: HPLC with Shimadzu Shim-pack VP-ODS(250mm?4.6mm,5??m) column was used. Methanol-water-dimethylformamide-acetic acid glacial (1∶81∶15∶3) was used as mobile phase. The flow rate was 0.5mL/min. The detection wavelength was at 272nm.Results: The linearity of this method was well. The recovery of the added sample was 98.16%. RSD was 1.18%.Conclusion: This method is convient with a good separating degree and can be used for the quality control of Ninbitai Capsules.