RESUMO
OBJECTIVE： To establish the qualitative and quantitative control method of Tibetan medicine Thlaspi semen. METHODS： TLC and HPLC method were used to identify and determine flavonoids isovitexin， swertisin and glucosinolates sinigrin from 15 batches of T. semen. The stationary phases identified by TLC of flavonoids and glucosinolates were polyamide film and high performance silica gel GF254. The developing agents were trichloromethane-methanol-glacial acetic acid （11 ∶ 1 ∶ 1，V/V/V） and ethyl acetate-methanol- triethylamine （4 ∶ 5 ∶ 0.5，V/V/V）. In chromatogram condition of content determination of isovitexin and swertisin， the separation was performed on CAPCELL PAK MGⅡ C18 column with mobile phase composed of acetonitrile-0.4％ glacial acetic acid solution （gradient elution） at the flow rate of 1.0 mL/min. The detection wavelength was set at 336 nm. In chromatogram condition of content determination of sinigrin， the separation was performed on CAPCELL PAK MGⅡ C18 column with mobile phase composed of acetonitrile-0.02 mol/L tetrabutylammonium hydrogen sulfate （15 ∶ 85，V/V，pH 6） at the flow rate of 1.0 mL/min. The detection wavelength was set at 227 nm. RESULTS： In TLC identification chromatogram， spots corresponding to isovitexin， swertisin and sinigrin control were detected in test samples. The linear ranges of isovitexin， swertisin and sinigrin were 1.26-79.00， 1.21-75.38， 12.80-640.00 μg/mL， respectively （all r≥0.999 5）. The limits of detection （LODs） were 0.09， 0.12， 0.15 μg/mL， and limits of quantitation （LOQs） were 0.39， 0.43， 0.54 μg/mL， respectively. RSDs of precision， stability （24 h） and reproducibility tests were all lower than 2.0％（n＝6）. The recoveries were 99.1％， 97.0％ and 98.1％， and RSDs were 1.9％， 1.8％， 1.8％（n＝6），respectively. The contents of isovitexin， swertisin and sinigrin in 15 batches of T. semen were 0.013-0.090， 0.020-0.130 and 18.92-40.75 mg/g， respectively. CONCLUSIONS： Established quality control method is simple， reproducible and stable， and can be used for the quality control of Tibetan medicine T. semen.
RESUMO
Objective: To establish the quality standard for Jiuwei Zhaxun pills. Methods: Fructus Chebulae, Flos Carthami and Herba Dracocephali Heterophylli were identified by TLC. HPLC was used to determine the content of gallic acid in Jiuwei Zhaxun pills. Results: TLC showed clear sports without any interference from the negative control. Gallic acid showed a good linear relationship (r=0. 999 7) within the range of 0. 028 6-0. 572 0 μg. The average recovery was 97. 74% with the RSD of 0. 95% (n=6). Conclusion:The methods are with strong specificity, high sensitivity and good reproducibility, which can be applied in the quality control of Jiuwei Zhaxun pills.
RESUMO
This study was aimed to establish a method for quality control of Tibetan medicine Shi-Wei Xiao-Shi-San (SWXSS). Thin layer chromatography (TLC) was established for the qualitative determination. Cinnamal and piperine were determined by HPLC. The separation was performed on Phenomenex C18 column (4.6 mm × 250 mm, 5μm). The results showed that TLC can be used in the identification of pomegranate seed and Terminalia chebula. The linear ranges of cinnamal and piperine were within the range of 0.06-0.37μg and 0.05-0.33μg, respectively. And the standard line was Y=9.273 2×106X-2.348 2×105, r=0.999 8;Y=7.315×103X-3.857, r=1.000 0. It was concluded that the identification method was specific, accurate and practical, which can be applied in the quality control of SWXSS.