| Dahuangzhechong tablet is a classic prescription in the “Synopsis of Golden Chamber”which was witten by Zhang Zhongjing who is a famous doctor in the Han Dynasty. The function of Dahuangzhechong tablet is promoting blood circulation and removing blood stasis,and it’s widely used in clinical practice. It’s Contains 12 kinds of Chinese medicinal powder. In the present study, we research the quality standard for Dahuangzhechong tablets by establish the method for identification of Rhubarb, Radix Scutellariae, Radix Paeoniae Alba and Licorice by TLC, and the HPLC method for determination the content of free emodin,free chrysophanol,total emodin and total chrysophanol. Part 1 TLC identification of Radix Paeoniae Alba, Radix Scutellariae,Rhubarb and LicoriceObjective: To study the TLC method of Radix Paeoniae Alba, Radix Scutellariae, Rhubarb and Licorice in the Dahuangzhechong tablets.Methods: Take the four components of Dahuangzhechong tablets,Rhubarb, Radix Scutellariae, Radix Paeoniae Alba and Licorice as the index components. By the four kinds of Chinese medicine control and negative control,study on the TLC identification method of Dahuangzhechong tablets.Results:(1)The rhubarb TLC identification was distinct,the spots were clear and the blank test showed no interference.(2)The radix scutellariae TLC identification was not distinct,the spots were not clear, but the blank test showed no interference.(3)The licorice TLC identification was distinct,the spots were clear and the blank test showed no interference.(4)The radix paeoniae alba TLC identification was not distinct,the spots were not clear,but the blank test showed no interference.Conclusion: The established TLC methods of rhubarb and licorice are very good. The established TLC methods of radix scutellariae and radix paeoniae alba are not perfect, we need to do further exploration and research from the extraction methods, developing agent proportioning and other aspects. Part 2 Content determination of free emodin and free Chrysophanol inDahuangzhechong tablets by HPLCObjective: To study the HPLC method for determination the content of free emodin and free chrysophanol in the Dahuangzhechong tablets.Methods:To study the HPLC method and methodology validation for determination the content of free emodin and free chrysophanol from the chromatographic condition,extraction methods, sample volume and other aspects.Results: Chromatographic conditions: the chromatographic column was ODS column(4.6 mm×250mm, 5μm); mobile phase was acetonitrile- methanol-0.1%phosphoric acid; isocratic elution;UV detection wavelength was set at 254 nm. Extraction conditions: extraction with methanol for 30 min by using ultrasound. Determine the content of free emodin and free chrysophanol in the 0.5g sample volume of Dahuangzhechong tablets by using the method above. This method is highly specific. Emodin peak purity and chrysophanol peak purity are meet the requirement.The linear relation,repeatability, rate of recovery, stability, durability are well.Conclusion: The established HPLC method for determination the content of free emodin and free chrysophanol is highly specific, simple and reliable. Part 3 Content determination of total emodin and total Chrysophanol inDahuangzhechong tablets by HPLCObjective: To study the HPLC method for determination the content of total emodin and total Chrysophanol in the Dahuangzhechong tablets. This method is feasible.Methods: To study the HPLC method and methodology validation for determination the content of total emodin and total Chrysophanol from the chromatographic condition,extraction methods, sample volume and other aspects.Results: Chromatographic conditions: the chromatographic column was ODS column(4.6 mm×250mm, 5μm); mobile phase was acetonitrile- methanol-0.1%phosphoric acid; isocratic elution;UV detection wavelength was set at 254 nm. Extraction conditions: reflux extraction with methanol-hydrochloric(10:1)acid at 80℃ in water for 30 min. Put 5ml of the filtrate and 2ml of 2﹪Na OH into 10 ml volumetric flask. Determine the content of total emodin and total chrysophanol in the 0.5g sample volume of Dahuangzhechong tablets by using the method above. This method is highly specific. Emodin peak purity and chrysophanol peak purity are meet the requirement. The linear relation,repeatability, rate of recovery, stability, durability are well.Conclusion: The established HPLC method for determination the content of total emodin and total chrysophanol is highly specific, simple and reliable. This method is feasible. |
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