ABSTRACT
Objective:To establish an HPLC method for the simultaneous determination of 18α-glycyrrhizic acid and 18β-glycyr-rhizic acid in diammonium glycyrrhizinate .Methods:A Diamonsil C18 column (200 mm ×4.6 mm, 5 μm) was used with the mobile phase of water (water-60%perchloric acid solution:48∶0.5, adjusting pH to 8.0 with ammonium hydroxide)-methanol (48∶52). The detection wavelength was set at 248 nm and the flow rate was 1.0 ml· min-1 .The column temperature was 30℃and the injection volume was 20 μl.Results:18α-Glycyrrhizic acid and 18β-glycyrrhizic acid were well separated .They had a good linear relationship within the range of 0.005 0-1.000 0 mg· ml-1(r=0.999 7 and 0.999 3).The average recovery was 99.7%and 99.1%, and RSD was 0.9%and 0.4%, respectively (n=9).Conclusion:The method is accurate, simple and reproducible, which can be used for the simultaneous determination of the two constituents in diammonium glycyrrhizinate .
ABSTRACT
Objective: To establish the methods for identifying the related substances in Diammonium Glycyrrhizinate Enteric Coated Tablet (DGECT) by ultra high performance liquid-diode array-ion trap-the time of flight tandem mass spectrometry (UPLC-DAD-IT- TOF-MS). Methods: The chromatographic separation was performed on an Agilent HC-C18 (250 mm × 4.6 mm, 5 μm) column, mobile phase was acetonitril-H2O-Hac (380:614:6), eluting sample was in equal degree flow, with volume flow rate of 1 mL/min, UV detection wavelength of 254 nm, and mass spectrum monitoring mass-to-charge ratio range m/z 100-1000. Results: Including licoricesaponine G2, H2, E2, B2, J2, C2, 18α-glycyrrhizic acid, and glycyrrhiza uralensis saponin (A or B), the eight kinds of related compounds existed were found. Conclusion: The related substances found in DGECT are valuable for the manufacturing process and quality control.