ABSTRACT
Objective: To analyze 167 batches of Weiling granules according to the quality standard and exploratory research, and evaluate the overall quality and standard condition of the preparation. Methods: A TLC method was established for the identification of Atractylodis macrocephalae Rhizoma;an HPLC method was established for the fingerprint and the content determination of paeoniflorin, tetrahydropalmatine and ammonium glycyrrhizinate. An Agilent Poroshell120,SB-C18analytical column (100 mm×4. 6 mm, 2. 7 μm) was employed with gradient elution of acetonitrile-0. 1% phosphoric acid as the mobile phase at the flow rate of 1. 8 ml·min-1, and the sample size was 3 μl. Acid base titration method was used for measuring acid-neutralizing capacity. Results: No interference from the negative controls was shown to the TLC identification of Atractylodis macrocephalae Rhizoma. The fingerprint exhibited better separation of each peak. The precision, reproducibility and stability of the method were good,and the RSDs of the relative retention time and rela-tive peak area were less than 3. 0% . The linear range of paeoniflorin, tetrahydropalmatine and ammonium glycyrrhizinate was 0. 057-0. 568 μg(r=0. 999 9), 0. 035-0. 353 μg(r=0. 999 9)and 4. 244×10 -3-42. 44×10 -3μg(r=0. 999 9), respectively, and the av-eragerecoverywas99.3%(RSD=1.0%,n=6),100.0%(RSD=0.8%,n=6) and99.8%(RSD=1.2%,n=6),respectively. The average recovery of acid-neutralizing capacity was 99. 5% (RSD=0. 5% ,n=6). Conclusion: Exploratory research increases the specificity, controllability and safety of the standards, which provides reference for the further drug standards revision and the drug quality control.
ABSTRACT
Objective:To establish a method for detecting synthetic pigments in Chinese patent drugs by solid phase extraction-HPLC(SPE-HPLC). Methods:Purified with SPE and concentrated, the sample was separated on a SHISEIDO C18 column with 0. 02 mol·L-1 ammonium acetate and methanol mixed solution as the mobile phase with gradient elution at the flow rate of 1. 0 ml·min-1 , the detection wavelength of 508nm, column temperature of 30℃,and the injection volume of 10μl. Results: The linear range of the synthetic pigments was 0. 005-0. 200 μg(r=0. 999 9), and the average recovery was 97. 6%(RSD=1. 3%,n=6),97. 0%(RSD=1. 4%,n=6) and 99. 5%(RSD=1. 4%,n=6), respectively. Conclusion:The proposed method is simple, reliable and reproduci-ble, and especially suitable for the detection of synthetic pigments in Chinese patent drugs.