RESUMEN
Ultra-performance liquid chromatography-evaporative light scattering detection (UPLC-ELSD) fingerprint analysis method was established for quality control of Guci tablets. Chromatographic separation was performed on Waters Acquity UPLC BEH C₁₈ column (2.1 mm×100 mm, 1.7 μm) at 30 °C of column temperature. Acetonitrile-0.1% formic acid solution was adopted as mobile phase for gradient elution. The flow rate was set at 0.3 mL·min⁻¹, and the injection volume was 3 μL. Detection was carried out on an ELSD with a nitrogen pressure of 0.28 MPa, drift tube temperature of 60 °C, and gain of 400. A total of 39 batches of samples produced by six manufacturers were measured by using the above method and the data were analyzed by ChemPattern software. The peak present in more than 75% of the samples was defined as a common peak, and 30 common peaks were determined. Among them, 19 peaks were identified by rapid resolution liquid chromatography/tandem mass spectrometry (RRLC-MS/MS) method, 16 of which were confirmed by reference substances. The similarity of the tested samples was 0.47-0.98, suggesting that the quality of the samples from different manufacturers varied greatly. Furthermore, principal component analysis (PCA) and hierarchical analysis (HCA) were performed to clarify the main different components in samples. The results indicated that there might be some feeding problems about Paeoniae Radix Alba, Notoginseng Radix et Rhizoma, and Clematidis Radix et Rhizoma in a few manufacturers. This study provided some evidences for the overall quality control of Guci tablets, as well as its quality standard improvements.
RESUMEN
Objective:To screen auramine O in Guci tablets. Methods:Auramine O was detected by HPLC method on a Diamon-sil-C18(250mm×4.6mm,5μm)columnwiththemobilephaseofacetonitrile-0.025mol·L-1monopotassiumphosphatebuffersolu-tion(containing 0. 2% triethylamine,adjusting pH to 3. 0 with phosphoric acid)(36∶65)at the flow rate of 0. 8 ml·min-1. The detec-tion wavelength was 432 nm and the column temperature was 35℃. Results:The LOD of auramine O was 0. 05ng. Among 45 batches of tested samples, auramine O was found in seven ones. Conclusion:The method is simple, rapid and accurate, which can guarantee the drug safety of Guci tablets.