Liquid chromatography-tandem mass spectrometry combined with high-performance liquid chromatography for evaluating the quality of Xiebai powder reference sample
Objective:To establish a method for determining the specific chromatogram of Xiebai powder refer-ence sample using liquid chromatography-tandem mass spectrometry(LC-MS/MS)for the identification and attribu-tion of each characteristic peak,and to evaluate the quality of the reference sample by establishing the methods for con-tent determination of quality control indicators for each traditional Chinese medicine(TCM)drug in the reference sam-ple.Methods:The fingerprint study was conducted on a Hypersil ODS2 column(250 mm × 4.6 mm,5 μm)with the mobile phase of acetonitrile-0.1％phosphoric acid/formic acid for gradient elution at a detection wavelength of 280 nm,a flow rate of 1.0 ml/min,a column temperature of 25℃,and a sample size of 10 μl,and LC-MS/MS with the same chromatograph conditions was performed for peak attribution and chemical component analysis.The specific peak identified for each TCM drug was used to establish the methods for content determination of quality control indica-tors for the reference sample.Results:The specific chromatogram of Xiebai powder reference sample had a good repro-ducibility,and the solution of the test article remained stable within 48 hours.Detection of multiple batches obtained 14 common peaks on the fingerprint of Xiebai powder,with a similarity of＞0.9,and peak attribution showed that 5 were attributed to fried Cortex Mori,5 were attributed to Radix Glycyrrhizae Preparata,and 3 were attributed to Cortex Lycii.A total of 11 chromatographic peaks were identified by LC-MS/MS.The method for content determination were estab-lished for mulberroside A,glycyrrhizic acid,and lyciumin B,and the results showed that the method had good specificity and reproducibility,with a recovery rate of 94.9％,93.5％,and 95.2％,respectively.Conclusion:The method for de-termining the fingerprint is feasible after validation and can effectively identify Xiebai powder decoction pieces with three TCM drugs,and its combination with LC-MS/MS component analysis can effectively determine the quality control components for each drug.Methodological investigation shows that the method for determining the content of mulberro-side A,glycyrrhizic acid,and lyciumin B is feasible.
Xiebai powderreference sampleliquid chromatography-tandem mass spectrometrycomponent analysishigh-performance liquid chromatography
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