Simultaneous determination of seven effective components in Shenkui Tongmai granules based on UHPLC-MS/MS

色谱法 化学 重复性 醋酸铵 选择性反应监测 淫羊藿苷 橙皮苷 串联质谱法 质谱法 高效液相色谱法 医学 病理 替代医学
作者
Shun Liu,Yixuan Wang,Haidan Wang,Zhirong Geng,Shihai Yan
出处
期刊:Journal of Pharmacy and Pharmacology [Oxford University Press]
卷期号:73 (6): 758-766 被引量:1
标识
DOI:10.1093/jpp/rgab017
摘要

Abstract Objectives The objective of the study was to establish the quality standard of the formulation of Shenkui Tongmai granules (SKTM) from the perspective of safety and effectiveness. Methods A sensitive and specific method to simultaneously detect seven effective components by ultra-high performance liquid chromatography-tandem-mass spectrometry (UHPLC-MS/MS) in SKTM, including calycosin 7-O-β-d-glucopyranoside, icariin, sodium danshensu, hyperoside, astragaloside IV, hesperidin, and salvianolic acid, was developed and validated. A Kromasil 100–3.5 C18 column with a mobile phase of 6.5 mmol/l ammonium acetate in acetonitrile was used to separate these above-listed components. Gradient programming was used with a flow rate of 0.2 ml/min, and the components were achieved in 13 min. Multiple reaction monitoring (MRM) in positive/negative mode was applied for the MS/MS detection. Key findings The analytical method was satisfactorily validated for linearity, accuracy and precision, repeatability and stability. The developed UHPLC-MS/MS method had high repeatability and accuracy and it was in a good linear relationship within their respective ranges (r = 0.9999) with the RSD value of the sample recovery of less than 5%. Conclusions The current method established here is suitable for use in determining seven effective components in SKTM simultaneously, which may provide a new reliable method for overall quality control of SKTM.
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