Simultaneous Determination of 19 Bioactive Constituents in QishenYiqi Dropping Pills by Ultra-Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry.

Background

QishenYiqi dripping pills (QSYQ), consisting of Salvia miltiorrhiza, Astragalus membranaceus, Panax notoginseng, and Dalbergia odorifera, is a widely used to treat ischemic cerebrovascular and hemorrhagic cerebrovascular in China.

Objective

In this study, a rapid and sensitive ultra-HPLC coupled with a triple quadrupole MS (UHPLC-QQQ-MS) method was established for the simultaneous quantification of 19 bioactive components.

Methods

Chromatographic separation was performed on an Agilent Eclipse Plus C18 Rapid Resolution High Definition (RRHD) column (2.1 × 50 mm, 1.8 μm) with a mobile phase composed of a 0.1% (v/v) formic acid aqueous solution and acetonitrile in a gradient elution manner. A QQQ-MS was used in positive and negative ionization mode with multiple reactions monitoring for quantitative analysis.

Results

The established methods were validated with linearity, precision, repeatability, stability, recovery, and matrix effect. All calibration curves exhibited excellent linear relationship with the correlation coefficient (r) >0.9985 for each analyte within the test range. This method was successfully applied to quantify target compounds of different structural types in 12 batches of QSYQ.

Conclusions

The results suggest that the established method is rapid, sensitive, and reliable. The developed UHPLC-QQQ-MS method can provide scientific basis and reference to quality control and consistency evaluation of QSYQ sample and other formulations. Highlights: A rapid, sensitive, and reliable UHPLC-QQQ-MS method has been developed and validated for simultaneous determination of 19 compounds including phenolic acids, saponins, isoflavonoids, and tanshinones in QSYQ for the first time.