Abstract

In the present study, we developed a liquid chromatography-diode array detector-electrospray ionization/mass spectrometric (LC-DAD-ESI/MS) method for analysis of saikosaponins in Bupleurum falcatum. The LC method employed a ZORBAX SB-Aq analytical column (150 × 4.6 mm i.d., 5 μm) at a flow rate of 0.8 mL/min coupled with a diode array detector at 204 nm. A step gradient of acetonitrile-water (v/v) containing 0.5% formic acid from 30 to 70% was applied, leading to a sample analysis time of 30 min. The ESI-MS was carried out in positive and negative modes from 500 to 1,500 m/z. Saikosaponins c, a, and d gave strong sodium adducts at m/z 949.6, 803.5 and 803.6, respectively, in positive mode. The data indicate that the present LC-DAD-ESI/MS assay is an effective method for the determination of saikosaponins c, a and d from the roots of Bupleurum falcatum.

Highlights

  • Radix bupleuri (Chaihu in Chinese), as an old member of the family of traditional Chinese herbs, has been used in China to treat cold fevers, chills, and menstrual disorders for more than 2000 years [1].Generally, Radix bupleuri is derived from the dried roots of B

  • The data indicate that the present LC-diode array detection (DAD)-Electrospray ionization (ESI)/MS assay is an effective method for the determination of saikosaponins c, a and d from the roots of Keywords: LC-DAD-ESI/MS; saikosaponins; pressurized liquid extraction; Bupleurum falcatum

  • To date quite a few approaches have been developed for the determination of these saikosaponins in Radix bupleuri [12,13,14], a systematic study on the simultaneous determination of the three saikosaponins from B. falcatum by LC-DAD-ESI/MS analysis was not available

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Summary

Introduction

Radix bupleuri (Chaihu in Chinese), as an old member of the family of traditional Chinese herbs, has been used in China to treat cold fevers, chills, and menstrual disorders for more than 2000 years [1]. Radix bupleuri is derived from the dried roots of B. Because of the increasing demand as well as a shortage of quality product, Bupleurum falcatum (Sandaochaihu in Chinese) as one of the most important cultivars, have been used as medicine in different areas of China. To date quite a few approaches have been developed for the determination of these saikosaponins in Radix bupleuri [12,13,14], a systematic study on the simultaneous determination of the three saikosaponins from B. falcatum by LC-DAD-ESI/MS analysis was not available. A fast and sensitive LC-DAD-ESI/MS method for analysis of saikosaponins c, a, and d from the roots of B. falcatum was developed, which would be useful for quality control applications to Radix bupleuri and other plants associated with these ingredients

Optimization of LC Conditions
Optimization of Sample Preparation
Optimization of LC-MS
Linearity and Calibration Curves
Precision
Stability
Recovery
Reagents and Materials
Preparation of Standard Solutions
Sample Preparation
Conclusions
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