Analysis of six bioactive components in Semen Ziziphi Spinosae by UPLC-ELSD and UPLC-Q/TOF-MS

Abstract

A simple and sensitive method was first developed for the simultaneous determination of six bioactive compounds in Semen Ziziphi Spinosae, which is commonly used in traditional Chinese medicines, by ultra-performance liquid chromatography coupled with an evaporative light scattering detector (UPLC-ELSD). Furthermore, the main compounds were identified using UPLC coupled with electrospray ionization and time-of-flight mass spectrometry (ESI-Q/TOF-MS). The separation of the compounds of interest was performed on a BEH C18 column with acetonitrile and water (0.1% aqueous formic acid) as the mobile phase. Six analytes (spinosin, jujuboside A, jujuboside D, jujuboside B, jujuboside B₁, betulinic acid) demonstrated good linearity (r² > 0.9984) over a relatively wide concentration range. The method revealed high average recovery (range, 94.36–99.49%) and good precision with inter- and intra-day variations with RSD less than 4.72%. The limits of detection (LOD) ranged from 10.4–31.2 ng, while the limits of quantification (LOQ) were defined in the range of 21.9–84.0 ng. The validated method was successfully applied to quantitatively analyze 28 samples of different places from China. The results show there are great variations among the contents of the six ingredients. These results demonstrate that this approach has the potential for the quality control of Semen Ziziphi Spinosae.