On-line stop-flow two-dimensional liquid chromatography–mass spectrometry method for the separation and identification of triterpenoid saponins from ginseng extract

Abstract

A method based on stop-flow two-dimensional liquid chromatography coupled with electrospray ionization mass spectrometry (2D LC-ESI MS) was established and applied to analyze triterpenoid saponins from the main root of ginseng. Due to the special structure of triterpenoid saponins (they contain polar sugar side chains and nonpolar aglycones), hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RPLC) were used for the two dimensions, respectively. A trap column was used to connect the two dimensions. The dilution effect, which is one of the main shortcomings of traditional comprehensive 2D LC methods, was largely avoided. The peak capacity of this system was 747 and the orthogonality was 56.6 %. Compared with one-dimensional HILIC or RP LC MS analysis, 257 and 185 % more mass spectral peaks (ions with intensities that were higher than 1,000) were obtained from the ginseng main root extracts, and 94 triterpenoid saponins were identified based on MS(n) information and summarized aglycone structures. Given its good linearity and repeatability, the established method was successfully applied to classify ginsengs of different ages (i.e., years of growth), and 19 triterpenoid saponins were found through statistical analysis to vary in concentration depending on the age of the ginseng.

PEI-assisted boronate affinity magnetic nanoparticle-based SELEX for efficient in vitro evolution of saponin-binding aptamers

“…Due to the rapid development of separation science, different techniques have been employed for separation of saponins, including TLC, 5,6 reverse phase chromatography (RPLC), 7–9 HILIC, 10 CE 11 and immunoaffinity chromatography (IAC). 12,13 However, the existing approaches are associated with several drawbacks.…”

Preparing molecularly imprinted nanoparticles of saponins via cooperative imprinting strategy

“…Up to now, a series of techniques have been developed to separate of saponins, including TLC [4,5], reverse phase chromatography [6‐8], HILIC [9,10], and CE [11]. However, the existing approaches are unable to discriminate specific saponins from real samples.…”

Application of fractionized sampling and stacking for construction of an interface for online heart-cutting two-dimensional liquid chromatography

“…For HILIC × RP 2D LC, dilution of 1 D eluate prior to injection into 2 D column has achieved lots of good performances [18][19][20][21][22]. Typically for those techniques using additional dilution pumps and trap columns, dilution and trapping of 1 D eluate occurred at the same time and thus usually need high pressure pump to provide high-flow-rate weak solvent.…”