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Elucidation of steroid glycosides in Anemarrhena asphodeloides extract by means of comprehensive two-dimensional reversed-phase/polyamine chromatography with mass spectrometric detection
Authors:Zhirui Liu  Dongliang Zhu  Yunpeng Qi  Xiaofei Chen  Zhenyu Zhu  Yifeng Chai
Institution:School of Pharmacy, Second Military Medical University, Shanghai, China; Shanghai Key Laboratory for Pharmaceutical Metabolite Research, Shanghai, China.
Abstract:In the work presented here, a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Reversed-phase liquid chromatography was employed for the first-dimension separation and polyamine chromatography was chosen for the second-dimension separation mode. The two dimensions are highly orthogonal and the separation efficacy of the developed octadecylsilica × polyamine was tested by separating an extract from Anemarrhena asphodeloides. The steroid glycosides identified by comprehensive two-dimensional liquid chromatography in this experiment were compared to those obtained for monodimensional liquid chromatography. The comprehensive two-dimensional liquid chromatography system, thanks to the complementary separation selectivity and enhanced peak capacity provided by the two columns, allowed to distribute five compounds of low amounts otherwise unachievable by monodimensional liquid chromatography. In addition, four steroid isomers with similar fragmentation characteristics in MS/MS spectra, were newly separated based on their different chemical structures.
Keywords:Anemarrhena asphodeloides  Comprehensive LC  Polyamine column  Steroid glycoside
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