101. On-line comprehensive two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography for preparative isolation of toad venom
- Author
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Xia Yan, Jia-Fu Li, Ying-Kun Qiu, Yun-Long Wu, Fang Rong Chang, Hua Fang, and Zhen Wu
- Subjects
Spectrometry, Mass, Electrospray Ionization ,Magnetic Resonance Spectroscopy ,Chemical substance ,Analytical chemistry ,01 natural sciences ,Biochemistry ,Bufo bufo ,Analytical Chemistry ,Vacuum evaporation ,Toad Venom ,Automation ,Adsorption ,Animals ,Chromatography, High Pressure Liquid ,Chromatography, Reverse-Phase ,Chromatography ,010405 organic chemistry ,Chemistry ,010401 analytical chemistry ,Organic Chemistry ,Temperature ,General Medicine ,Reversed-phase chromatography ,0104 chemical sciences ,Separation process ,Bufanolides ,Solvent ,Amphibian Venoms ,Chromatography, Liquid ,Bufo bufo gargarizans - Abstract
An on-line comprehensive preparative two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography (2D NPLC×RPLC) system was constructed with a newly developed vacuum evaporation assisted adsorption (VEAA) interface, allowing fast removal of NPLC solvent in the vacuum condition and successfully solving the solvent incompatibility problem between NPLC and RPLC. The system achieved on-line solvent exchange within the two dimensions and its performance was illustrated by gram-scale isolation of crude extract from the venom of Bufo bufo gargarizans. Within separation time of ∼20h, 19 compounds were obtained with high purity in a single run. With the VEAA interface, the 2D system exhibited apparent advantages in separation efficiency and automation compared with conventional methods, indicating its promising application in the routine separation process for complicated natural products.
- Published
- 2016