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Date of Publication:2014-01-01

Journal:分析测试学报

Issue:9

Page Number:986-992

ISSN No.:1004-4957

Abstract:Bufadienolide is a kind of natural steroids with significant anti-cancer activities. Hitherto, the number of structural modification on the bufadienolides has reached more than 100 . The purifica-tion of sulfated,a trace cytotoxic component bufadienolides from toad skin is a tough work due to its low content and unstable structures. However,there is no report on synthesis of bufadienolides sul-fonation though they have promising cytotoxic activities. In this paper,the arenobufagin was firstly taken as an example,to develop an effective method for the synthesis of arenobufagin-3-O-sulfonate. In order to enrich the arenobufagin-3-O-sulfonate quickly and mildly,a reversed phase/hydrophilic solid-phase extraction method based on our homemade hydrophilic Click TE -Cys was developed. The structures of arenobufagin-3-O-sulfonate and arenobufagin were both identified by MS,1 H NMR and 13 C NMR spectra. In addition,the total bufogenins were sulfonated by this method and the sul-fated bufogenins were also successfully enriched via the reversed phase/hydrophilic solid-phase extrac-tion approach. Finally,a LC-MS system was employed to test the result,and about 20 sulfated bu-fogenins were primarily identified according to their molecular weight. Based on this, a systemic method was first developed for the synthesis and enrichment of the sulfated total bufogenins and a large number of potential anticancer new compounds were obtained,which provided lots of agents for fur-ther screening to achieve high effective and low toxic compounds. The efficient reversed phase/hydro-philic solid-phase extraction method for the enrichment of sulfated bufogenins could be used to enrich sulfated bufogenins in toad skin extract.

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