期刊
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
卷 1026, 期 -, 页码 67-74出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2015.11.015
关键词
Bufadienolides; Normal-phase liquid chromatography; Two-dimensional liquid chromatography; MS/MS; Toad skin
资金
- National Science Foundation of China [21305138]
- External Cooperation Program of BIC, Chinese Academy of Science [121421KYSB20130013]
- Key Projects in the National Science & Technology Pillar Program in the twelfth Five-year Plan [2012BAI29B08]
Bufadienolides possess various bioactivities especially antitumor. Due to the high structural diversity, the separation of bufadienolides often suffers from coelution problem on conventional RP columns. In this work, an off-line two-dimensional normal-phase liquid chromatography x reversed-phase liquid chromatography (2D-NPLC x RPLC) method was developed to separate and characterize bufadienolides in toad skin. Several RP and NP columns were evaluated with five reference bufadienlides. The XUnion C18 and XAmide columns exhibited superior chromatographic performances for bufadienlide separation, and were selected in RPLC and NPLC, respectively. RPLC was used in the second-dimension for the good compatibility with MS, while NPLC was adopted in the first-dimension. The orthogonality of the 2D-NPLC x RPLC system was investigated by the geometric approach using fifteen bufadienolide mixtures. The result was 49.6%, demonstrating reasonable orthogonality of this 2D-LC system. By combining the 2D-LC system with MS, 64 bufadienlides including 33 minor ones and 11 pairs of isomers in toad skin were identified. This off-line 2D-NPLC x RPLC allowed to solve the coelution problem of bufadienlides in one-dimension RPLC, and thus facilitated the identification significantly. (C) 2015 Elsevier B.V. All rights reserved.
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