Two-dimensional countercurrent chromatography x high performance liquid chromatography for preparative isolation of toad venom

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	Two-dimensional countercurrent chromatography x high performance liquid chromatography for preparative isolation of toad venom
	Qiu, Ying-Kun ; Yan, Xia ; Fang, Mei-Juan ; Chen, Lin ; Wu, Zhen ; Zhao, Yu-Fen ; Qiu YK(邱鹰昆) ; Fang MJ(方美娟) ; Wu Z(吴振) ; Zhao YF(赵玉芬)
刊名	http://dx.doi.org/10.1016/j.chroma.2014.01.029
	2014-02-28
关键词	SOLID-PHASE EXTRACTION BUFO-BUFO GARGARIZANS NATURAL-PRODUCTS CYTOTOXIC CONSTITUENTS PURIFICATION COMBINATION SEPARATION SKIN
英文摘要	National Natural Science Foundation of China [81102333, 81273400]; Fundamental Research Funds for the Central Universities [2010121108]; Fujian Natural Science Foundation for Distinguished Young Scholars [2012106020]; Natural Science Foundation of Fujian Province of China [2011J05101]; In this work, a new on-line two-dimensional chromatography coupling of flow programming countercurrent chromatography and high-performance liquid chromatography (2D CCC x HPLC) was developed for preparative separation of complicated natural products. The CCC column was used as the first dimensional isolation and a preparative ODS column operated in reversed-phase (RP) mode as the second dimension. The CCC was operated at a controlled flow rate to ensure that each fraction eluted within one hour, corresponding to the isolation time of the 2nd dimensional preparative HPLC. The eluent from the 1st dimensional CCC was diluted using a makeup pump and trapped onto holding column, before been eluted and transferred to the 2nd dimensional HPLC. The performance of the holding column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure, for the solution to the issue of online trapping of low pressure eluent from a CCC column. Satisfactory trapping efficiency and tolerable CCC pressure can be achieved using a commercially available 15 mm x 30 mm i.d. ODS pre-column. The present integrated system was successfully applied in a one-step preparative separation of 12 compounds, from the crude methanol extract of venom of Bufo bufo gargarizans. Compounds 1-12 were isolated in overall yield of 1.0%, 0.8%, 2.0%, 13%, 2.0%, 1.5%, 1.9%, 3.6%, 6.1%, 4.8%, 3.5% and 4.1%, with HPLC purity of 99.9%, 99.7%, 90.6%, 99.9%, 77.0%, 99.9%, 90.4%, 99.9%, 52.0%, 99.9%, 99.3%, and 85.0%, respectively. All the results demonstrate that the flow programming CCC x HPLC method is an efficient and convenient way for the separation of compounds from toad venom and it can also be applied to isolate other complex multi-component natural products. (C) 2014 Elsevier B.V. All rights reserved.
语种	英语
出版者	ELSEVIER SCIENCE BV
内容类型	期刊论文
源URL	[http://dspace.xmu.edu.cn/handle/2288/93664]
专题	医学院－已发表论文
推荐引用方式 GB/T 7714	Qiu, Ying-Kun,Yan, Xia,Fang, Mei-Juan,et al. Two-dimensional countercurrent chromatography x high performance liquid chromatography for preparative isolation of toad venom[J]. http://dx.doi.org/10.1016/j.chroma.2014.01.029,2014.
APA	Qiu, Ying-Kun.,Yan, Xia.,Fang, Mei-Juan.,Chen, Lin.,Wu, Zhen.,...&赵玉芬.(2014).Two-dimensional countercurrent chromatography x high performance liquid chromatography for preparative isolation of toad venom.http://dx.doi.org/10.1016/j.chroma.2014.01.029.
MLA	Qiu, Ying-Kun,et al."Two-dimensional countercurrent chromatography x high performance liquid chromatography for preparative isolation of toad venom".http://dx.doi.org/10.1016/j.chroma.2014.01.029 (2014).