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首页> 美国卫生研究院文献>Molecules >Preparative Isolation of Two Prenylated Biflavonoids from the Roots and Rhizomes of Sinopodophyllum emodi by Sephadex LH-20 Column and High-Speed Counter-Current Chromatography
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Preparative Isolation of Two Prenylated Biflavonoids from the Roots and Rhizomes of Sinopodophyllum emodi by Sephadex LH-20 Column and High-Speed Counter-Current Chromatography

机译：Sephadex LH-20色谱柱和高速逆流色谱法从中华对虾的根和根中分离制备两种炔丙基双黄酮类化合物

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摘要

Two prenylated biflavonoids, podoverines B–C, were isolated from the dried roots and rhizomes of Sinopodophyllum emodi using a Sephadex LH-20 column (SLHC) and high-speed counter-current chromatography (HSCCC). The 95% ethanol extract was partitioned with ethyl acetate in water. Target compounds from the ethyl acetate fraction were further enriched and purified by the combined application of SLHC and HSCCC. n-Hexane–ethyl acetate–methanol–water (3.5:5:3.5:5, v/v) was chosen as the two phase solvent system. The flow rate of mobile phase was optimized at 2.0 mL·min−1. Finally, under optimized conditions, 13.8 mg of podoverine B and 16.2 mg of podoverine C were obtained from 200 mg of the enriched sample. The purities of podoverines B and C were 98.62% and 99.05%, respectively, as determined by HPLC. For the first time, podoverins B and C were found in the genus Sinopodophyllum. Their structures were determined by spectroscopic methods (HR-ESI-MS, 1H-NMR, 13C-NMR, HSQC, HMBC). Their absolute configurations were elucidated by comparison of their experimental and calculated ECD spectra. The cytotoxic activities were evaluated against MCF-7 and HepG2 cell lines. The separation procedures proved to be practical and economical, especially for trace prenylated biflavonoids from traditional Chinese medicine.
机译：使用Sephadex LH-20色谱柱（SLHC）和高速逆流色谱法（HSCCC）从中华po的干燥根和根茎中分离出两个烯丙基化的类黄酮类化合物— Podoverine B–C。将95％乙醇萃取物用乙酸乙酯在水中分配。通过合并应用SLHC和HSCCC，进一步纯化和纯化乙酸乙酯级分中的目标化合物。选择正己烷-乙酸乙酯-甲醇-水（3.5：5：3.5：5，v / v）作为两相溶剂系统。流动相的流速最优化为2.0 mL·min -1 。最后，在优化的条件下，从200 mg的富集样品中获得13.8 mg的Podoverine B和16.2 mg的PodoverineC。通过HPLC测定，足蛋白B和C的纯度分别为98.62％和99.05％。首次在中华Sino子属中发现了Podoverins B和C。通过光谱法（HR-ESI-MS， 1 H-NMR， 13 C-NMR，HSQC，HMBC）确定它们的结构。通过比较实验和计算的ECD光谱，阐明了它们的绝对构型。评价了针对MCF-7和HepG2细胞系的细胞毒性活性。分离方法被证明是实用且经济的，特别是对于中药中痕量的烯丙基双黄酮类化合物而言。

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