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首页> 外文期刊>Journal of Planar Chromatography-Modern TLC: JPC >Application of column chromatography and preparative TLC for isolation and purification of coumarins from Peucedanum tauricum Bieb. fruits
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Application of column chromatography and preparative TLC for isolation and purification of coumarins from Peucedanum tauricum Bieb. fruits

机译:柱色谱法和制备型薄层色谱法在金合欢中分离和纯化香豆素的应用。水果

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摘要

Column chromatography and normal- and reversed-phase TLC have been used for the purification, separation, and isolation of coumarins from the fruits of Peucedanum tauricum Bieb. (Umbelliferae = Apiaceae). Preliminary purification of the coumarin sediment obtained from a petroleum ether extract was performed by preparative column chromatography on silica gel with a gradient of ethyl acetate in dichloromethane as mobile phase, and by preparative reversed-phase thin-layer chromatography with 90% aqueous MeOH as mobile phase. Preparative normal-phase TLC with cyclohexane and ethyl acetate as mobile phase, then re-chromatography with more selective mobile phase mixtures of ethyl acetate, dichloromethane, n-heptane, and acetonitrile enabled isolation of four crystalline coumarins (A-D). All the steps of these procedures were monitored by analytical TLC (with detection by UV illumination at < lambda > = 366 nm and densitometric scanning at < lambda > = 320 nm). Isolated crystalline coumarins were identified by comparison with standards in analytical TLC and in RPHPLC with gradient elution, and by melting point (m.p.) measurement and UV spectroscopy. Two were identified as isoimperatorin (A), and bergapten (C); this is the first time these compounds have been isolated from P. tauricum Bieb.
机译:柱色谱以及正相和反相TLC已用于从金合欢(Peucedanum tauricum Bieb)果实中纯化,分离和分离香豆素。 (伞形科=伞形科)。从石油醚提取物中获得的香豆素沉淀物的初步纯化是通过硅胶制备柱色谱法,以乙酸乙酯在二氯甲烷中的梯度为流动相,以及制备反相薄层色谱法,以90%MeOH水溶液为流动相。相。使用环己烷和乙酸乙酯作为流动相的制备型正相薄层色谱,然后使用乙酸乙酯,二氯甲烷,正庚烷和乙腈等更具选择性的流动相混合物进行色谱分离,可以分离出四种结晶香豆素(A-D)。这些步骤的所有步骤均通过分析TLC进行监控(通过在<λ> = 366 nm处的紫外线照射和在<λ> = 320 nm处的光密度扫描进行检测)。分离的结晶香豆素通过与分析型TLC和RPHPLC中的标准品进行梯度洗脱比较,并通过熔点(m.p.)测量和UV光谱法进行鉴定。两种被鉴定为异欧前胡素(A)和香柠檬素(C);这是第一次从金牛假单胞菌中分离出这些化合物。

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