Column chromatography normal values

Normal-phase TLC has been employed for the separation of two new flavans in the extract of the undergorund tubers of Cyperus conglomeratus Rottb. (family Cyperaceae). The underground tubes were dried, ground and were extracted with with petroleum ether diethyl ether-methanol (1 1 1, v/v) for 24 h at ambient temperature. The extract was defatted with cold methanol. The components of the extract were preliminarily separated by traditional column chromatography followed by GC/MS and TLC. New flavans (5-hydroxy-7,3, 5 -trimethoxyflavan and 5,7-hydroxy-3, 5 -dimethoxyflavan) were separated on silica TLC layers using petroleum ether-diethyl ether (1 3, v/v) with the RF values of 0.50 and 0.37 for dimethoxy and trimethoxy derivatives, respectively [115]. 

Relative retentions..the a values..usually vary Inversely with column temperature, but are most strongly affected by the choice of liquid phase. In packed column chromatography, the choice of liquid phase Is usually the most effective route by which separation efficiency Is Influenced. In capillary GC, however, there Is normally such an abundance of theoretical plates that the choice of liquid phase Is a relatively unimportant parameter for many analyses. In some cases however. It does become desirable (or even necessary) to select a liquid phase in which the relative retentions of certain solutes Is larger. Until quite recently, this posed a real problem with the fused silica capillary column, because the more polar liquid phases, l.e. those In which relative retentions are usually greater, coated fused silica only reluctantly, and produced columns whose useful lives were quite limited. The development of stable bonded phase columns ( ) eventually overcame this difficulty (vide Infra). 

Aboul-Enein and Ali [78] compared the chiral resolution of miconazole and two other azole compounds by high performance liquid chromatography using normal-phase amylose chiral stationary phases. The resolution of the enantiomers of ( )-econazole, ( )-miconazole, and (i)-sulconazole was achieved on different normal-phase chiral amylose columns, Chiralpak AD, AS, and AR. The mobile phase used was hexane-isopropanol-diethylamine (400 99 1). The flow rates of the mobile phase used were 0.50 and 1 mL/min. The separation factor (a) values for the resolved enantiomers of econazole, miconazole, and sulconazole in the chiral phases were in the range 1.63-1.04 the resolution factors Rs values varied from 5.68 to 0.32. 

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