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Thermodynamic study of the retention behaviour of selected macrocycles using reversed-phase high-performance thin-layer chromatography plates and methanol-water mobile phases

机译:反相高效薄层色谱板和甲醇-水流动相对选定大环化合物保留行为的热力学研究

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摘要

The influence of temperature and mobile-phase composition on retention of α-, β-, and γ-cyclodextrins and two macrocyclic antibiotics (rifamycin B and rifampicin) has been examined by reversed-phase thin-layer chromatography, using wide-range (0-100%) binary mixtures of methanol-water. Retardation fact9rs (R_F) of the solute molecules were measured at different temperatures from 5 to 60°C. Temperature changes of the chromatographic conditions produce significant differences in migration of the investigated macrocyclic compounds. Generally, the plots of the rate mobility factor (R_M) versus the reciprocal of the absolute temperature are linear. The ranges of mobile-phase composition in which R_F values are equal to unity were wider at higher temperatures. From linear Van't Hoff plots thermodynamic parameters such as the change of enthalpy (△H°) and the change of entropy (△S") were estimated. In each case the sign of the calculated parameters is negative. However, the magnitudes of △H° and △S° indicate significant thermodynamic differences between two groups of solutes, one of which includes α- and γ-cyclodextrins and the other macrocyclic antibiotics and β-cyclodextrin.
机译:温度和流动相组成对α-,β-和γ-环糊精和两种大环抗生素(利福霉素B和利福平)保留的影响已通过反相薄层色谱法进行了研究,使用宽范围(0 -100%)甲醇-水的二元混合物。在5至60°C的不同温度下测量了溶质分子的延迟事实(R_F)。色谱条件的温度变化在所研究的大环化合物的迁移方面产生了显着差异。通常,速率迁移率因子(R_M)与绝对温度的倒数的关系图是线性的。 R_F值等于1的流动相组成范围在较高温度下较宽。从线性Van't Hoff图可以估算出热力学参数,例如焓变(△H°)和熵变(△S“)。在每种情况下,计算出的参数的符号均为负。 △H°和△S°表示两组溶质之间存在明显的热力学差异,其中一组包含α-和γ-环糊精,另一类包含大环抗生素和β-环糊精。

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