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Enantiomer Separation of Acidic Chiral Compounds on a Clarithromycin‐Zirconia Hybrid Monolith by Capillary Electrochromatography

机译:毛细管电色谱法分离克拉霉素-锆杂化整体上酸性手性化合物的对映异构体

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A carbamoylated clarithromycin‐incorporated zirconia hybrid monolith (CLA‐ZHM) was prepared in a fused silica capillary via an in situ sol–gel process. The CLA‐ZHM capillary column was employed for enantiomer separation of acidic chiral compounds by capillary electrochromatography in eluents consisting of acetonitrile, methanol, and acetic acid and triethylamine as electrolytes. Influences of the composition of eluent and applied voltage on enantiomer separation were investigated. Baseline resolutions were achieved for 10 acidic compounds in an eluent consisting of 70/30 acetonitrile/methanol with 255 mM acetic acid and 17.4 mM triethylamine at an applied voltage of ?10 kV and capillary temperature of 25 °C. Relative standard deviation values in resolution parameters for column to column and batch to batch repeatability were less than 2.7% (for n = 3) under the optimal separation settings, indicating that stability of the ZHM columns and reproducibility of the column preparation method are acceptable.
机译:在熔融石英毛细管中,通过原位溶胶-凝胶法制备了氨基甲酰化的克拉霉素结合的氧化锆杂化整料(CLA-ZHM)。 CLA-ZHM毛细管柱用于通过毛细管电色谱在由乙腈,甲醇,乙酸和三乙胺为电解质的洗脱液中分离酸性手性化合物的对映异构体。研究了洗脱液组成和施加电压对对映体分离的影响。在?10 kV的施加电压和25°C的毛细管温度下,在由70/30乙腈/甲醇与255 mM乙酸和17.4 mM三乙胺组成的洗脱液中,获得了10种酸性化合物的基准分辨率。在最佳分离设置下,色谱柱对色谱柱和批次与批次之间重复性的分辨率参数中的相对标准偏差值小于2.7%(n = 3),这表明ZHM色谱柱的稳定性和柱制备方法的重现性是可以接受的。

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