Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-11-05 , DOI: 10.1016/j.chroma.2020.461685 Matías E. Díaz Merino , Carlina Lancioni , Juan M. Padró , Cecilia B. Castells
In this study, we describe the experimental variables influencing enantioseparation of twelve β-blockers when analyzed under polar-organic, reversed-phase and hydrophilic interaction liquid chromatography conditions on a column with immobilized amylose tris(3-chloro-5-methylphenylcarbamate) as chiral stationary phase. Regarding polar-organic mode, two component mobile phases consisting of methanol, ethanol or acetonitrile with the addition of basic additives such as diethylamine, triethylamine, mono-ethanolamine, ethylendiamine or trifluoroacetic acid/diethylamine mixture were evaluated. Studies of retention at different temperatures were also performed. In reversed-phase mode, mixtures consisting of methanol or acetonitrile with either aqueous boric acid-borate buffer or sodium hydrogen carbonate-carbonate buffer solutions were compared aiming to study the influence of organic modifier as well as buffer type and pH on resolution. In addition, a systematic evaluation of the retention factors of β-blockers enantiomers in hydro-organic eluents containing acetonitrile in presence of diethylamine as additive was carried out by increasing progressively the water content, in order to check for retention dependencies indicative of the interplay of both hydrophilic interaction liquid chromatography and reversed-phase modes.
中文翻译:
极性-有机,反相和亲水作用液相色谱条件下以直链淀粉三(3-氯-5-甲基苯基氨基甲酸酯)为手性固定相对映体拆分β-阻滞剂的研究
在这项研究中,我们描述了固定化直链淀粉三柱在极性有机,反相和亲水相互作用液相色谱条件下分析时,影响十二种β受体阻滞剂对映体分离的实验变量(3-氯-5-甲基苯基氨基甲酸酯)为手性固定相。关于极性有机模式,评估了由甲醇,乙醇或乙腈组成的两个组分流动相,并添加了碱性添加剂,例如二乙胺,三乙胺,单乙醇胺,乙二胺或三氟乙酸/二乙胺混合物。还研究了在不同温度下的保留率。在反相模式下,比较了由甲醇或乙腈与硼酸硼酸盐水溶液或碳酸氢钠-碳酸氢钠缓冲溶液组成的混合物,旨在研究有机改性剂以及缓冲液类型和pH对分离度的影响。此外,