Simultaneous separation of the enantiomer and impurities is a huge challenge for the quality control of the chiral drug. In this work, mixed-mode chiral ligand exchange stationary phases (CSPs) modified by octyl and sulfhydryl ligands were prepared by vapor deposition and click chemistry methods. Qualitative and quantitative determination of the prepared CSPs were achieved by Fourier transform infrared spectroscopy, solid-state ¹³C CP/MAS NMR, and elemental analysis. The chiral resolution of CSPs was investigated through a comprehensively chromatographic evaluation of various racemates. Besides, the thermodynamic experiment was carried out to elucidate the contribution of hydrophobic ligand to the improvement of chiral recognition and selectivity. Atenolol and its degradation products were analyzed on the synthesized CSPs and compared with the commercial chiral column. A good separation of atenolol enantiomers from its acid and alkaline degradation impurities was simultaneously achieved on the C₈/L-Hypro CSP. This new CSP is expected to have more applications in the quality control of other chiral drugs.

中文翻译：

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在混合模式手性配体交换固定相上同时分离阿替洛尔对映体及其酸/碱降解杂质

同时分离对映异构体和杂质是手性药物质量控制的巨大挑战。在这项工作中，通过气相沉积和点击化学方法制备了由辛基和巯基配体改性的混合模式手性配体交换固定相 (CSP)。通过傅里叶变换红外光谱、固态¹³实现对制备的 CSP 的定性和定量测定C CP/MAS NMR，和元素分析。通过对各种外消旋体的综合色谱评估，研究了 CSP 的手性拆分。此外，还进行了热力学实验以阐明疏水配体对提高手性识别和选择性的贡献。在合成的 CSP 上分析阿替洛尔及其降解产物，并与商业手性柱进行比较。在 C ₈ /L-Hypro CSP上同时实现了阿替洛尔对映体与其酸和碱降解杂质的良好分离。这种新的CSP有望在其他手性药物的质量控制方面有更多的应用。