Supercritical fluid chromatography for milligram preparation of enantiomers.

IF 1.8 4区 医学 Q4 BIOCHEMICAL RESEARCH METHODS Biomedical Chromatography Pub Date : 2024-11-06 DOI:10.1002/bmc.6030
Naomi Knavs, Alina Ghinet, Emmanuelle Lipka
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Abstract

Preparative chromatographic enantioseparation is now the preferred technique for obtaining milligram quantities of pure enantiomers in the initial phase of development of a therapeutic compound. Supercritical fluid chromatography offers several advantages over liquid chromatography and was therefore selected for the preparative enantioseparation of a new potential anti-inflammatory molecule. Approximately 10 mg of each of the two enantiomers was successfully prepared using a Chiralpak AD-H (tris-3,5-dimethylphenylcarbamate of amylose) polysaccharide-based stationary phase with 40% of ethanol as a co-solvent, using a stacked injection mode. A peak distortion was observed during volume overloading, which may be due to the mixed-stream injection method.

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超临界流体色谱法制备毫克级对映体。
制备色谱法对映体分离是目前在治疗化合物研发初期获得毫克级纯对映体的首选技术。与液相色谱法相比,超临界流体色谱法具有多项优势,因此被选为一种潜在抗炎新分子的制备对映体分离技术。使用 Chiralpak AD-H(淀粉的三-3,5-二甲基苯基氨基甲酸酯)多糖基固定相,以 40% 的乙醇作为辅助溶剂,采用叠加进样模式,成功制备出两种对映体各约 10 毫克。在体积过载时观察到峰值变形,这可能是混流进样方法造成的。
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来源期刊
Biomedical Chromatography
Biomedical Chromatography 生物-分析化学
CiteScore
3.60
自引率
5.60%
发文量
268
审稿时长
2.3 months
期刊介绍: Biomedical Chromatography is devoted to the publication of original papers on the applications of chromatography and allied techniques in the biological and medical sciences. Research papers and review articles cover the methods and techniques relevant to the separation, identification and determination of substances in biochemistry, biotechnology, molecular biology, cell biology, clinical chemistry, pharmacology and related disciplines. These include the analysis of body fluids, cells and tissues, purification of biologically important compounds, pharmaco-kinetics and sequencing methods using HPLC, GC, HPLC-MS, TLC, paper chromatography, affinity chromatography, gel filtration, electrophoresis and related techniques.
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