He Jianfeng, Fan Jun, Yan Yilun, Chen Xiaodong, Wang Tai, Zhang Yaomou, Zhang Weiguang
School of Chemistry and Environment, South China Normal University, Guangzhou, China.
Guangdong YanJie Pharmatech Co. Ltd, Guangzhou, China.
J Sep Sci. 2016 Nov;39(21):4251-4257. doi: 10.1002/jssc.201600820. Epub 2016 Sep 27.
Enantiomeric pairs of triticonazole have been successfully separated by supercritical fluid chromatography coupled with a tris(3,5-dimethylphenylcarbamoyl) cellulose-coated chiral stationary phase in this work. The effects of co-solvent, dissolution solvent, flow rate, backpressure, and column temperature have been studied in detail with respect to retention, selectivity, and resolution of triticonazole. As indicated, the co-solvents mostly affected the retention factors and resolution, due to the different molecular structure and polarity. In addition, the dissolution solvents, namely, chloromethanes and alcohols, have been also important for enantioseparation because of the different interaction with stationary phase. Higher flow rate and backpressure led to faster elution of the triticonazole molecules, and the change of column temperature showed slight effect on the resolution of triticonazole racemate. Moreover, a comparative separation experiment between supercritical fluid chromatography and high performance liquid chromatography revealed that chiral supercritical fluid chromatography gave the 3.5 times value of R /t than high performance liquid chromatography, which demonstrated that supercritical fluid chromatography had much higher separation efficiency.
在本研究中,采用超临界流体色谱法结合涂覆有三(3,5-二甲基苯基氨基甲酰基)纤维素的手性固定相,成功分离了戊唑醇的对映体对。详细研究了共溶剂、溶解溶剂、流速、背压和柱温对戊唑醇保留、选择性和分离度的影响。结果表明,由于分子结构和极性不同,共溶剂对保留因子和分离度影响较大。此外,溶解溶剂(即氯甲烷和醇类)由于与固定相的相互作用不同,对映体分离也很重要。较高的流速和背压导致戊唑醇分子洗脱更快,柱温变化对戊唑醇外消旋体的分离度影响较小。此外,超临界流体色谱与高效液相色谱的对比分离实验表明,手性超临界流体色谱的R/t值是高效液相色谱的3.5倍,这表明超临界流体色谱具有更高的分离效率。