Spudeit Daniel A, Breitbach Zachary S, Dolzan Maressa D, Micke Gustavo A, Armstrong Daniel W
Department of Chemistry and Biochemistry, University of Texas at Arlington, Arlington, Texas, USA.
Department of Chemistry, Federal University of Santa Catarina, Florianopolis, Brazil.
Chirality. 2015 Nov;27(11):788-94. doi: 10.1002/chir.22526. Epub 2015 Sep 17.
A superficially porous particle (SPP)-based hydroxypropyl-β-cyclodextrin (HPBCD) chiral stationary phase (CSP) was produced and its chromatographic performance was compared to both 5 µm and 3 µm fully porous particle (FPP)-based CSPs. The relative surface coverage of the HPBCD chiral selector on each particle was approximately equal, which resulted in equivalent enantiomeric selectivity (α) values on each phase when constant mobile phase conditions were used. Under such conditions, the SPP column resulted in greatly reduced analysis times and three times greater efficiencies compared to the FPP columns. When higher flow rates were used, efficiency gains per analysis times were five times greater for the SPP column compared to the FPP-based columns. When the mobile phases were altered to give similar analysis times on each column, resolution values were doubled for the SPP column. Finally, the novel SPP based HPBCD column proved to be stable for 500 injections under high flow rate (4.5 mL/min) and high pressure (400 bar) conditions used for an ultrafast (~45 sec) enantiomeric separation.
制备了一种基于表面多孔颗粒（SPP）的羟丙基-β-环糊精（HPBCD）手性固定相（CSP），并将其色谱性能与基于5μm和3μm全多孔颗粒（FPP）的CSP进行了比较。HPBCD手性选择剂在每个颗粒上的相对表面覆盖率大致相等，这使得在使用恒定流动相条件时，每个固定相上的对映体选择性（α）值相当。在这种条件下，与FPP柱相比，SPP柱的分析时间大大缩短，效率提高了三倍。当使用更高的流速时，与基于FPP的柱相比，SPP柱每次分析时间的效率提升是其五倍。当改变流动相以使每个柱上的分析时间相似时，SPP柱的分离度值翻倍。最后，新型基于SPP的HPBCD柱在用于超快速（约45秒）对映体分离的高流速（4.5 mL/min）和高压（400 bar）条件下，经500次进样证明具有稳定性。
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