School of Pharmacy, Southwest Medical University, Luzhou, Sichuan, 646000, China.
School of Pharmacy, Southwest Medical University, Luzhou, Sichuan, 646000, China; School of Nursing, Southwest Medical University, Luzhou, Sichuan, 646000, China.
J Chromatogr A. 2020 Dec 20;1634:461674. doi: 10.1016/j.chroma.2020.461674. Epub 2020 Nov 2.
A novel reversed-phase/hydrophilic interaction/ion-exchange (RPLC/HILIC/IEC) and chiral recognition mixed-mode stationary phase material was synthesized using 3-n-octadecyl-1-vinylimidazolium bromide and 6-(1-allylimidazolium)-cyclodextrin tosylate as functional monomers. After identifications of intermediates and stationary phase materials using nuclear magnetic resonance analysis, Fourier transform infrared spectrometer, element analysis and thermogravimetric analysis, the synthesized Sil-VMBD material was packed into an empty column under high pressure. The mixed-mode retention performance was researched by hydrophobic, hydrophilic and ionic compounds. And the retention mechanism of the multi-mode stationary phase was studied via changing the mobile phase composition and pH value. Moreover, the enantiomers of 1-phenyl-1-propanol, warfarin and styrene oxide were separated rapidly under reverse-phase mode. Fast enantioseparation of ibuprofen and ketoprofen were obtained within 4 min under polar organic mode. The experimental results show that the as-prepared mixed-mode column possesses reversed-phase, hydrophilic and ion-exchange interactions with various analytes, and these interactions also enable the stationary phase with multi-mode and chiral separation abilities.
一种新型反相/亲水作用/离子交换（RPLC/HILIC/IEC）和手性识别混合模式固定相材料，是使用 3-正十八烷基-1-乙烯基咪唑溴盐和 6-（1-烯丙基咪唑）-环糊精对甲苯磺酸盐作为功能单体合成的。通过核磁共振分析、傅里叶变换红外光谱、元素分析和热重分析对中间体和固定相材料进行鉴定后，在高压下将合成的 Sil-VMBD 材料填充到空柱中。通过疏水性、亲水性和离子化合物研究了混合模式保留性能。通过改变流动相组成和 pH 值研究了多模式固定相的保留机制。此外，在反相模式下，1-苯基-1-丙醇、华法林和氧化苯乙烯对映体能够快速分离。在极性有机模式下，布洛芬和酮洛芬能够在 4 分钟内快速实现对映体分离。实验结果表明，所制备的混合模式柱对各种分析物具有反相、亲水和离子交换相互作用，这些相互作用还使固定相具有多模式和手性分离能力。
