酯化苯乙烯-马来酸共聚物改性二氧化硅作为混合模式聚合物刷固定相用于色谱分离。
Esterified styrene-maleic acid copolymer modified silica as mixed-mode polymer-brush stationary phases for chromatographic separation.
发表日期:2024 Aug 05
作者:
Yibo Yan, Ruilin Yang, Yanan Wang, Yinan Wu, Xiaofei Gu, Xiaoqiang Qiao
来源:
JOURNAL OF CHROMATOGRAPHY A
摘要:
苯乙烯-马来酸(SMA)共聚物因其优异的增溶特性而备受关注。在这项工作中,首次开发和开发了基于SMA共聚物刷的色谱固定相。首先,通过活性/受控可逆加成断裂链转移(RAFT)聚合方法,在球形二氧化硅表面原位生长SMA共聚物刷。随后,作为概念验证演示,该共聚物分别用二甘醇单-2-乙基己基醚 (DGME) 和 2-(2-乙基己氧基) 乙醇 (EHOE) 进行酯化。分别通过透射电子显微镜、傅里叶变换红外光谱仪、X射线光电子能谱和热重分析对所得Sil-SMA-DGME和Sil-SMA-EHOE共聚物刷色谱固定相进行了表征。色谱保留机制表明,两种填充柱均表现出亲水/反向混合模式保留模式。最大柱效可达71,000 N/m。色谱分离性能评价表明,新型固定相对亲水性、疏水性化合物和磷脂标准品具有优异的分离能力。此外,结合质谱鉴定,Sil-SMA-DGME柱进一步用于人肺癌细胞中磷脂的分离和鉴定。总共成功鉴定出9类186种磷脂。研究结果展示了新型SMA共聚物刷色谱固定相的良好应用前景。版权所有©2024 Elsevier B.V.保留所有权利。
Styrene-maleic acid (SMA) copolymer has received much attention for its excellent solubilization characteristics. In this work, SMA copolymer brush-based chromatographic stationary phases were exploited and developed for the first time. First, SMA copolymer brush was in situ grown on the surface of spherical silica via living/controlled reversible addition-fragmentation chain transfer (RAFT) polymerization method. Subsequently, as a proof-of-concept demonstration, the copolymer was esterified by diethylene glycol mono-2-ethylhexyl ether (DGME) and 2-(2-ethylhexyloxy) ethanol (EHOE), respectively. The obtained Sil-SMA-DGME and Sil-SMA-EHOE copolymer-brush chromatographic stationary phases were characterized by transmission electron microscopy, Fourier transform infrared spectrometer, X-ray photoelectron spectroscopy, and thermogravimetric analysis, respectively. The chromatographic retention mechanism indicated that both the two packed columns exhibited hydrophilic/reverse mixed-mode retention modes. The maximum column efficiency was up to 71,000 N/m. The chromatographic separation performance evaluation indicated that the novel kind of stationary phases had excellent separation capabilities for hydrophilic, hydrophobic compounds and phospholipid standards. In addition, by combination with mass spectrometry identification, the Sil-SMA-DGME column was further exploited for separation and identification of phospholipids in human lung cancer cells. Totally, 9 classes including 186 phospholipid species were successfully identified. The results demonstrated the promising application prospects of the novel kind of SMA copolymer-brush chromatographic stationary phases.Copyright © 2024 Elsevier B.V. All rights reserved.