College of Pharmaceutical Sciences, Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Hebei University, Baoding 071002, China.
College of Urban and Rural Construction, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2024 Sep 13;1732:465227. doi: 10.1016/j.chroma.2024.465227. Epub 2024 Aug 5.
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.
苯乙烯-马来酸酐（SMA）共聚物因其优异的溶解特性而受到广泛关注。本工作首次开发了 SMA 共聚物刷基色谱固定相。首先，通过活性/可控可逆加成-断裂链转移（RAFT）聚合方法将 SMA 共聚物刷原位生长在球形硅胶表面上。随后，作为概念验证的演示，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）对共聚物进行酯化。通过透射电子显微镜、傅里叶变换红外光谱、X 射线光电子能谱和热重分析分别对 Sil-SMA-DGME 和 Sil-SMA-EHOE 共聚物刷色谱固定相进行了表征。色谱保留机理表明，两个填充柱均表现出亲水/反相混合模式保留模式。最大柱效高达 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，通过与质谱鉴定相结合，Sil-SMA-DGME 柱进一步用于分离和鉴定人肺癌细胞中的磷脂。总共成功鉴定了 9 类，包括 186 种磷脂。结果表明，新型 SMA 共聚物刷色谱固定相具有广阔的应用前景。
