Synthesis of a novel multifunctional stationary phase derived from diethanolamine, HILIC/RPLC/WAX mixed-mode HPLC applications, and investigation of the retention mechanism.
Tarık Aral, Meryem Dokdemir, Hayriye Aral, Kübra Tunç, Murat Sunkur, Mehmet Çolak
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引用次数: 0
Abstract
Mixed-mode chromatography is increasingly valued for retaining analytes with diverse polarity and charge by integrating hydrophilic interaction (HILIC), reversed-phase (RPLC), and ion-exchange mechanisms. However, designing stationary phases that are both easy to synthesize and chromatographically versatile remains challenging. This study presents DEA-Mix-SP, a novel silica-based stationary phase functionalized with diethanolamine via [2-(3,4-epoxycyclohexyl)ethyl]trimethoxysilane, offering a simple synthetic route for broad-spectrum separation. Three variants with different ligand densities were characterized by elemental analysis, FTIR, SEM, and BET. The columns showed excellent separation for various analytes: nine nucleobases/nucleosides were resolved within 13 min, achieving up to 35,000 theoretical plates per meter, and eight benzoic acid derivatives were fully separated in 9 min with efficiencies up to 50,000 N/m. Alkylbenzenes, PAHs, Sudan dyes, phenols, and anilines were also effectively separated. Retention mechanisms were studied using quantitative parameters such as logD, logS, and pKa, confirming significant anion-exchange effects. Performance was compared with ACE C18 (RPLC) and aminopropyl (HILIC) columns: DEA-Mix-SP showed superior separation performance in HILIC over the aminopropyl column and better separation of phenols, benzoic acids, and anilines than ACE C18, while achieving comparable results for fully non-polar analytes like alkylbenzenes, Sudan dyes, and PAHs. DEA-Mix-SP thus combines cost-effectiveness and high mixed-mode selectivity, providing reliable separation for analytes with wide polarity and charge ranges, making it a strong option for pharmaceutical, environmental, and food analyses.
期刊介绍:
Analytical and Bioanalytical Chemistry’s mission is the rapid publication of excellent and high-impact research articles on fundamental and applied topics of analytical and bioanalytical measurement science. Its scope is broad, and ranges from novel measurement platforms and their characterization to multidisciplinary approaches that effectively address important scientific problems. The Editors encourage submissions presenting innovative analytical research in concept, instrumentation, methods, and/or applications, including: mass spectrometry, spectroscopy, and electroanalysis; advanced separations; analytical strategies in “-omics” and imaging, bioanalysis, and sampling; miniaturized devices, medical diagnostics, sensors; analytical characterization of nano- and biomaterials; chemometrics and advanced data analysis.