title: Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.
abstract: A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase.
authors.affiliation: Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030, China.
authors.forename: Qing
authors.initials: Q
authors.lastname: Wang
authors.affiliation: Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030, China.
authors.forename: Yao
authors.initials: Y
authors.lastname: Long
authors.affiliation: Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030, China.
authors.forename: Lin
authors.initials: L
authors.lastname: Yao
authors.affiliation: Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030, China.
authors.forename: Li
authors.initials: L
authors.lastname: Xu
authors.affiliation: Department of Chemistry, Wuhan University, Wuhan 430072, China. Electronic address: shizg@whu.edu.cn.
authors.forename: Zhi-Guo
authors.initials: ZG
authors.lastname: Shi
authors.affiliation: Hubei Key Laboratory for Processing and Application of Catalytic Materials, Huanggang Normal University, Huangzhou 438000, China.
authors.forename: Lanying
authors.initials: L
authors.lastname: Xu
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000470:Alkaloids / Q000032:analysis; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis; D002021:Buffers; D002264:Carboxylic Acids / Q000032:analysis; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D004229:Dithiothreitol / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis; D012822:Silicon Dioxide / Q000737:chemistry*; D013696:Temperature
chemical_list: D000097:Acetonitriles; D000470:Alkaloids; D000894:Anti-Inflammatory Agents, Non-Steroidal; D002021:Buffers; D002264:Carboxylic Acids; D011084:Polycyclic Aromatic Hydrocarbons; D012822:Silicon Dioxide; D004229:Dithiothreitol; C032159:acetonitrile
keywords: Click chemistry; Hydrophilic interaction chromatography; Mixed-mode chromatography; Reversed phase liquid chromatography