[Preparation of an anion stationary phase modified by quaternary ammoniated allyl glycidyl ether]. 2022

Zongying Li, and Xin Chen, and Feifang Zhang, and Bingcheng Yang
School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China.

A polymer-based strong anion stationary phase modified by quaternary ammoniated allyl glycidyl ether (AGE) for ion chromatography (IC) was developed. It was prepared by surface copolymerization between AGE and the pedant double bonds associated with hydrolyzed poly(glycidylmethacrylate-divinylbenzene) (GMA-DVB) substrate, followed by quaternization with N,N-methyldiethanolamine (a tertiary amine, MDEA). The synthesis conditions were optimized, including the type of organic tertiary amines (MDEA, N,N-dimethylethanolamine, trimethylamine), substrate hydrolysis, the amount of monomer and initiator, reaction temperature and reaction time. The obtained anion stationary phase was characterized by scanning electron microscope and elemental analysis. MDEA was observed to be the best quaternization reagent since the anion exchanger obtained by such reagent showed good separation and suitable retention time towards model inorganic anions. The resulting reason probably lies in higher hydrophilicity of MDEA relative the other two ones. The use of rich epoxy groups of GMA-DVB to introduce the functional groups was commonly used in many previous reports. Here the epoxy groups were firstly hydrolyzed to be diol groups and the pendant double bonds onto the surface of GMA-DVB particles were used to graft AGE. The data achieved indicated that the use of hydrolyzed GMA-DVB substrate would be helpful to reduce anion exchange capacity and unwanted non-ion exchange interaction, in which the rich epoxy groups were converted to hydroxy groups. More important, the obtained anion exchanger after hydrolytic treatment could offer a significantly reduction of retention time (~68%) and a ~1.67-fold higher plate count (take Br- as an example). The apparent capacity of the phase was computed to be 264 μmol/g by content of N data and its effective capacity was measured to be 98.5 μmol/column by the breakthrough curve method. Under the optimal chromatographic conditions, the obtained stationary phase showed baseline separation of seven common inorganic anions in less than 13 min using carbonate-bicarbonate mixed eluent, exhibiting high separation efficiency and peak shape, e. g. 49000 plate/m and 38000 plate/m of the theoretical plate counts respectively for chloride and nitrate, and their asymmetric factor were 1.3 and 1.4. These can be comparable or slightly higher than those of commercial columns. The fitted equation of the eluent concentration and the retention factors of model anions was proved that ion exchange model dominates the retention mechanism of the anion stationary phase. This offers a simple way to prepare anion exchanger and to manipulate anion exchange capacity. The utility of the obtained anion exchanger has been demonstrated to the analysis of tap water.

UI MeSH Term Description Entries
D002852 Chromatography, Ion Exchange Separation technique in which the stationary phase consists of ion exchange resins. The resins contain loosely held small ions that easily exchange places with other small ions of like charge present in solutions washed over the resins. Chromatography, Ion-Exchange,Ion-Exchange Chromatography,Chromatographies, Ion Exchange,Chromatographies, Ion-Exchange,Ion Exchange Chromatographies,Ion Exchange Chromatography,Ion-Exchange Chromatographies
D004852 Epoxy Compounds Organic compounds that include a cyclic ether with three ring atoms in their structure. They are commonly used as precursors for POLYMERS such as EPOXY RESINS. Epoxide,Epoxides,Epoxy Compound,Oxiranes,Compound, Epoxy,Compounds, Epoxy
D000838 Anions Negatively charged atoms, radicals or groups of atoms which travel to the anode or positive pole during electrolysis. Anion
D057927 Hydrophobic and Hydrophilic Interactions The thermodynamic interaction between a substance and WATER. Hydrophilic Interactions,Hydrophilic and Hydrophobic Interactions,Hydrophilicity,Hydrophobic Interactions,Hydrophobicity,Hydrophilic Interaction,Hydrophilicities,Hydrophobic Interaction,Hydrophobicities,Interaction, Hydrophilic,Interaction, Hydrophobic,Interactions, Hydrophilic,Interactions, Hydrophobic

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