title: Preparation of phosphorylcholine-based hydrophilic monolithic column and application for analysis of drug-related impurities with capillary electrochromatography.
abstract: A hydrophilic monolithic CEC column was prepared by thermal copolymerization of zwitterionic monomer 2-methacryloyloxyethyl phosphorylcholine (MPC), pentaerythritol triacrylate (PETA), either methacrylatoethyl trimethyl ammonium chloride (META) or sodium 2-methylpropene-1-sulfonate (MPS) in a polar binary porogen consisting of methanol and THF. A typical hydrophilic interaction LC retention mechanism was observed for low-molecular weight polar compounds including amides, nucleotides, and nucleosides in the separation mode of hydrophilic interaction CEC, when high content of ACN (>60%) was used as the mobile phase. The effect of the electrostatic interaction between the analytes and the stationary phase was found to be negligible. The poly(MPC-co-PETA-co-META or MPS) monolithic columns have an average column efficiency of 40 000 plates/m and displayed with a satisfactory repeatability in terms of migration time and peak areas. Finally, the column was successfully applied to determine the impurities of a positively charged drug pramipexole which are often separated by ion pair RP chromatography due to their high hydrophilicity. All four components can be baseline separated within 5 min with BGE consisting of ACN/20 mM ammonium formate buffer (pH 3.0; 80/20).
authors.affiliation: State Key Laboratory of Bioorganic and Natural Products Chemistry, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, P. R. China.
authors.forename: Danye
authors.initials: D
authors.lastname: Qiu
authors.affiliation: State Key Laboratory of Bioorganic and Natural Products Chemistry, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, P. R. China.
authors.forename: Feng
authors.initials: F
authors.lastname: Li
authors.affiliation: State Key Laboratory of Bioorganic and Natural Products Chemistry, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, P. R. China.
authors.forename: Mingyu
authors.initials: M
authors.lastname: Zhang
authors.affiliation: State Key Laboratory of Bioorganic and Natural Products Chemistry, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, P. R. China.|School of Physical Science and Technology, ShanghaiTech University, Shanghai, P. R. China.
authors.forename: Jingwu
authors.initials: J
authors.lastname: Kang
mesh_terms: D052160:Benzothiazoles / Q000302:isolation & purification; D053801:Capillary Electrochromatography / Q000295:instrumentation* / Q000379:methods; D004340:Drug Contamination; D057927:Hydrophobic and Hydrophilic Interactions; D010767:Phosphorylcholine; D000077487:Pramipexole
chemical_list: D052160:Benzothiazoles; D010767:Phosphorylcholine; D000077487:Pramipexole
keywords: Hydrophilic interaction capillary electrochromatography; Impurity analysis; Pramipexole; Zwitterionic monolithic column