亲水单分散聚合物基质强阴离子色谱固定相的制备及应用

Preparation and Application of Strong Anion Exchange Column Based on Hydrophilic Monodisperse Polymer Resins

以自合成6.0μm大孔单分散交联聚甲基丙烯酸环氧丙酯微球为基质,采用化学键合法制备了季铵型强阴离子色谱填料,该填料具有良好的色谱性能。选用6.0 mmol/L Na2CO3＋5.5 mmol/L NaHCO3混合液作淋洗液,在流速为1.0 mL/min下,可以很好地分离常见的6种无机阴离子（F-、Cl-、NO-2、Br-、NO-3、SO2-4）、4种低碳链酸（甲酸、乙酸、一氯乙酸、草酸）以及甲酸、乙酸和一些无机阴离子的混合物。考察了淋洗液种类、pH值和有机溶剂对6种无机阴离子分离的影响。在最佳色谱条件下,6种无机阴离子在一定浓度范围内具有良好的线性关系和低的检出限。采用该方法对本地自来水进行测定,4种离子可在22 min内完全分离,各离子的加标回收率为96.4%～100.6%。

Monodisperse macroporous poly（ glycidylmethacrylate-co-ethylenedimethacrylate）（ PGMA /EDMA） beads were synthesized,and a new kind of strong anion stationary phase was prepared by chemical modification of the PGMA /EDMA beads. This column has a superior separation ability for some inorganic anions（ e. g. F-,Cl-,NO-2,Br-,NO-3and SO2-4） and organic acids（ e. g.methane acid,acetic acid,monochloroacetic acid and oxalic acid） by elution of 6. 0 mmol /L sodium carbonate and 5. 5 mmol /L sodium bicarbonate at a flow rate of 1. 0 mL /min. Moreover,the separation of a mixture of anions and organic acids can also be well obtained at the same chromatographic conditions. The influences of eluent type,pH value and organic solvent on retention of six inorganic anions were studied. Under the optimized chromatorgraphic conditions,the six anions had good linear relationships in the certain concentration range and low detection limits. The column was used in the separation of inorganic anions in running water,and four anions were separated in 22 min. The recoveries of four anions were between 96. 4% and 100. 6%.