School of Biological and Chemical Engineering, NingboTech University, Ningbo 315100, China; College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, China.
Department of Chemistry, Zhejiang University, Xixi Campus, Hangzhou 310028, China.
J Chromatogr A. 2021 Oct 11;1655:462508. doi: 10.1016/j.chroma.2021.462508. Epub 2021 Aug 28.
High hydrophilic anion stationary phases play a crucial role in the separation behavior of ion chromatography. Herein, we report novel polymeric anion exchangers grafted with polyethylene polyamines, including ethylenediamine, diethylenetriamine, triethylenetetramine and tetraethylene pentaamine, via a facile epoxy-amine polymerization method. The anion exchangers were characterized by scanning electron microscopy, thermogravimetry, Fourier transform infrared spectrometry and elemental analysis. The chromatographic performance of the stationary phases was evaluated with the separation of common inorganic anions, organic weak acids and highly polarizable anions. Seven common anions (F, Cl, NO, Br, NO, SO and HPO) can be separated within 18 min by using hydroxide eluent in isocratic mode. By adopting different polyethylene polyamines as hyperbranched units, the four types of new stationary phases displayed high efficiencies and good reproducibility. The columns exhibit large exchange capacities at 76.5-184.8 μmol•column (4.6 × 150 mm, i.d.) with efficiency up to 20293 plate m (Cl). The RSDs of the retention time were less than 0.27% and the RSDs of the efficiency were less than 1.95% by consecutive injections after working for two months. The self-fabricated column was successfully applied to determine the chloride content in exhaled breath condensate.
高亲水性阴离子固定相在离子色谱的分离行为中起着至关重要的作用。本文报道了一种通过简便的环氧-胺聚合方法，将聚乙烯多胺接枝到新型聚合阴离子交换剂上的方法。这些阴离子交换剂通过扫描电子显微镜、热重分析、傅里叶变换红外光谱和元素分析进行了表征。通过分离常见的无机阴离子、有机弱酸和高极化性阴离子来评估固定相的色谱性能。在等度模式下，使用氢氧根洗脱液可以在 18 分钟内分离出七种常见阴离子（F、Cl、NO、Br、NO、SO 和 HPO）。通过采用不同的聚乙烯多胺作为超支化单元，四种新型固定相表现出高效率和良好的重现性。该柱在 76.5-184.8 μmol·柱（4.6×150mm，内径）下具有高达 20293 板 m（Cl）的高交换容量。在连续进样两个月后，保留时间的 RSD 小于 0.27%，效率的 RSD 小于 1.95%。自制柱成功应用于测定呼气冷凝液中的氯含量。
