College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin, P. R. China.
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Science, Chinese Academy of Sciences, Beijing, P. R. China.
J Sep Sci. 2020 Jul;43(14):2743-2749. doi: 10.1002/jssc.202000234. Epub 2020 May 5.
A method of reversed-phase ion-pair solid-phase extraction combined with ion chromatography for determination of pyrrolidinium ionic liquid cations (N-methyl-N-ethyl pyrrolidinium, N-methyl-N-propyl pyrrolidinium, and N-methyl-N-butyl pyrrolidinium) in water samples was developed in this study. First, ion-pair reagent sodium heptanesulfonate was added to the water samples after static, centrifugation and filteration. Then, pyrrolidinium cations in the samples were enriched and purified by a reversed-phase solid-phase extraction column, and eluted from the column with methanol aqueous solution as eluent. Finally, the eluate collected was analyzed by ion chromatography. The separation and direct conductivity detection of these pyrrolidinium cations by ion-exchange column using 1.0 mM methanesulfonic acid (in water)/acetonitrile (97:3, v:v) as mobile phase was achieved within 10 min. By using this method, pyrrolidinium cations in Songhua River and Hulan River were successfully extracted with the recoveries ranging from 74.2 to 97.1% and the enrichment factor assessed as 60. Pyrrolidinium cations with the concentration of 0.001-0.03 mg/L can be enriched and detected in the water samples. The developed method for the determination of pyrrolidinium ionic liquid cations in water samples is simple and reliable, which provides a reference for the study of the potential impact of ionic liquids on the environment.
本研究建立了一种反相离子对固相萃取-离子色谱法测定水样中吡咯烷离子液体阳离子(N-甲基-N-乙基吡咯烷、N-甲基-N-丙基吡咯烷和 N-甲基-N-丁基吡咯烷)的方法。首先,将离子对试剂庚烷磺酸钠加入到水样中,然后进行静态、离心和过滤。然后,通过反相固相萃取柱对样品中的吡咯烷阳离子进行富集和纯化,用甲醇水溶液作为洗脱液从柱上洗脱。最后,收集洗脱液进行离子色谱分析。这些吡咯烷阳离子在离子交换柱上,以 1.0mM 甲烷磺酸(水中)/乙腈(97:3,v:v)为流动相,在 10min 内实现了分离和直接电导率检测。采用该方法,成功地从松花江和呼兰河水中提取了吡咯烷阳离子,回收率在 74.2%至 97.1%之间,富集因子评估为 60。水样中浓度为 0.001-0.03mg/L 的吡咯烷阳离子可以被富集和检测。该方法简单可靠,为研究离子液体对环境的潜在影响提供了参考。