Hydrophilic interaction chromatography separation mechanisms of tetracyclines on amino-bonded silica column.

Hydrophilic interaction chromatography separation mechanisms of tetracyclines on amino-bonded silica column.
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DOI:
10.1002/jssc.201100130
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发表时间:
2011-07
影响因子:
3.1
通讯作者:
Rui-ping Li;Yi Zhang;Charles C. Lee;Liming Liu;Yingping Huang
Rui-ping Li;Yi Zhang;Charles C. Lee;Liming Liu;Yingping Huang
中科院分区:
工程技术3区
文献类型:
--
作者:
Rui-ping Li;Yi Zhang;Charles C. Lee;Liming Liu;Yingping Huang

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研究了亲水作用色谱(HILIC)中流动相变化对土霉素、强力霉素、金霉素和四环素4种两性离子四环素类抗生素(TC)分离的影响。提出了氨基HILIC保留过程的混合模式保留机理,包括分配、吸附和离子交换作用。缓冲液类型和pH值显着影响保留的TC,但测试的分析物显示出类似的分离选择性。不同缓冲盐浓度和pH值的实验证明了TC保留中存在离子交换相互作用。有机改性剂的类型和浓度也影响了分析物的保留和选择性,为HILIC的Alpert保留模型提供了直接证据。分析物的保留时间按以下顺序增加:四氢呋喃<甲醇<异丙醇<乙腈。在移动的相中,logk'与%水(v/v)曲线和logk'与%水(v/v)对数的线性关系表明,TC在氨基相中的分离受分配和吸附控制。所开发的方法被成功地利用在河水和废水样品中使用固相萃取(SPE)的样品净化检测的TC。
Effects of mobile-phase variations on the chromatographic separation on amino-bonded silica column in hydrophilic interaction chromatography (HILIC) were investigated for four zwitterionic tetracyclines (TCs): oxytetracycline, doxycycline, chlortetracycline, and tetracycline. A mixed-mode retention mechanism composed of partitioning, adsorption, and ion exchange interactions was proposed for the amino HILIC retention process. Buffer type and pH significantly influenced the retention of TCs, but showed similar separation selectivity for the tested analytes. Experiments varying buffer salt concentration and pH demonstrated the presence of ion exchange interactions in TCs retention. The type and concentration of organic modifier also affected the retention and selectivity of the analytes, providing direct evidence supporting the Alpert retention model for HILIC. The retention time of the analytes increased in the following order of organic modifiers: tetrahydrofuran < methanol < isopropanol < acetonitrile. The linear relationships of logk' versus %water (v/v) curve and logk' versus logarithm of %water (v/v) in the mobile phase indicated that TCs separation on the amino phase was controlled by partitioning and adsorption. The developed method was successfully utilized in the detection of TCs in both river water and wastewater samples using solid-phase extraction (SPE) for sample cleanup.