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采用磁强化分子印迹整体柱微萃取与非水毛细管电泳联用技术测定水样中的醛类物质。

Determination of aldehydes in water samples by coupling magnetism-reinforced molecular imprinting monolith microextraction and non-aqueous capillary electrophoresis.

机构信息

School of environmental science and engineering, Guangzhou University, Guangzhou 510006, China.

School of environmental science and engineering, Guangzhou University, Guangzhou 510006, China; Guangdong Provincial Key Laboratory of Radionuclides Pollution Control and Resources, Guangzhou 510006, China.

出版信息

J Chromatogr A. 2020 Nov 22;1632:461602. doi: 10.1016/j.chroma.2020.461602. Epub 2020 Oct 10.

Abstract

Excess 2, 4-dinitrophenylhydrazine (2, 4-DNPH) is often applied for the derivatization of aldehyde prior to the chromatographic analysis. However, the residual 2, 4-DNPH may cause background interference and limit the enrichment efficiency of trace aldehydes. To overcome the above bottle-neck problems, improve the extraction efficiency and omit the manipulation for changing the polarity of solvent for the hydrophobic analytes separation, a new method combining magnetism-reinforced in-tube solid phase microextraction (IT-SPME) technique with non-aqueous capillary electrophoresis (NACE) was developed. The monolithic extraction cartridge was prepared in situ inside a capillary and doped with magnetic molecular imprinting polymers (mMIPs). The selective and efficient extraction of the derived analytes with simultaneous removal of the superfluous derivatization agent was achieved owing to the combined effect of molecular imprinting and magnetism reinforcement. By coupling with NACE, the highly hydrophobic effluent can be analyzed directly. The LODs of the method are between 0.00320.0049 mg L and the recoveries are between 87.399.8% for the tested aldehydes. The developed approach is sensitive enough for detection of surface (drinking) water. The aldehydes in real water samples have been detected by this method, showing results that are in good agreement with the standard SPE-HPLC method.

摘要

过量的 2,4-二硝基苯肼(2,4-DNPH)通常用于醛类化合物的衍生化,然后再进行色谱分析。然而,残留的 2,4-DNPH 可能会导致背景干扰,并限制痕量醛类化合物的富集效率。为了克服上述瓶颈问题,提高萃取效率,并省略改变溶剂极性以分离疏水性分析物的操作步骤,我们开发了一种将磁强化管内固相微萃取(IT-SPME)技术与非水毛细管电泳(NACE)相结合的新方法。整体式萃取柱在毛细管内原位制备,并掺杂有磁性分子印迹聚合物(mMIPs)。由于分子印迹和磁强化的联合作用,实现了衍生分析物的选择性和高效萃取,同时去除了多余的衍生化试剂。通过与 NACE 耦合,可以直接分析高度疏水性的流出物。该方法的检出限在 0.00320.0049 mg/L 之间,回收率在 87.399.8%之间,适用于测试的醛类化合物。该方法足够灵敏,可用于检测地表水。通过该方法检测了实际水样中的醛类化合物,结果与标准 SPE-HPLC 方法吻合良好。

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