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用于阴离子交换色谱的微流控离子抑制模块的设计与性能评估

Design and performance evaluation of a microfluidic ion-suppression module for anion-exchange chromatography.

作者信息

Wouters Sam, Wouters Bert, Jespers Sander, Desmet Gert, Eghbali Hamed, Bruggink Cees, Eeltink Sebastiaan

机构信息

Vrije Universiteit Brussel, Department of Chemical Engineering, Pleinlaan 2, B-1050 Brussels, Belgium.

Leiden University Medical Center, Center for Proteomics and Metabolomics, PO box 9600, 2300 RC Leiden, The Netherlands.

出版信息

J Chromatogr A. 2014 Aug 15;1355:253-60. doi: 10.1016/j.chroma.2014.06.025. Epub 2014 Jun 12.

Abstract

A microfluidic membrane suppressor has been constructed to suppress ions of alkaline mobile-phases via an acid-base reaction across a sulfonated poly(tetrafluoroethylene)-based membrane and was evaluated for anion-exchange separations using conductivity detection. The membrane was clamped between two chip substrates, accommodating rectangular microchannels for the eluent and regenerant flow, respectively. Additionally, a clamp-on chip holder has been constructed which allows the alignment and stacking of different chip modules. The response and efficacy of the microfluidic chip suppressor was assessed for a wide range of eluent (KOH) concentrations, using 127 and 183μm thick membranes, while optimizing the flow rate and concentration of the regenerant solution (H2SO4). The optimal operating eluent flow rate was determined at 5μL/min, corresponding to the optimal van-Deemter flow velocity of commercially-available column technology, i.e. a 0.4mm i.d.×250mm long column packed with 7.5μm anion-exchange particles. When equilibrated at 10mM KOH, a 99% decrease in conductivity signal could be obtained within 5min when applying 10mM H2SO4 regenerant at 75μL/min. A background signal as low as 1.2μS/cm was obtained, which equals the performance of a commercially-available electrolytic hollow-fiber suppressor. When increasing the temperature of the membrane suppressor from 15 to 20°C, ion suppression was significantly improved allowing the application of 75mM KOH. The applicability of the chip suppressor has been demonstrated with an isocratic baseline separation of a mixture of seven inorganic ions, yielding plate numbers between 5300 and 10,600 and with a gradient separation of a complex ion mixture.

摘要

已构建一种微流控膜抑制器,通过基于磺化聚四氟乙烯的膜上的酸碱反应来抑制碱性流动相的离子,并使用电导检测对阴离子交换分离进行了评估。该膜夹在两个芯片基板之间,分别容纳用于洗脱液和再生液流动的矩形微通道。此外,还构建了一个夹式芯片支架,可实现不同芯片模块的对齐和堆叠。使用127μm和183μm厚的膜,在优化再生液(H2SO4)流速和浓度的同时,评估了微流控芯片抑制器在各种洗脱液(KOH)浓度下的响应和效果。确定最佳操作洗脱液流速为5μL/min,这与市售柱技术的最佳范德姆特流速相对应,即内径0.4mm×长250mm、填充7.5μm阴离子交换颗粒的柱。当在10mM KOH下平衡时,以75μL/min的流速施加10mM H2SO4再生液,5分钟内电导率信号可降低99%。获得了低至1.2μS/cm的背景信号,这与市售电解空心纤维抑制器的性能相当。当将膜抑制器的温度从15°C提高到20°C时,离子抑制得到显著改善,从而可以使用75mM KOH。通过对七种无机离子混合物的等度基线分离以及对复杂离子混合物的梯度分离,证明了芯片抑制器的适用性,分离塔板数在5300至10600之间。

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