Gogiashvili Mikheil, Telfah Ahmad, Lambert Jörg, Hergenröder Roland
Leibniz Institut für Analytische Wissenschaften - ISAS e.V., Postfach 101352, 44013, Dortmund, Germany.
Anal Bioanal Chem. 2017 Mar;409(9):2471-2475. doi: 10.1007/s00216-017-0196-y. Epub 2017 Feb 7.
We report on the hyphenation of capillary isotachophoresis (cITP) separations with online nuclear magnetic resonance (NMR) detection using a planar microslot waveguide probe design. While cITP is commonly coupled with a solenoidal microcoil NMR probe, the structural information provided is limited by broad resonances and poor spectral resolution due to the magnetic field created by the separation current. The microslot probe design described herein allows the separation capillary to be oriented parallel to the static magnetic field, B , eliminating the spectral broadening produced by the secondary magnetic field induced by the separation current. This allows high-resolution nuclear magnetic resonance spectra of the charged analytes to be obtained in online mode, whereas conventional solenoidal capillary NMR designs must resort to the stopped flow mode. The potential of the microslot probe for hyphenated electrophoretic separations is demonstrated by performing cITP focusing and online NMR detection of the H NMR spectrum of a system containing spermine and aniline. Graphical Abstract High resolution NMR spectra in flow capillarelectrophoretic separations with microslot NMR probe.
我们报道了使用平面微槽波导探头设计，将毛细管等速电泳（cITP）分离与在线核磁共振（NMR）检测联用的情况。虽然cITP通常与螺线管微线圈NMR探头联用，但由于分离电流产生的磁场，所提供的结构信息受到宽共振和低光谱分辨率的限制。本文所述的微槽探头设计允许分离毛细管平行于静磁场B定向，消除了分离电流感应产生的二次磁场所导致的光谱展宽。这使得能够以在线模式获得带电分析物的高分辨率核磁共振谱，而传统的螺线管毛细管NMR设计必须采用停流模式。通过对含有精胺和苯胺的体系进行cITP聚焦和1H NMR谱的在线NMR检测，证明了微槽探头用于联用电泳分离的潜力。图形摘要：使用微槽NMR探头在流动毛细管电泳分离中获得的高分辨率NMR谱。
