Investigation and application of LC/1H-NMR using semimicro LC and a micro-probe.

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  • セミミクロ液体クロマトグラフィーとマイクロプローブを用いる液体クロマトグラフィー／プロトン核磁気共鳴法の検討と応用
  • セミミクロ エキタイ クロマトグラフィー ト マイクロプローブ オ モチイル

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Abstract

A semimicro LC/1H-NMR was constructed with a 3 mm i.d. micro-probe equipping a glass NMR flow cell of ca. 50μl volume. A semimicro polymer-coated ODS column (1.5 mm i.d. × 250 mm) was used for various studies with a mobile phase of D2O, and deuterated an acetonitrile mixture at a 100μl/min flow rate. Identification and detection limits were determined by a flow-injection mode for ethyl p-hydoroxybenzoate as ca. 5 μg and sub-μg, respectively. A comparison of a UV chromatogram and a protonogram, which was obtained by projecting the on-flow spectrum on the time-axis was made in order to study the state of diffusion of the sample in the NMR flow cell. The results indicated that a separation of adjacent peaks eluted through LC was well maintained in the NMR flow cell. The semimicro system was also applied to a keto-enol tautomeric mixture, which was hardly isolated by a preparative procedure. Each tautomer was identified by the individual spectra of the keto and enol forms, and the usefulness of semimicro LC/1H-NMR has been fully demonstrated.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 47 (11), 845-851, 1998

    The Japan Society for Analytical Chemistry

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