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High-Sensitivity Detection of 4-(3-Pyridinylmethylamino-carboxypropyl) Phenylthiohydantoins by Capillary Liquid Chromatography–Microelectrospray Ion Trap Mass Spectrometry

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Abstract

We describe the separation and detection at the low-femtomole level of 4-(3-pyridinylmethylaminocarboxypropyl) phenylthiohydantoins (311-PTHs) by capillary liquid chromatography–microelectrospray ion trap mass spectrometry. Highest sensitivity was obtained in the multiple-ion monitoring operating mode in which we detected 311-PTHs at the 5-fmol level with a signal-to-noise ratio of approximately 10. We investigated the fragmentation patterns of the isobaric 311-PTH isoleucine and 311-PTH leucine by electrospray ionization ion trap tandem mass spectrometry. The compounds could be differentiated by a fragment ion of mass m/z=366.1 which was specific for the breakdown of 311-PTH leucine, thus allowing for the unambiguous identification of the 311-PTH derivatives of all 20 naturally occurring amino acids by their masses and fragmentation patterns.

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Authors and Affiliations

  1. Department of Molecular Biotechnology, University of Washington, Seattle, Washington, 98195, USA

    Axel Ducret, Edward J. Bures & Ruedi Aebersold

  2. Amgen, Thousand Oaks, California, USA

    Edward J. Bures

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  1. Axel Ducret
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  2. Edward J. Bures
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  3. Ruedi Aebersold
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Ducret, A., Bures, E.J. & Aebersold, R. High-Sensitivity Detection of 4-(3-Pyridinylmethylamino-carboxypropyl) Phenylthiohydantoins by Capillary Liquid Chromatography–Microelectrospray Ion Trap Mass Spectrometry. J Protein Chem 16, 323–328 (1997). https://doi.org/10.1023/A:1026316217581

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  • DOI: https://doi.org/10.1023/A:1026316217581

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