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In-capillary micro solid-phase extraction and capillary electrophoresis separation of heterocyclic aromatic amines with nanospray mass spectrometric detection

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Abstract

A miniaturised technique to analyse and detect heterocyclic aromatic amines (HAs) using micro solid-phase extraction (μSPE) coupled on-line (in-capillary) to capillary electrophoresis (CE) separation with nanospray (nESI) mass spectrometry (MS) detection has been developed. HAs are mutagenic and carcinogenic compounds formed at low levels in protein-rich food during cooking. Due to the low concentrations of HAs and the high complexity of the matrix in which they exist, sensitive and selective analytical methods are required for quantification. μSPE was performed on a packed bed of C18 particles inside the CE capillary, which minimised the dead volume. The on-line coupling of SPE, CE and nESI-MS reduced the time for extraction and identification to less than half an hour, which will allow for screening of several samples per day. The new technique provides short analysis time, low sample and solvent consumption, and HAs in standard solutions were easily detected at 12–17 fmol injections, and in spiked urine samples at 750–810 fmol injections.

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Acknowledgements

The authors wish to thank Thanh Wang for assistance in the CE–UV experiments, and Maria Petersson for valuable discussions on solid-phase extraction. Financial support from the Swedish Council for Forestry and Agricultural Research, The Swedish Cancer Society, The Swedish Research Council (VR), The Crafoord Foundation and The Royal Physiographic Society in Lund is greatly appreciated. This study was also supported by the Commission of the European Communities specific RTD programme “Quality of Life and Management of Living Resources” QLK1-CT99-01197, Heterocyclic Amines in Cooked Foods—Role in Human Health”. It does not necessarily reflect views and in no way anticipates the Commission’s future policy in this area.

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Authors and Affiliations

  1. Division of Applied Nutrition and Food Chemistry, Department of Food Technology, Engineering and Nutrition, Lund University, P.O.B. 124, 22100, Lund, Sweden

    Peter Viberg & Kerstin Skog

  2. Department of Technical Analytical Chemistry, Center for Chemistry and Chemical Engineering, Lund University, P.O.B. 124, 22100, Lund, Sweden

    Staffan Nilsson

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  1. Peter Viberg
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  2. Staffan Nilsson
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  3. Kerstin Skog
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Correspondence to Peter Viberg.

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Viberg, P., Nilsson, S. & Skog, K. In-capillary micro solid-phase extraction and capillary electrophoresis separation of heterocyclic aromatic amines with nanospray mass spectrometric detection. Anal Bioanal Chem 378, 1729–1734 (2004). https://doi.org/10.1007/s00216-003-2480-2

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  • DOI: https://doi.org/10.1007/s00216-003-2480-2

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