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

Viberg, Peter, Nilsson, Staffan, Skog, Kerstin
Analytical and bioanalytical chemistry 2004 v.378 no.7 pp. 1729-1734
aromatic amines, capillary electrophoresis, carcinogens, cooking, mass spectrometry, mutagenicity, screening, solid phase microextraction, solvents, urine
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.