In-capillary micro solid-phase extraction and capillary electrophoresis separation of heterocyclic aromatic amines...

A miniaturised technique to analyse and detect heterocyclic aromatic amines (HAs) using micro solid-phase extraction ( microSPE) 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. microSPE was performed on a packed bed of C(18 )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.