A procedure is presented for quantification of Ethyl Carbamate at low μg/L levels in distilled spirits. A 100 μL large volume injection was used followed by orthogonal 2-dimensional GC-MS with heartcutting. The direct large volume injection ensured sufficient availability of analyte without an initial sample preparation step, and the 2D step allowed clean elution of ethyl carbamate and it’s labelled internal standard and compensated for the difficult detection of low mass non-specific ions in a complex matrix. The 2D separation was achieved using the new GERSTEL μFlow- Manager based on metal ferrules for simple connection of the orthogonal columns. The principle and apparatus required for both large volume injection and 2D separation will be described together with results from actual samples.