A sample preparation method for gas chromatography using a two-phase, laminar flow extraction PDMS/glass chip has been developed. A stable two-phase laminar interface was obtained by surface modification, and the organic extraction phase and the aqueous sample phase were separated effectively when the two-phase laminar flows exit the chip. Experiments were conducted on the chip to extract ephedrine from aqueous solution. Good reproducibility was obtained over the entire range of ephedrine concentration using the extraction chips (CV range 2.7%-4.5%). Effects of salt and solvent on extraction efficiency were studied.