In the present study, a new method using microwave-assisted solvent extraction (MASE) technique followed directly GC analysis was developed for the extraction of volatile organic acids (VOAs) in tobacco. The MASE conditions (heating time, volume of extracting solvent and extraction temperature) were optimized by means of an orthogonal array design (OAD) procedure. The results suggested that extractant, temperature and heating time were statistically the most significant factors. The extracts were directly analyzed with capillary GC operating in splitless-injection mode on an Agilent HP-FFAP capillary column. Under optimum operating conditions, MASE showed significantly better recoveries than those obtained by the conventional extraction method (ultrasonic and reflux extraction), ranging from 90.6% to 103.2%. In addition, a drastic reduction of the extraction time (20 min versus 4h) and solvent consumption (20 mL versus 100 mL) was achieved with an outstanding reproducibility (CV < or =5%).