Urinary hippuric acid was analyzed by gas chromatography/mass spectrometry method. A simple and economical derivatization procedure using excessive methanol in acidic condition was adopted to esterify hippuric acid. Quantitative analysis was performed with two internal standards, heptadecanoic acid and hydrocinnamic acid, to evaluate the derivatization procedure as an analytical method. Using the standard addition method, linear and reproducible calibration curves were obtained for both internal standards. Calibration experiment showed that good quantitative result could also be obtained with the calibration curve obtained without urine matrix. Recovery rates for the urine samples were in the range of 95.6~111.4%. Using hydrocinnamic acid as internal standard, analysis time could be reduced.