A testing method by using gas chromatograph-mass spectrometry has been established, which might be employed to carry out simultaneous analyses of total petroleum hydrocarbons. In addition, quality assurance and quality control (QA/QC) of the analysis method have also been performed. The range of petroleum hydrocarbons determined in the soil by this method covers the range from C8 (C7.6) to C34 (C34.01) for aliphatics (aromatics). Soxhlet extraction and column chromat-ography separation had been taken as the pretreatment. C8 (C7.6), C10 (C10.1), C12 (C11.7), C16 (C15.5), C21 (C20.8) and C34 (C34.01) substitute C8–C10 (C7.6–C10.1), ＞C10–C12 (＞C10.1–C11.7), ＞C12–C16 (＞C11.7–C15.5), ＞C16–C21 (＞C15.5– C20.8) and ＞C21–C34 (＞C20.8–C34.01) , respectively for quantitative determination. Using the“substitute”linear relationship calculate each segment fractions’ concentration，then integrate all the peak areas from C8 to C34. The results of linear relationship and precision test of aliphatic petroleum hydrocarbon in this method demonstrate the correlation coefficient (0.990 3 to 0.999 8), the method detection limits (MDLs) (0.011 to 0.373 ng/μl), recovery rates (50.3% to 109.3%) and relative standard deviation (1.5% to 11.3%); and those of aromatic petroleum hydrocarbon in this method are the correlation coefficient (0.991 3 to 0.997 6), the method detection limits (MDLs) (0.004 to 0.048 ng/μl), recovery rates (53.6% to 107.7%) and relative standard deviation (3.2% to 12.2%). The test results of the method could accurately reflect the degree of soil contamination and toxicity.