The invention provides a gas chromatography-mass spectrometry detection method for a methylaniline compound. The method comprises the following steps of: A) extraction of a sample, namely adding an acid into the sample to extract the methylaniline compound into an acid liquor phase, adding alkaline into acid liquor phase extract to regulate pH to be neutral, adding methylene chloride to reextract the methylaniline compound in the neutral extract into the methylene chloride, and performing volume fixing to obtain a sample detection solution; and B) detection of the sample, namely separating the obtained sample detection solution by using a DB-1MS fused silica capillary column, and performing gas chromatography-mass spectrometry detection. The quantitative detection of the methylaniline compound is realized; the method is high in accuracy, low in detection limit, high in extraction efficiency and easy to operate, and can be widely applied to the detection of the methylaniline compound in a crude oil sample, a gasoline sample, a diesel sample and the like; the interference of other compounds in an extraction process can be eliminated; and powerful support can be provided for the environmental performance evaluation and monitoring of the sample.