This study was aimed to develop a quick detection method to test aldehydes and ketones in textiles in order to control the quality of automotive textiles in the development process from fabric production to end-use in vehicles. In this study, a pretreatment of samples was applied to simulate the actual environment of textiles used in vehicles. Collected volatiles were reacted with 2,4-dinitrophenylhydrazine and then eluted with acetonitrile tetrahydrofuran. The eluent was analyzed with high-performance liquid chromatography. Findings showed more than 90% volatiles could be detected in the established method; the lowest determination limit was 0.0297 mg/mL; and the lowest quantification limit was 0.0991 mg/mL, which meant sensitivity and capability of the method were high. Regression coefficients of linear models between volatile concentrations and chromatographic peak characteristics were >0.995, indicating that the method could effectively and efficiently determine the contents of volatiles in automotive textiles.