Abstract: 1.000 g of the cut textile sample was ultrasoni-extracted with 10.0 mL of toluene at normal temperature for 60 min. An aliquot of the extract was taken with an injector and filtered through 0.45 μm PTCE filtering membrane, and the filtrate was used for gas chromatography-mass spectrometry analysis under the instrumental working condition. DB-5MS chromatographic column (30 m×0.25 mm, 0.25 μm) was used as the separation column on which quinoline and isoquinoline were well separated by passing the filtrate through it with the column temperature raising at a rate of 12℃·min^-1 from 80℃ to 220℃. EI and identifying be whole scanning, quantifying by selected ion scanning were adopted in MS determination. Linear relationships between values of peak areas found and the respective mass concentrations of quinoline and isoquinoline were obtained in the range of 10.0-250.0 μg·L^-1. The detection limits found for the 2 compounds were same as 0.1 mg·kg^-1. Tests for recovery were made by addition of standard solutions at 3 concentration levels to blank samples and analyzed by the proposed method. Values of recovery in the range of 82.9%-92.0% and 85.5%-98.1% were found for the 2 compounds respectively. Average values of RSDs (n=6) found were 2.5% and 3.1% respectively. 22 samples of textiles were analyzed by the present method, and 5 samples were found to contain quinoline and isoquinoline in the mass fraction range of 1.2-27.8 mg·kg^-1, which were much lower than the limitation value of 50 mg·kg^-1 as given by the OEKO-TEX^® STANDARD 100, 2019 (50 mg·kg^-1).