OBJECTIVE： To establish a method for simultaneous determination of residual methanol， ethanol， acetonitrile， isopropanol， methylbenzene， tetrahydrofuran and ethyl acetate in Nilethylenol raw material. METHODS： GC was performed. The determination was performed on DB-WAX capillary column. The detector was hydrogen flame ionization detector with split ratio of 5 ∶ 1. The carrier gas was nitrogen （purity： 99.999％） at the flow rate of 1.0 mL/min. The sample size was 1 μL， directly sampling with bonded crosslinked polyethylene glycol as stationary phase. The initial temperature was 40 ℃ and was maintained for 5 min， increased to 90 ℃ at 10 ℃/min， and then increased to 200 ℃ at 5 ℃/min. The temperature of injector was 220 ℃， and detector temperature was 230 ℃. RESULTS： The linear range was 0.24-12.00 μg/mL for methanol （r＝0.999 7）， 0.40-20.00 μg/mL for ethanol （r＝0.999 5）， 0.033-1.64 μg/mL for acetonitrile （r＝0.999 8）， 0.40-20.00 μg/mL for isopropanol （r＝0.999 5）， 0.071-3.56 μg/mL for methylbenzene （r＝0.999 6）， 0.058-2.88 μg/mL for tetrahydrofuran （r＝0.999 8）， 0.40-20.00 μg/mL for ethyl acetate （r＝0.999 7）， respectively. The limits of quantitation were 0.24， 0.40， 0.033， 0.40， 0.071， 0.058， 0.40 μg/mL， respectively. The limits of detection were 0.08， 0.10， 0.01， 0.13， 0.02， 0.02， 0.13 μg/mL， respectively. RSDs of precision， stability and reproducibility tests were all lower than 2％. The recoveries were 98.17％-100.48％ （RSD＝0.92％，n＝9）， 97.77％-101.30％（RSD＝1.32％，n＝9）， 97.56％-100.85％（RSD＝1.20％，n＝9）， 98.64％-100.92％（RSD＝0.87％，n＝9）， 98.54％-100.62％（RSD＝0.76％，n＝9），98.26％-100.00％（RSD＝0.74％，n＝9）， 98.30％-100.59％（RSD＝0.76％，n＝9）， respectively. CONCLUSIONS： The method has high sensitivity and good accuracy， and can be used for the simultaneous determination of residual methanol， ethanol， acetonitrile， isopropane， methylbenzene， tetrahydrofuran and ethyl acetate in Nilethylenol raw material.