In order to determine the residual aromatic compounds in electromagnetic shielding textiles, the followed pretreatment parameters should be clear and optimized: the pressure of rotary vacuum evaporator，water-bath vibration shake and the pH value of buffer solution. It is found that, when the pressure of rotary vacuum evaporator is 300 mbar, highest recovery of the aromatic amines and experiment efficiency will be gained. The investigation also points out that with waterbath vibration shaking and the pH value of buffer solution between 5.5 and 6.1 , relatively ideal detection results can be got.