Abstract: The residual solvent,1,2-dichloroethane in a tanning preventive,2-hydroxy-4-methoxy-benzophenone-5-sulfonic acid (also known as benzophenone-4) was determined by GC-MS,with head-space solid phase micro-extraction (HS-SPME) and SIS mode. Copolymer of ethylene glycol and divinylbenzene (CW/DVB) was used as extracting fiber in SPME and method of standard addition as well as calculation by extrapolation were applied to eliminate the matrix effect. Linear relationship between values of peak area and mass fraction (w) of 1,2-dichloroethane was obtained in the range of 2.5 to 250 μg·g-1,and detection limit (3S/N) found for the method was 0.06 μg·g-1. Test for recovery was performed by analyzing a known sample for 5 determinations by the proposed method,values of recovery found were range from 99.0%-107.7%. Precision of the method was also tested,and the value of RSD (n=5) obtained was 7.84%.