Abstract: Today, DDVP is still commonly encountered by forensic toxicologists in China. In this paper, the possibility by HS-GC to determine DDVP in blood has been investigated, the method given allows simple and rapid procedure, excellent linearity in the range of 0.2-22ug/ml blood with requal to 0.998, and a detection limit 0.2ug/ml blood. The results from HS-GC were confirmed by those from conventional GC.