Atractylenolide Ⅱ and atractylenolide Ⅲ sulfur-containing derivatives were identified as major characteristic markers of sulfur fumigated CR. With the increase of sulfur-fumigationtime,the content of sulfur dioxide residues was continuously increased,while the content of sulfur-containing derivatives was elevated at the beginning and then reached to a plateau, so there was not necessarily a positive correlation between sulfur dioxide residue and the amount of sulfur derivatives. With the increase of heat-treated time,the content of sulfur dioxide residues was continuously decreased,while the content of sulfur-containing derivatives was decreased first and remained at a high level later. There was no clear correlation between sulfur dioxide residue and sulfur-containing derivatives in different sulfur-fumigated and heat-treating de-sulfur degrees of CR.