A simple and efficient extraction and purification procedure for Deoxynivalenol was developed by means of the immunoaffinity column (IAC-SEP ® DON) as a cleanup tool．Deoxynivalenol content in corn, wheat, oats, barley, rice, and other grains are cleaned up by IAC and determined by HPLC or LC-MS/MS. It is a fast, simple, safe and highly accurate method for quantitatively measuring DON.