A rapid sequence of oxidation and iodination using 2-iodosobenzoate as an oxidizing agent and N,N-dimethylaniline as an iodine scavenger at pH 6.4, when 4-iodo-N,N-dimethylaniline is formed, has been used for the determination of iodide by GC-MS. Solid phase microextraction (SPME) and single drop microextraction (SDME) have been used for the extraction of the iodo-derivative and their relative efficiencies compared. Pharmaceutical samples were subjected to solid phase extraction (SPE) for cleanup and the eluate analyzed for iodide. Iodate in salt samples was reduced to iodide with ascorbic acid. Milk powder and dried vegetables were wet combusted with peroxydisulfate to liberate covalently bound iodine as iodate which was reduced before derivatization. A rectilinear calibration graph was obtained for 0.1 microg-10 mg l(-1) iodide by both extraction methods, the correlation coefficient and limit of detection (LOD) were 0.9995 and 25 ng l(-1) iodide by SPME method, and 0.9998 and 10 ng l(-1) iodide by SDME method, respectively. SDME appeared to be more efficient technique than SPME for the present system. From the pooled data, the average recovery of spiked iodide to real samples was 100.7% (range 96.5-107.0%) with an average R.S.D. of 3.1% (range 2.6-4.5%).