An indirect method for the determination of trace bound selenomethionine (SeMet) has been developed. SeMet reacts with cyanogen bromide (CNBr) quantitatively in the presence of SnCl2 to form CH3SeCN, and after extraction with CHCl3 is acid-digested to form Se(IV). Selenium(IV) reacts with 4-nitro-o-phenylenediamine reagent to form 5-NO2-piazselenol which is then determined by gas chromatography equipped with electron capture detector. The sensitivity of this method (CNBr-piazselenol-GC method) is 6 ng SeMet/g of sample. Trace-bound SeMet in plants and some biological materials has been successfully determined by this method and its content has been compared with the total selenium in the sample.