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Objective: Inductively coupled plasma atomic emission spectroscopy (ICP/AES) has been used for the determination of phosphine residues in cereal and tissue biological samples. Methods: The method used is based on the reaction of phosphine residue with H2SO4 in a headspace vial, determining the phosphor of the liberated phosphine gas by ICP/AES at 213.6 nm. At this wavelength, there is a linear relationship between emission and concentration of phosphine in the range of 0.10 up to 0.50 μg g-1 (R2 = 0.990). The method is rapid and sensitive with the detection limit of 3.1 μg (S/N =3), and the precision expressed as relative standard deviations (RSD %) is below 12% for 10 replicates. Results: The obtained results showed good agreement with the GC/NPD method. Conclusion: In this study, we develop a rapid analysis, inexpensive, easier handling, simple, repeatable, and sensitive method for the determination of phosphine residue in various samples.