A gas chromatographic assay for spectinomycin hydrochloride is described. The method is based on that prescribed by the United States Pharmacopeia (USP XXII). The method involves silylation of spectinomycin hydrochloride; phenazone is used as an internal standard. Spectinomycin and phenazone have adequate stability under the prescribed conditions. The stationary phase is 3 % OV-17 on Gaschrom Q 100-120 mesh. The selectivity of the proposed method is better than that of the GLC method described in the USP XXII.