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An analytical procedure for the qualitative and quantitative analysis of human lens tissue for polyol and aldose content is described. Profile samples are obtained by direct derivatization of lyophilized lenses. The components are analyzed as per-O-acetylpolyols (from the polyols) and per-O-acetylaldononitriles (from the aldoses). This procedure converts each component into a single derivative and terminal dissymmetry for each aldose is retained. The derivatives form in quantitative yield, give good chromatographic peaks, are thermally stable and readily volatilized. They are not subject to adsorption on gas chromatographic columns and are suitable for both qualitative and quantitative analytical studies. Six non-cataractous lenses and fourteen lenses from patients with senile cataract (in seven instances complicated by diabetic pathology) were analyzed. Thermostable borosilicate glass open-tubular capillary columns, coated with the nonpolar phase SE-30, and containing dispersed particles of silanized silicic acid, were used for the gas chromatographic separations. The results are discussed in relation to what is known from earlier studies of human and animal cataracts. A gas chromatographic method for determining the polyol and aldose excretion levels of controlled diabetics is also reported along with a typical metabolic profile.