The aim of this investigation was to develop a quantitative gas-liquid chromatographic method of analysis forhyosyamine and scopolamine, and to apply this method to the analysis of preparations. The trimethylsily(TMS) derivatives of the alkaloids were found to be far superior to the nonsilylating compounds in charomatagrams. Bis(trimethylsilyl) acetamide(BSA) was evaluated and found to be a good reagent for silyation of the alkaloids. The optimum derivatization conditions were heating the alkaloids in a closed tube at $70^{circ)$ for 30 min with a 150 molar excess of BSA to the alkaloids were found to be alkaloids. Calibration curves for the two alkaloids were alkaloid. The standard deviations were 1.1% for hyoscyamine and 1.5% for scopolamine. The minimum detectable amount using the hydrogen flame ionization edtector was determined to be 2$ imes$10$^{-11}$ moles of each alkaloid injected.