An accurate analytical method was developed to determine amino acids in some biological specimens by GC/MS technique. Stable isotopes provide useful tools for a variety of studies, offering ideal internal standards in quantitative information. Isotopic dilution gas chromatography -mass spectrometry (ID-GC/MS) is the techniques used for quantitative analysis of compounds labeled with stable isotopes. A Trace DSQ Thermo Finnigan quadrupole mass spectrometer coupled with a Trace GC was used. Amino acids were separated on a Rtx-5MS capillary column, 30 m x 0.25 mm, 0.25µm film thickness, using a temperature program from 50 o C, 1 min, 6 o C/min at 100 o C, 4 o C/min at 200 o C, 20 o C/min at 300 o C, (3min). The transfer line temperature was 250 o C, the injector temperature 200 o C and ion source temperature 250 o C; splitter: 10:1. Electron energy was 70eV and emission current, 100µA. The amino acids were purified on a Dowex 50W-W8 exchange resin and were derivatized in a procedure following two steps to obtain trifluoroacetyl butyl esters. The identification of amino acids was obtained by using NIST library but also by using amino acid standards.