Nineteen biogenic D,L-amino acids are derivatized with highly reactive N-fluorenylmethoxycarbonyl-L-alanyl N-carboxyanhydride. Using a 0.5M borate buffer at pH 7.5 and acetone, the derivatization of amino acids is completed in 5 min at room temperature. Some of the resulting diastereomeric N-protected dipeptides are successfully separated on an octylsilica stationary phase using 100mM acetate buffer (pH 4.4) and acetonitrile as the eluent.