A batch-type chemiluminescence detection cell using a peroxyoxalate system was easily combined with capillary elec-trophoresis equipment; the device was operated without any tedious procedures. Peroxyoxalate reagents and hydrogen peroxide were examined in detail concerning their usage and concentration with the cell. Fluorescence-labeled a -amino acids showed the detection limits of 10–100 nM order (S/N=3), which were approximately 2 or 3 orders of magnitude lower than those obtained with the absorbance. A mixture sample of the labeled a -amino acids was successfully separated and detected.