Antioxidants, both synthetic and of natural origin, are widely applied to prevent the oxidative degradation of processed foods. Propyl gallate and butylated hydroxyanisole, as synthetic phenolic antioxidants, display high chemical activity for suppressing chain initiation, or breaking chain propagation of the peroxidation of unsaturated fatty acids. 1 Their molecular structures are shown in Fig. 1. Although they are powerful for protecting product quality in food distribution, excess antioxidants added to food might produce toxicities or mutagenicities, and thus harm the health of people. In most countries, the contents of phenolic antioxidants in processed food are strictly limited. Thus, the development of new analytical techniques for the fast determination of those antioxidants in food science has seen a huge recent increase as the result of an increased concern of consumers about food safety. 3 In general, the combination of two synthetic antioxidants is more effective than a single antioxidant used for food samples. Thus, difficulties have been encountered in the determination and separation of antioxidants due to a chemical similarity of the analytes, 4-6 which have resulted in mutual interference. Several detection methods without previous separation have been studied. With the aid of chemometrics approaches, the electroanalytical-voltammetric technique 1 and spectrophotometry 2 were employed to analyze antioxidants. Based on a joining of the stopped-flow mixing technique and a diode-array detector, photometric methodology was used for the simultaneous determination of BHA and PG. 7,8 Also, a continuous-flow injection means was described for the determination of two binary mixtures of the antioxidants in foods and cosmetics. Although many approaches for the analysis of PG and BHA reported above seem to be relatively simple, complicated calculations and a large volume sample requirement were the main problems concerning the detection process. Thus, the development of a faster, cleaner and simpler analytical procedure for the simultaneous determination of BHA and PG in food samples is very necessary in order to meet the demand Capillary electrophoretic separation coupled with end-column amperometric detection for the simultaneous quantification of butylated hydroxyanisole (BHA) and propyl gallate (PG) in food was developed. Important factors affecting separation and detection, such as the running buffer, separation voltage, and detection potential, were investigated in detail. An improved working electrode preparation method was used, where a carbon disk of 33 μm in diameter was sealed in a tip and positioned opposite the outlet of a capillary. The experiments indicated that the preparation method was simple, and the obtained electrode exhibited good flexibility and stability for the determination of phenolic antioxidants. The separation was carried out within 5 min using a 50 cm length capillary, with a solution containing 5 mM phosphate and 5 mM borax of pH 8.84 as a separation buffer, and a separation p...