Development of a capillary zone electrophoresis method including a factorial design and simplex optimisation for analysis of amphetamine, amphetamine analogues, cocaine, and heroin

Abstract

A capillary zone electrophoresis (CZE) method was developed for the analysis of amphetamine and 13 amphetamine analogues. A full factorial design was used to screen for important design variables (i.e. carrier electrolyte concentration, pH, and separation temperature), and a modified simplex was employed in a final optimisation step. The resolution values of the target compounds were used as responses in the screening and optimisation phases. This approach made it possible to control the effects of the design variables on the separation of the target compounds. The best results were obtained using a 100 mM Tris/phosphate buffer (pH 3.1) at a separation temperature of 10 °C, and the analysis time was 23 min under these conditions. After slight modification, the method also enabled baseline resolution of the most commonly encountered amphetamine derivatives, as well as cocaine and heroin, within 7 min. There was a linear relationship between peak area and concentration for all substances, with correlation coefficients in the range of 0.9975–0.9999. Moreover, the technique was repeatable and exhibited relative standard deviation (R.S.D.) values in the ranges of 0.01–0.11% and 0.54–1.60% for relative migration time and corrected peak area, respectively. Lastly, the method was successfully applied to analyse street samples.