The importance of benzyltriethyl ammonium chloride (BTEAC) in industrial applications has stimulated the development of a number of methods for its determination. In this paper, a high performance capillary electrophoresis (CE) method, coupled with an extraction technique for determining BTEAC in organic matrices, was developed. BTEAC was extracted from organic samples with a 20 mM sodium phosphate solution. Sonication was used to improve extraction efficiency. The repeatability and recovery of the technique have been studied and it was proven that the technique is satisfactory for quantitative determination of BTEAC in organic matrices. Separation was achieved within 6 min in 20 mM sodium phosphate buffer at pH 5.0. The recovery was above 92%. The detection limit for BTEAC is 5 mg L-1 with a signal-to-noise ratio of 3. The linear range of the technique is 5-100 mg L-1. This method is simple, fast, low-cost, and can be easily used for product quality control in industrial laboratories.