Six antihyperlipidemic agents—bezafibrate, ciprofibrate, clofibrate, clofibric acid, fenofibrate and gemfibrozil were separated by means of capillary electrophoresis, using unmodified fused silica tubing of 75μ m internal diameter and 87 cm length (65 cm to the UV detector at 227 nm). Migration time and selectivity were examined in differing pH of separation buffer, varying separation voltage and differing temperature. Optimal separation was achieved using 1/15 M phosphate buffer pH 10, 240 V/cm at 25 ° C. The optimal separation conditions were then used to elaborate the method of quantitation of bezafibrate, ciprofibrate and gemfibrozil in Bezamidin®, Lipanor® and Gemfibral® pharmaceuticals. The clofibric acid was used as internal standard. The calibration curve was constructed from 0.2 to 0.8 mg/ml of each compound and 0.5 mg/ml of internal standard. The calibration data were proved to be linear by Mandel and Lack-of-fit tests. Statistical evaluation of results proved proper recovery of elaborated method (102.42, 97.32 and 101.51%, respectively) and good repeatability (9.51, 5.52 and 11.15%, respectively). The linearity of recovery was also tested by analyzing increasing amount of the samples. Three fortified samples of each drug were also analyzed to perform additional accuracy validation.