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A rapid and sensitive CZE (Capillary Zone Electrophoresis) method for pharmaceutical analysis was developed and fully validated. The active compounds: Pseudoephedrine hydrochloride (PSE), Triprolidine hydrochloride (TRI) and Paracetamol (PAR) were separated and quantitatively determined using the tris-borate 30 mM buffer at pH = 9.0 as a Background Electrolyte (BGE). The electrophoretic separation was carried out at 25 kV in an unmodified fused silica capillary of I.D. = 50 μm with a “bubble-cell” for UV detection at 210 nm and 25°C. The separation was reached in about 3 min. After calibration the method was applied for analysis of three commercially available pharmaceutical preparations. The repeatability (RSD%) of migration time (tm) was ranging between 0.47% and 0.90% and of peak areas (A) between 0.63% and 3.64%. The Limit of Detection (LOD) values was of 0.19 μg/mL, 0.31 μg/mL and 0.08 μg/mL for respectively PSE, TRI and PAR. The results obtained in this study showed that the proposed method was useful in routinely analysis of pharmaceuticals.