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Capillary electrophoresis coupled with a capacitively coupled contactless conductivity detector (CE-C
4
D) has been employed for the determination of the β-blocker drugs (atenolol and amiloride) in pharmaceutical formulations.150 mM acetic acid was used as background electrolyte. The influence of several factors (detector excitation voltage and frequency,buffer concentration, applied voltage, capillary temperature, and injection time) was studied. Non-UV absorbing
l
-valine was used as an internal standard; the analytes were all separated in less than 7 min. The separation was carried outin normal polarity mode at 28 �C, 25 kV, and using hydrodynamic injection (25 s). The separation was effected in a bare fused-silicacapillary 75 μm � 52 cm. The CE-C
4
D method was validated with respect to linearity, limit of detection and quantification, accuracy, precision, and selectivity. Calibration curves were linear over the range 5–250 μg mL
−1
for the studied analytes. The relative standard deviations of intra- and inter-day precisions of migration times and correctedpeak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneousdetermination of the β-blocker drugs in different pharmaceutical tablets.