Abstract
A new, highly sensitive voltammetric method for the determination of aceclofenac (ACL) was developed. As a working electrode, GCE modified with carbon nanofibers, carbon nanotubes and NiCo nanoparticles (eCNF/CNT/NiCo-GCE) was used. Signal repeatability obtained on the applied sensor, expressed as relative standard deviation (RSD%) was very good:RSD = 1.2% (n = 9, ACL concentration 0.1 µM). The instrumental parameters were optimized and were as follows: waiting time t w = 5 ms, sampling time t s = 10 ms, step potential E s = 6mV, pulse amplitude ΔE = 100 mV. Supporting electrolyte was consisted of 0.025 M HClO 4 . Accumulation step was performed at the potential 500 mV. Based on the calibration conducted (accumulation time t acc = 45 s) limit of detection (LOD) and the limit of quantification (LOQ) were calculated and were equal to 0.7 and 2.1 nM, respectively. Linear range was estimated to be between 0.05 and 1.4 µM (slope: 4.45 ± 0.07 µA µM -1 , intercept: 0.18 ± 0.05 µA, r = 0.998). Applicability of the method was verified by determination of ACL in tablets, urine and plasma. Calculated recoveries were in the range 98 – 105% what suggest that method might be considered as accurate.

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