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. 2012 Feb 21:6:15.
doi: 10.1186/1752-153X-6-15.

Development of square-wave adsorptive stripping voltammetric method for determination of acebutolol in pharmaceutical formulations and biological fluids

Ali F Al-Ghamdi  1 , Mohamed M Hefnawy, Abdulrahman A Al-Majed, Fatallah F Belal
Affiliations

Development of square-wave adsorptive stripping voltammetric method for determination of acebutolol in pharmaceutical formulations and biological fluids

Ali F Al-Ghamdi et al. Chem Cent J. .

Abstract

A validated simple, rapid, sensitive and specific square-wave voltammetric technique is described for the determination of acebutolol (AC) following its accumulation onto a hanging mercury drop electrode in a Britton-Robinson universal buffer of pH 7.5. The optimal procedural conditions were: accumulation potential Eacc = - 0.8 V versus Ag/AgCl/KCl, accumulation duration tacc = 30 s, pulse-amplitude = 70 mV, scan rate = 100 mV/s, frequency = 30 Hz, surface area of the working electrode = 0.6 mm2 and the convection rate = 2000 rpm. Under these optimized conditions, the adsorptive stripping voltammetry (AdSV) peak current was proportional over the concentration range 5 × 10-7 - 6 × 10-6 M (r = 0.999). Recoveries for acebutolol from human plasma and urine were in the range 97-103% and 96-104% respectively. The method proved to be precise (intra-day precision expressed as %RSD in human plasma ranged from 2.9 - 3.2% and inter-day precision expressed as %RSD ranged from 3.4 - 3.8%) and accurate (intra-day accuracies expressed as % error in human urine ranged from -3.3 - 2.8% and inter-day accuracies ranged from -3.3 - 1.7%). The limit of quantitation (LOQ) and limit of detection (LOD) for acebutolol were 1.7 × 10-7 and 5 × 10-7 M, respectively. Possible interferences by substances usually present in the pharmaceutical formulations were investigated with a mean recovery of 101.6 ± 0.64%. Results of the developed square-wave adsorptive stripping voltammetry (SW-AdSV) method were comparable with those obtained by reference analytical method.

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Figures

Scheme 1
Scheme 1
Suggested mechanism of the studied electrochemical reduction process for acebutolol.
Figure 1
Figure 1
Repetitive cyclic voltammograms for 5 × 10-6 mol L-1 acebutolol in pH 7.5 B-R buffer, scan rate 50 mV-1, accumulation potential 0.0 V and preconcentration time 30 s (scan A).
Figure 2
Figure 2
SW-AdSV voltammogram for acebutolol in B-R buffer (pH 7.5), tacc: 60 s, E acc: -0.8 V, scan rate: 100 mVs-1, SW frequency: 30 Hz and pulse amplitude: 70 mV. acebutolol concentration: (A) 5.0 × 10-6 10 mol L-1.
Figure 3
Figure 3
Effect of pH on SW-AdSV peak current of 5 × 10-6 mol L-1 acebutolol in B-R buffer after an accumulation period of 60 s at Eacc = 0.0 V.
Figure 4
Figure 4
Effect of accumulation time on the stripping voltammetric peak current of 5 × 10-6 mol L-1 acebutolol in pH 7.5 B-R buffer. Accumulation potential: 0.0 V.
Figure 5
Figure 5
Effect of accumulation potential on the stripping voltammetric peak current of 5 × 10-6 mol L-1 acebutolol in pH 7.5 B-R buffer. Accumulation time: 30 s.
Figure 6
Figure 6
Effect of scan rate on AdSV peak current of 5 × 10-6 mol L-1 acebutolol in pH 7.5 B-R buffer. Accumulation time: 30 s and accumulation potential: -0.8 V.
Figure 7
Figure 7
Effect of pulse amplitude on the stripping voltammetric peak current of 5 × 10-6 mol L-1 acebutolol in pH 7.5 B-R buffer. Accumulation time: 30 s, accumulation potential: -0.8 V and scan rate: 100 mV s-1.
Figure 8
Figure 8
Effect of frequency on the stripping voltammetric peak current of 5 × 10-6 mol L-1 acebutolol in pH 7.5 B-R buffer. Accumulation time: 30 s, accumulation potential: -0.8 V, scan rate: 100 mV s-1 and pulse amplitude 20 mV.
Figure 9
Figure 9
SW-AdSV voltammograms for Acebutolol in B-R buffer, pH = 7.5, tacc = 30 sec, Eacc= -0.80 V, Drug Conc.:- (A = 5 × 10-7 M, B = 1 × 10-6 M, C = 3 × 10-6 M, D = 6 × 10-6 M)
Figure 10
Figure 10
SW-AdSV voltammograms for Acebutolol in human urine.
Figure 11
Figure 11
SW-AdSV voltammograms for Acebutolol in human plasma.
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