Voltammetric behaviour of bromhexine and its determination in pharmaceuticals

M. Turchán, P. Jara-Ulloa, S. Bollo, L. J. Nuñez-Vergara, J. A. Squella, A. Álvarez-Lueje

Resultado de la investigación: Article

19 Citas (Scopus)

Resumen

A complete electrochemical study and a novel electroanalytical procedure for bromhexine quantitation are described. Bromhexine in methanol/0.1 mol L-1 Britton-Robinson buffer solution (2.5/97.5) shows an anodic response on glassy carbon electrode between pH 2 and 7.5. By DPV and CV, both peak potential and current peak values were pH-dependent in all the pH range studied. A break at pH 5.5 in EP versus pH plot revealing a protonation-deprotonation (pKa) equilibrium of bromhexine was observed. Spectrophotometrically, an apparent pKa value of 4.3 was also determined. An electrodic mechanism involving the oxidation of bromhexine via two-electrons and two-protons was proposed. Controlled potential electrolysis followed by HPLC-UV and GC-MS permitted the identification of three oxidation products: N-methylcyclohexanamine, 2-amino-3,5-dibromobenzaldehyde and 2,4,8,10-tetrabromo dibenzo[b,f][1,5] diazocine. DPV at pH 2 was selected as optimal pH for analytical purposes. Repeatability, reproducibility and selectivity parameters were adequate to quantify bromhexine in pharmaceutical forms. The recovery was 94.50 ± 2.03% and the detection and quantitation limits were 1.4 × 10-5 and 1.6 × 10-5 mol L-1, respectively. Furthermore, the DPV method was applied successfully to individual tablet assay in order to verify the uniformity content of bromhexine. No special treatment of sample were required due to excipients do not interfered with the analytical signal. Finally the method was not time-consuming and less expensive than the HPLC one.

Idioma originalEnglish
Páginas (desde-hasta)913-919
Número de páginas7
PublicaciónTalanta
Volumen73
N.º5
DOI
EstadoPublished - 31 oct 2007

Huella dactilar

Bromhexine
Pharmaceutical Preparations
High Pressure Liquid Chromatography
Oxidation
Deprotonation
Electrolysis
Excipients
Protonation
Glassy carbon
Tablets
Methanol
Protons
Assays
Buffers
Limit of Detection
Electrodes
Carbon
Recovery
Electrons

ASJC Scopus subject areas

  • Chemistry(all)

Citar esto

Turchán, M., Jara-Ulloa, P., Bollo, S., Nuñez-Vergara, L. J., Squella, J. A., & Álvarez-Lueje, A. (2007). Voltammetric behaviour of bromhexine and its determination in pharmaceuticals. Talanta, 73(5), 913-919. https://doi.org/10.1016/j.talanta.2007.05.010
Turchán, M. ; Jara-Ulloa, P. ; Bollo, S. ; Nuñez-Vergara, L. J. ; Squella, J. A. ; Álvarez-Lueje, A. / Voltammetric behaviour of bromhexine and its determination in pharmaceuticals. En: Talanta. 2007 ; Vol. 73, N.º 5. pp. 913-919.
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abstract = "A complete electrochemical study and a novel electroanalytical procedure for bromhexine quantitation are described. Bromhexine in methanol/0.1 mol L-1 Britton-Robinson buffer solution (2.5/97.5) shows an anodic response on glassy carbon electrode between pH 2 and 7.5. By DPV and CV, both peak potential and current peak values were pH-dependent in all the pH range studied. A break at pH 5.5 in EP versus pH plot revealing a protonation-deprotonation (pKa) equilibrium of bromhexine was observed. Spectrophotometrically, an apparent pKa value of 4.3 was also determined. An electrodic mechanism involving the oxidation of bromhexine via two-electrons and two-protons was proposed. Controlled potential electrolysis followed by HPLC-UV and GC-MS permitted the identification of three oxidation products: N-methylcyclohexanamine, 2-amino-3,5-dibromobenzaldehyde and 2,4,8,10-tetrabromo dibenzo[b,f][1,5] diazocine. DPV at pH 2 was selected as optimal pH for analytical purposes. Repeatability, reproducibility and selectivity parameters were adequate to quantify bromhexine in pharmaceutical forms. The recovery was 94.50 ± 2.03{\%} and the detection and quantitation limits were 1.4 × 10-5 and 1.6 × 10-5 mol L-1, respectively. Furthermore, the DPV method was applied successfully to individual tablet assay in order to verify the uniformity content of bromhexine. No special treatment of sample were required due to excipients do not interfered with the analytical signal. Finally the method was not time-consuming and less expensive than the HPLC one.",
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Turchán, M, Jara-Ulloa, P, Bollo, S, Nuñez-Vergara, LJ, Squella, JA & Álvarez-Lueje, A 2007, 'Voltammetric behaviour of bromhexine and its determination in pharmaceuticals', Talanta, vol. 73, n.º 5, pp. 913-919. https://doi.org/10.1016/j.talanta.2007.05.010

Voltammetric behaviour of bromhexine and its determination in pharmaceuticals. / Turchán, M.; Jara-Ulloa, P.; Bollo, S.; Nuñez-Vergara, L. J.; Squella, J. A.; Álvarez-Lueje, A.

En: Talanta, Vol. 73, N.º 5, 31.10.2007, p. 913-919.

Resultado de la investigación: Article

TY - JOUR

T1 - Voltammetric behaviour of bromhexine and its determination in pharmaceuticals

AU - Turchán, M.

AU - Jara-Ulloa, P.

AU - Bollo, S.

AU - Nuñez-Vergara, L. J.

AU - Squella, J. A.

AU - Álvarez-Lueje, A.

PY - 2007/10/31

Y1 - 2007/10/31

N2 - A complete electrochemical study and a novel electroanalytical procedure for bromhexine quantitation are described. Bromhexine in methanol/0.1 mol L-1 Britton-Robinson buffer solution (2.5/97.5) shows an anodic response on glassy carbon electrode between pH 2 and 7.5. By DPV and CV, both peak potential and current peak values were pH-dependent in all the pH range studied. A break at pH 5.5 in EP versus pH plot revealing a protonation-deprotonation (pKa) equilibrium of bromhexine was observed. Spectrophotometrically, an apparent pKa value of 4.3 was also determined. An electrodic mechanism involving the oxidation of bromhexine via two-electrons and two-protons was proposed. Controlled potential electrolysis followed by HPLC-UV and GC-MS permitted the identification of three oxidation products: N-methylcyclohexanamine, 2-amino-3,5-dibromobenzaldehyde and 2,4,8,10-tetrabromo dibenzo[b,f][1,5] diazocine. DPV at pH 2 was selected as optimal pH for analytical purposes. Repeatability, reproducibility and selectivity parameters were adequate to quantify bromhexine in pharmaceutical forms. The recovery was 94.50 ± 2.03% and the detection and quantitation limits were 1.4 × 10-5 and 1.6 × 10-5 mol L-1, respectively. Furthermore, the DPV method was applied successfully to individual tablet assay in order to verify the uniformity content of bromhexine. No special treatment of sample were required due to excipients do not interfered with the analytical signal. Finally the method was not time-consuming and less expensive than the HPLC one.

AB - A complete electrochemical study and a novel electroanalytical procedure for bromhexine quantitation are described. Bromhexine in methanol/0.1 mol L-1 Britton-Robinson buffer solution (2.5/97.5) shows an anodic response on glassy carbon electrode between pH 2 and 7.5. By DPV and CV, both peak potential and current peak values were pH-dependent in all the pH range studied. A break at pH 5.5 in EP versus pH plot revealing a protonation-deprotonation (pKa) equilibrium of bromhexine was observed. Spectrophotometrically, an apparent pKa value of 4.3 was also determined. An electrodic mechanism involving the oxidation of bromhexine via two-electrons and two-protons was proposed. Controlled potential electrolysis followed by HPLC-UV and GC-MS permitted the identification of three oxidation products: N-methylcyclohexanamine, 2-amino-3,5-dibromobenzaldehyde and 2,4,8,10-tetrabromo dibenzo[b,f][1,5] diazocine. DPV at pH 2 was selected as optimal pH for analytical purposes. Repeatability, reproducibility and selectivity parameters were adequate to quantify bromhexine in pharmaceutical forms. The recovery was 94.50 ± 2.03% and the detection and quantitation limits were 1.4 × 10-5 and 1.6 × 10-5 mol L-1, respectively. Furthermore, the DPV method was applied successfully to individual tablet assay in order to verify the uniformity content of bromhexine. No special treatment of sample were required due to excipients do not interfered with the analytical signal. Finally the method was not time-consuming and less expensive than the HPLC one.

KW - Bromhexine

KW - Differential pulse voltammetry

KW - Oxidation mechanism

KW - Tablets

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Turchán M, Jara-Ulloa P, Bollo S, Nuñez-Vergara LJ, Squella JA, Álvarez-Lueje A. Voltammetric behaviour of bromhexine and its determination in pharmaceuticals. Talanta. 2007 oct 31;73(5):913-919. https://doi.org/10.1016/j.talanta.2007.05.010