A voltammetric sensor based on carbon fiber paper modified with shungite and copper formazanate for the determination of lidocaine

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Abstract

A highly sensitive sensor based on carbon fiber paper modified with a shungite–copper formazanate composite is presented for the voltammetric determination of lidocaine. The synthesized organometallic complex, composite, and modified electrode are characterized by infrared spectroscopy, high-resolution mass spectrometry, elemental analysis, scanning electron microscopy, and cyclic and linear sweep voltammetry. The twofold increase in the current of the lidocaine oxidation peak on the modified electrode compared to the unmodified one is associated with the sensitizing effect of the composite modifier, which is due to an increase in the electroactive area and the number of lidocaine binding sites on the electrode surface. The sensor exhibits a wide dynamic range from 2 to 2120 µM with a low limit of detection of 0.18 µM lidocaine and high sensitivity of 0.755 µA/V µM. The interelectrode and intraelectrode repeatability of the analytical signal do not exceed 3.5%. The sensor response is stable within three weeks. The developed sensor was used for the determination of lidocaine in pharmaceuticals. The results of an analysis of real samples demonstrated good reproducibility (RSD ≤ 5.5%) and recovery (98–102%).

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About the authors

M. А. Bukharinova

Ural State Economic University

Email: sny@usue.ru
Russian Federation, 620144, Yekaterinburg

N. Yu. Stozhko

Ural State Economic University

Author for correspondence.
Email: sny@usue.ru
Russian Federation, 620144, Yekaterinburg

T. G. Fedorchenko

Postovskii Institute of Organic Synthesis, Ural Branch, Russian Academy of Sciences

Email: sny@usue.ru
Russian Federation, 620990, Yekaterinburg

G. N. Lipunova

Postovskii Institute of Organic Synthesis, Ural Branch, Russian Academy of Sciences

Email: sny@usue.ru
Russian Federation, 620990, Yekaterinburg

E. V. Shabrova

Ural State Economic University

Email: sny@usue.ru
Russian Federation, 620144, Yekaterinburg

Е. I. Khamzina

Ural State Economic University

Email: sny@usue.ru
Russian Federation, 620144, Yekaterinburg

А. V. Tarasov

Ural State Economic University

Email: sny@usue.ru
Russian Federation, 620144, Yekaterinburgс

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Supplementary files

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1. JATS XML
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2. Scheme 1. The structural formula of lidocaine.

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3. Scheme 2. Scheme of synthesis of copper formazanate (Cu CA).

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4. Scheme 3. The proposed structure of the lidocaine–SiOC complex.

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5. Scheme 4. The proposed mechanism of lidocaine oxidation at Sh-Cook/UVE.

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6. Fig. 1. IR spectra of copper (Cuoh) formazanates, shungite (I), and iCook composite.

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7. Fig. 2. Fragment of the mass spectrum of the CuOK complex, simulated for the composition C40H30N12O2S2ClCu2 and experimental.

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8. Fig. 3. SEM images of (a) an unmodified carbon fiber paper-based electrode (UVE) and (b) a modified Sh-SiOC/UVE. Accelerating voltage of 20 kV in the scattered electron mode.

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9. 4. The effect of (a) the mass fraction of the CuOR complex in the composite modifier and (b) the number of layers of the I-CuOK modifier on a carbon fiber electrode on the 0.64 mM lidocaine signal. Background: universal buffer solution with pH 8.

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10. Fig. 5. (a) Cyclic voltammograms of 1 mM K4[Fe(CN)6] solution recorded in 0.1 M KCl using an unmodified carbon fiber electrode (UVE) and a modified Sh-SiOC/UVE. (b) Chronoamperograms of a 1 mM solution of K4[Fe(CN)6] recorded at E = 0.6 V on different electrodes. Insert: dependence I = f(t-1/2), obtained from chronoamperometric measurements for different electrodes.

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11. 6. Cyclic voltammograms of 0.64 mM lidocaine solution on different electrodes: 1 ‒ UVE, 2 ‒ SiOK/UVE, 3 ‒ Sh/UVE, 4 ‒ Sh-SiOK/UVE. Background: universal buffer solution with pH 8, v = 50 mV/s.

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12. Fig. 7. (a) Cyclic voltammograms of 0.64 mM lidocaine solution, registered on the S-SiOC/UVE in a universal buffer solution with pH 6.5, 7.0, 7.5, 8.0, 8.3, 8.8, 9.0, 9.6, v = 50 mV/s; (b) the effect of the pH of the universal buffer solution on the oxidation peak potential of 0.64 mM lidocaine solution; (c) the dependence of the maximum current of 0.64 mM lidocaine solution on the pH of the universal buffer solution.

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13. Fig. 8. Linear voltammograms with correction of the baseline of 0.32 mM lidocaine solution in a universal buffer solution with pH 9 at the rate of potential expansion 50, 75, 100, 125, 150, 175, 200, 250, 300 mV/sec.

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14. Fig. 9. Derived voltammograms registered on W-Cook/UVE at different concentrations of lidocaine. Insert: dependence of the analytical signal on the concentration of lidocaine in solution.

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