Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone
Testosterone (TST), despite its good properties, may be harmful to the human organism and the environment. Therefore, monitoring biological fluids and environmental samples is important. An electrochemically pretreated screen-printed carbon sensor modified with Pb nanoparticles (pSPCE/PbNPs) was suc...
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2022-07-01
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author | Jędrzej Kozak Katarzyna Tyszczuk-Rotko Magdalena Wójciak Ireneusz Sowa Marek Rotko |
author_facet | Jędrzej Kozak Katarzyna Tyszczuk-Rotko Magdalena Wójciak Ireneusz Sowa Marek Rotko |
author_sort | Jędrzej Kozak |
collection | DOAJ |
description | Testosterone (TST), despite its good properties, may be harmful to the human organism and the environment. Therefore, monitoring biological fluids and environmental samples is important. An electrochemically pretreated screen-printed carbon sensor modified with Pb nanoparticles (pSPCE/PbNPs) was successfully prepared and used for the determination of TST. The surface morphology and electrochemical properties of unmodified and modified sensors were characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), scanning and transmission electron microscopy (SEM and TEM), and energy-dispersive X-ray spectroscopy (EDS). Selective determinations of TST at the pSPCE/PbNPs were carried out by differential pulse adsorptive stripping voltammetry (DPAdSV, E<sub>Pb dep.and TST acc.</sub> of −1.1 V, t <sub>Pb dep.and TST acc.</sub> of 120 s, ΔE<sub>A</sub> of 50 mV, ν of 175 mV s<sup>−1</sup>, and t<sub>m</sub> of 5 ms) in a solution containing 0.075 mol L<sup>−1</sup> acetate buffer of pH = 4.6 ± 0.1, and 7.5 × 10<sup>−5</sup> mol L<sup>−1</sup> Pb(NO<sub>3</sub>)<sub>2</sub>. The analytical signal obtained at the potential around −1.42 V (vs. silver pseudo-reference electrode) is related to the reduction process of TST adsorbed onto the electrode surface. The use of pSPCE/PbNPs allows obtaining a very low limit of TST detection (2.2 × 10<sup>−12</sup> mol L<sup>−1</sup>) and wide linear ranges of the calibration graph (1.0 × 10<sup>−11</sup>–1.0 × 10<sup>−10</sup>, 1.0 × 10<sup>−10</sup>–2.0 × 10<sup>−9</sup>, and 2.0 × 10<sup>−9</sup>–2.0 × 10<sup>−8</sup> mol L<sup>−1</sup>). The pSPCE/PbNPs were successfully applied for the determination of TST in reference material of human urine and wastewater purified in a sewage treatment plant without preliminary preparation. |
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institution | Directory Open Access Journal |
issn | 1996-1944 |
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spelling | doaj.art-c1aa75bfaac54ef08e6f4e266eee348b2023-11-30T21:22:01ZengMDPI AGMaterials1996-19442022-07-011514494810.3390/ma15144948Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of TestosteroneJędrzej Kozak0Katarzyna Tyszczuk-Rotko1Magdalena Wójciak2Ireneusz Sowa3Marek Rotko4Institute of Chemical Sciences, Faculty of Chemistry, Maria Curie-Skłodowska University in Lublin, 20-031 Lublin, PolandInstitute of Chemical Sciences, Faculty of Chemistry, Maria Curie-Skłodowska University in Lublin, 20-031 Lublin, PolandDepartment of Analytical Chemistry, Medical University of Lublin, 20-093 Lublin, PolandDepartment of Analytical Chemistry, Medical University of Lublin, 20-093 Lublin, PolandInstitute of Chemical Sciences, Faculty of Chemistry, Maria Curie-Skłodowska University in Lublin, 20-031 Lublin, PolandTestosterone (TST), despite its good properties, may be harmful to the human organism and the environment. Therefore, monitoring biological fluids and environmental samples is important. An electrochemically pretreated screen-printed carbon sensor modified with Pb nanoparticles (pSPCE/PbNPs) was successfully prepared and used for the determination of TST. The surface morphology and electrochemical properties of unmodified and modified sensors were characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), scanning and transmission electron microscopy (SEM and TEM), and energy-dispersive X-ray spectroscopy (EDS). Selective determinations of TST at the pSPCE/PbNPs were carried out by differential pulse adsorptive stripping voltammetry (DPAdSV, E<sub>Pb dep.and TST acc.</sub> of −1.1 V, t <sub>Pb dep.and TST acc.</sub> of 120 s, ΔE<sub>A</sub> of 50 mV, ν of 175 mV s<sup>−1</sup>, and t<sub>m</sub> of 5 ms) in a solution containing 0.075 mol L<sup>−1</sup> acetate buffer of pH = 4.6 ± 0.1, and 7.5 × 10<sup>−5</sup> mol L<sup>−1</sup> Pb(NO<sub>3</sub>)<sub>2</sub>. The analytical signal obtained at the potential around −1.42 V (vs. silver pseudo-reference electrode) is related to the reduction process of TST adsorbed onto the electrode surface. The use of pSPCE/PbNPs allows obtaining a very low limit of TST detection (2.2 × 10<sup>−12</sup> mol L<sup>−1</sup>) and wide linear ranges of the calibration graph (1.0 × 10<sup>−11</sup>–1.0 × 10<sup>−10</sup>, 1.0 × 10<sup>−10</sup>–2.0 × 10<sup>−9</sup>, and 2.0 × 10<sup>−9</sup>–2.0 × 10<sup>−8</sup> mol L<sup>−1</sup>). The pSPCE/PbNPs were successfully applied for the determination of TST in reference material of human urine and wastewater purified in a sewage treatment plant without preliminary preparation.https://www.mdpi.com/1996-1944/15/14/4948testosteroneelectrochemical preparationscreen-printed carbon sensorlead nanoparticlesdifferential-pulse adsorptive stripping voltammetryhuman urine |
spellingShingle | Jędrzej Kozak Katarzyna Tyszczuk-Rotko Magdalena Wójciak Ireneusz Sowa Marek Rotko Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone Materials testosterone electrochemical preparation screen-printed carbon sensor lead nanoparticles differential-pulse adsorptive stripping voltammetry human urine |
title | Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone |
title_full | Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone |
title_fullStr | Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone |
title_full_unstemmed | Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone |
title_short | Electrochemically Pretreated Sensor Based on Screen-Printed Carbon Modified with Pb Nanoparticles for Determination of Testosterone |
title_sort | electrochemically pretreated sensor based on screen printed carbon modified with pb nanoparticles for determination of testosterone |
topic | testosterone electrochemical preparation screen-printed carbon sensor lead nanoparticles differential-pulse adsorptive stripping voltammetry human urine |
url | https://www.mdpi.com/1996-1944/15/14/4948 |
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