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Silver Nanoparticles‐silsesquioxane Nanomaterial Applied to the Determination of 4‐nitrophenol as a Biomarker
Electroanalysis ( IF 2.7 ) Pub Date : 2019-07-25 , DOI: 10.1002/elan.201900217 Paola Zimmermann Crocomo 1 , João Paulo Winiarski 1 , Marília Reginato Barros 1 , Eloah Latocheski 1 , Glaucio Régis Nagurniak 2 , Renato Luis Tame Parreira 3 , Diogo Alexandre Siebert 1 , Gustavo Amadeu Micke 1 , Hérica Aparecida Magosso 1 , Cristiane Luisa Jost 1
Electroanalysis ( IF 2.7 ) Pub Date : 2019-07-25 , DOI: 10.1002/elan.201900217 Paola Zimmermann Crocomo 1 , João Paulo Winiarski 1 , Marília Reginato Barros 1 , Eloah Latocheski 1 , Glaucio Régis Nagurniak 2 , Renato Luis Tame Parreira 3 , Diogo Alexandre Siebert 1 , Gustavo Amadeu Micke 1 , Hérica Aparecida Magosso 1 , Cristiane Luisa Jost 1
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A novel silsesquioxane material was synthetized and used as a stabilizing agent for silver nanoparticles. This hybrid material was characterized by FTIR, 29Si CP‐MAS NMR, 13C DEPT 135° NMR and TGA techniques and the silver nanoparticles were characterized from DLS, UV‐Vis spectroscopy, zeta‐potential, TEM and SAXS results. The silver nanoparticles obtained were spherical in shape with a diameter of 3.74 nm. The nanomaterial was successfully applied in the modification of a glassy carbon electrode and a pronounced current response was obtained in the determination of the biomarker 4‐nitrophenol. Quantum chemical calculations, using density functional theory, were also performed in order to evaluate the redox properties of the analyte. Two different linear ranges were obtained applying optimal square wave voltammetry conditions. The reduction peak currents obtained were linear for 4‐NP concentrations in the ranges of 0.29 to 1.50 μmol L−1 (Ed=−0.6 V and td=20 s) and 2.75 to 31.5 μmol L−1, with a theoretical (signal to noise=3) limit of detection of 0.05 μmol L−1 (td=20 s). The proposed method was successfully applied to the determination of 4‐NP in synthetic serum samples at different levels of 4‐NP with a recovery range of 94–101 %. Validation was performed using a comparative method through the capillary electrophoresis (CE) technique.
中文翻译：
纳米银-倍半硅氧烷银纳米材料用于测定4-硝基苯酚作为生物标志物
合成了一种新的倍半硅氧烷材料，并用作银纳米颗粒的稳定剂。这种杂化材料的特征是FTIR，29 Si CP‐MAS NMR，13C DEPT 135°NMR和TGA技术以及银纳米颗粒通过DLS，UV-Vis光谱，ζ-电势，TEM和SAXS结果进行了表征。获得的银纳米颗粒为球形，直径为3.74nm。纳米材料已成功地应用于修饰玻碳电极，并在测定生物标记物4-硝基苯酚中获得了明显的电流响应。为了评估分析物的氧化还原特性，还使用密度泛函理论进行了量子化学计算。应用最佳方波伏安条件获得了两个不同的线性范围。在4-NP浓度范围为0.29至1.50μmolL -1（E d = -0.6 V和td = 20 s）和2.75至31.5μmolL -1，理论（信噪比= 3）检测极限为0.05μmolL -1（t d = 20 s）。所提出的方法已成功地用于测定不同浓度的4–NP合成血清样品中的4–NP，回收率在94–101％之间。使用比较方法通过毛细管电泳（CE）技术进行验证。
更新日期：2019-11-18
中文翻译：
纳米银-倍半硅氧烷银纳米材料用于测定4-硝基苯酚作为生物标志物
合成了一种新的倍半硅氧烷材料，并用作银纳米颗粒的稳定剂。这种杂化材料的特征是FTIR，29 Si CP‐MAS NMR，13C DEPT 135°NMR和TGA技术以及银纳米颗粒通过DLS，UV-Vis光谱，ζ-电势，TEM和SAXS结果进行了表征。获得的银纳米颗粒为球形，直径为3.74nm。纳米材料已成功地应用于修饰玻碳电极，并在测定生物标记物4-硝基苯酚中获得了明显的电流响应。为了评估分析物的氧化还原特性，还使用密度泛函理论进行了量子化学计算。应用最佳方波伏安条件获得了两个不同的线性范围。在4-NP浓度范围为0.29至1.50μmolL -1（E d = -0.6 V和td = 20 s）和2.75至31.5μmolL -1，理论（信噪比= 3）检测极限为0.05μmolL -1（t d = 20 s）。所提出的方法已成功地用于测定不同浓度的4–NP合成血清样品中的4–NP，回收率在94–101％之间。使用比较方法通过毛细管电泳（CE）技术进行验证。
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