Abstract Here, aluminum (Al) doped Zirconia nanoparticles (ZrO2 NPs) were proposed as a novel material for the fabrication of an efficient electrochemical immunosensor. X-ray diffraction (XRD) analysis and high resolution–transmission electron microscopy (HR-TEM) images visualized phase stabilization and generation of oxygen deficiency in the ZrO2 lattice due to doping of Al ions (Al3+). On the increase in Al3+ concentration, a sequential decrease in crystallite size of ZrO2 NPs describes the Zener pinning effect. Further increase in Al3+concentration (beyond 11 mol%) terminated crystallinity of ZrO2 NPs. The generated oxygen deficiency due to Al3+ doping increased the surface charge and hydrophilicity of ZrO2 NPs as observed by zeta potential and contact angle measurements, respectively. Moreover, oxygen deficiency was the main reason for the remarkable enhancement in the electrochemical behavior of Al3+ doped ZrO2 NPs, and maximum was observed for 7 mol% Al3+ doped ZrO2 NPs. Thus, 7 mol% Al3+ doped ZrO2 NPs based Al3+-ZrO2/ITO electrodes were fabricated via electrophoretic deposition and further functionalized with antibodies specific to Ochratoxin A (anti-OTA) and bovine serum albumin (BSA). Fabricated BSA/anti-OTA/Al3+-ZrO2/ITO immunoelectrode showed improved sensitivity of 34.07 μA (log ng mL−1)−1 and LOD of 0.14 ng mL−1 in the detection range of 1–10 ng mL−1 as compared to BSA/anti-OTA/ZrO2/ITO immunoelectrode for the detection of OTA. Moreover, recovery of OTA from the spiked sample was observed in the range of 93.3–99.2% with maximum relative standard deviation (RSD) of 4.86.

中文翻译：

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用于检测赭曲霉毒素 A 的金属掺杂氧化锆纳米粒子的电化学性能的改进

摘要 这里，铝 (Al) 掺杂的氧化锆纳米粒子 (ZrO2 NPs) 被提议作为一种新型材料，用于制造高效的电化学免疫传感器。X 射线衍射 (XRD) 分析和高分辨率透射电子显微镜 (HR-TEM) 图像显示了由于掺杂 Al 离子 (Al3+) 而导致的 ZrO2 晶格中的相稳定和缺氧现象。随着 Al3+ 浓度的增加，ZrO2 NPs 微晶尺寸的连续减小描述了齐纳钉扎效应。Al3+ 浓度的进一步增加（超过 11 mol%）终止了 ZrO2 NPs 的结晶度。分别通过 zeta 电位和接触角测量观察到，由于 Al3+ 掺杂而产生的氧缺陷增加了 ZrO2 NPs 的表面电荷和亲水性。而且，氧缺乏是 Al3+ 掺杂的 ZrO2 NPs 电化学行为显着增强的主要原因，并且在 7 mol% Al3+ 掺杂的 ZrO2 NPs 中观察到最大值。因此，基于 Al3+-ZrO2/ITO 电极的 7 mol% Al3+ 掺杂的 ZrO2 NPs 通过电泳沉积制成，并进一步用赭曲霉毒素 A（抗 OTA）和牛血清白蛋白（BSA）特异性抗体进行功能化。相比之下，制造的 BSA/anti-OTA/Al3+-ZrO2/ITO 免疫电极在 1-10 ng mL-1 的检测范围内显示出 34.07 μA (log ng mL-1)-1 的灵敏度提高和 0.14 ng mL-1 的 LOD用于检测 OTA 的 BSA/anti-OTA/ZrO2/ITO 免疫电极。此外，从加标样品中观察到 OTA 的回收率在 93.3-99.2% 的范围内，最大相对标准偏差 (RSD) 为 4.86。