This paper reports the application of a carbon paste electrode modified with magnetite nanoparticles and the ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate in the electroanalytical determination of 17β-estradiol and estriol. These estrogens are potential endocrine disruptors and thus it is relevant the development of devices for their monitoring. Transmission electron microscopy, scanning electron microscopy and zeta potential techniques were applied to characterization of the modifier materials. In cyclic voltammetry experiments, irreversible oxidation peaks were observed for 17β-estradiol and estriol at +0.320 V and +0.400 V, respectively. The anodic currents obtained were approximately three times greater than those provided by the unmodified electrode due to the presence of magnetic nanoparticles and the ionic liquid, which improved the sensitivity of modified electrode. For the analysis, the parameters of the square-wave voltammetry (scan increment, amplitude and frequency) were optimized by Box-Behnken factorial design for each estrogen. For 17β-estradiol in B-R buffer pH 12.0, the calibration plot was linear from 0.10 to 1.0 μmol L-1, with a detection limit of 50.0 nmol L-1. For estriol in B-R buffer pH 11.0, the linear range was 1.0 to 10.0 μmol L-1, with a detection limit of 300.0 nmol L-1. The modified electrode was applied in the determination of 17β-estradiol and estriol in pharmaceutical formulations and the results were comparable to those obtained using UV/VIS spectrometry. Statistical tests were applied to evaluate the results and it was concluded that there was no significant difference regarding the precision and accuracy of the data provided by the two methods.

译文

:本文报道了用磁铁矿纳米粒子和离子液体1-丁基-3-甲基咪唑鎓六氟磷酸盐修饰的碳糊电极在电分析中测定17β-雌二醇和雌三醇的应用。这些雌激素是潜在的内分泌干扰物,因此与其监测装置的开发有关。透射电子显微镜,扫描电子显微镜和ζ电势技术被用于表征改性剂材料。在循环伏安法实验中,分别在0.320 V和0.400 V处观察到17β-雌二醇和雌三醇的不可逆氧化峰。由于存在磁性纳米粒子和离子液体,因此获得的阳极电流约为未修饰电极提供的阳极电流的三倍,从而提高了修饰电极的灵敏度。为了进行分析,通过Box-Behnken因子设计针对每种雌激素对方波伏安法的参数(扫描增量,幅度和频率)进行了优化。对于pH值为12.0的B-R缓冲液中的17β-雌二醇,校正曲线在0.10至1.0?μmolL-1之间呈线性关系,检出限为50.0 nmol L-1。对于在pH 11.0的B-R缓冲液中的雌三醇,线性范围为1.0至10.0μmolL-1,检测极限为300.0 nmol L-1。修饰的电极用于测定药物制剂中的17β-雌二醇和雌三醇,其结果与使用UV / VIS光谱法获得的结果相当。应用统计测试评估结果,得出的结论是,两种方法提供的数据的准确性和准确性没有显着差异。

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