Kemmegne-Mbouguen Justin Claude, Tamne Guy Bertrand, Ngo-Ngwem Marcelline Carine, Toma Henrique Eisi, Araki Koiti, Constantino Vera Regina Leopoldo, Angnes Lúcio
Laboratory of Porous Materials for Sensors and Energy, Faculty of Science, University of Yaounde 1 P.O. Box 812 Yaounde Cameroon
Department of Chemistry, High Teacher Training College, University of Yaounde 1 P.O. Box 49 Yaounde Cameroon.
RSC Adv. 2024 Jun 18;14(27):19592-19602. doi: 10.1039/d4ra03253e. eCollection 2024 Jun 12.
A supramolecular complex μ--tetra(4-pyridyl) porphyrinate nickel(ii)tetrakis[bis(bipyridine)(chloro)ruthenium(ii)] ([NiTPyP{Ru(bipy)Cl}]) was intercalated into the interlayer space of natural smectite clay (shortened as Ba) collected in a Cameroonian deposit at Bagba hill. Physicochemical characterization of the resulting material using ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared (FTIR) spectroscopy, and X-ray diffraction (XRD) confirmed the intercalation of the porphyrin within the interlayer space of the clay. The intercalated clay was then used to form a stable thin film onto a glassy carbon electrode (GCE) by drop casting a suspension of the hybrid material. The GCE modified with the intercalated organoclay endowed the electrode with a larger electrochemically active surface area, good stability, high selectivity, and sensitivity toward dopamine (DA), acetaminophen (AC) and tryptophan (Trp). In addition, it was observed that the modified electrodes exhibited good and pH-dependent electrocatalytic properties toward these analytes. The simultaneous determination of DA, AC and Trp at [NiTPyP{Ru(bipy)Cl}]-Ba/GCE was thus possible without the interference of one analyte on the others, and the resulting calibration curve exhibits two segments for the three analytes. For DA, AC and Trp, the detection limits were found to be 0.8 μM, 0.3 μM and 0.3 μM, respectively. The [NiTPyP{Ru(bipy)Cl}]-Ba/GCE modified electrodes were successfully applied for the determination of AC in Paracetamol, a commercial product, and Trp in real pharmaceutical formulation samples.
一种超分子配合物μ-四(4-吡啶基)卟啉镍(ii)四双(联吡啶)(氯)钌(ii)被插入到在喀麦隆巴格巴山矿床采集的天然蒙脱石粘土(简称为Ba)的层间空间中。使用紫外可见光谱(UV-vis)、傅里叶变换红外(FTIR)光谱和X射线衍射(XRD)对所得材料进行的物理化学表征证实了卟啉在粘土层间空间中的插入。然后通过滴铸混合材料的悬浮液,将插层粘土用于在玻碳电极(GCE)上形成稳定的薄膜。用插层有机粘土修饰的GCE赋予电极更大的电化学活性表面积、良好的稳定性、高选择性以及对多巴胺(DA)、对乙酰氨基酚(AC)和色氨酸(Trp)的灵敏度。此外,观察到修饰电极对这些分析物表现出良好的且依赖于pH的电催化性能。因此,在[NiTPyP{Ru(bipy)Cl}]-Ba/GCE上可以同时测定DA、AC和Trp,而一种分析物不会对其他分析物产生干扰,并且所得校准曲线对三种分析物呈现出两个部分。对于DA、AC和Trp,检测限分别为0.8 μM、0.3 μM和0.3 μM。[NiTPyP{Ru(bipy)Cl}]-Ba/GCE修饰电极成功应用于商业产品扑热息痛中AC的测定以及实际药物制剂样品中Trp的测定。