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通过β-环糊精聚合对天然羟基磷灰石进行表面功能化:用作电化学检测Pb(II)的电极材料

Surface functionalization of natural hydroxyapatite by polymerization of β-cyclodextrin: application as electrode material for the electrochemical detection of Pb(II).

作者信息

Tchoffo Rodrigue, Ngassa Guy B P, Doungmo Giscard, Kamdem Arnaud T, Tonlé Ignas K, Ngameni Emmanuel

机构信息

Laboratory of Analytical Chemistry, Faculty of Science, The University of Yaounde 1, P.O. Box 812, Yaounde, Cameroon.

Department of Chemistry, University of Douala, P.O. Box 24157, Douala, Cameroon.

出版信息

Environ Sci Pollut Res Int. 2022 Jan;29(1):222-235. doi: 10.1007/s11356-021-15578-8. Epub 2021 Aug 3.

DOI:10.1007/s11356-021-15578-8
PMID:34342829
Abstract

A composite material prepared by polymerization of β-cyclodextrin (β-CD) on the surface of natural hydroxyapatite using citric acid as cross linker, was employed as electrode material for the detection of Pb(II). Hydroxyapatite was obtained from bovine bones, following a three-step procedure including pre-calcination, chemical treatment with (NH)HPO and calcination. The structure and morphology of the pristine hydroxyapatite (NHAP) and its functionalized counterpart (NHAP-CA-β-CD) were examined using XRD, FTIR, and SEM. Upon deposition as thin film on a glassy carbon electrode (GCE), the ion exchange ability of NHAP-CA-β-CD was exploited to elaborate a sensitive sensor for the detection of lead. The electroanalytical procedure was based on the chemical accumulation of Pb(II) ions under open-circuit conditions, followed by the detection of the preconcentrated species using differential pulse anodic stripping voltammetry. The reproducibility of the proposed method, based on a series of 8 measurements in a solution containing 2 μM Pb(II) gave a coefficient of variation of 1.27%. Significant parameters that can affect the stripping response of Pb(II) were optimized, leading to a linear calibration curve for lead in the concentration range of 2 × 10 mol L - 20 × 10 mol L (R = 0.998). The detection limit (3S/m) and the sensitivity of the proposed sensor were 5.06 × 10 mol L and 100.80 μA.μM, respectively. The interfering effect of several ions expected to affect the determination of lead was evaluated, and the proposed sensor was successfully applied in the determination of Pb(II) ions in spring water, well water, river water and tap water samples.

摘要

以柠檬酸为交联剂,通过β-环糊精(β-CD)在天然羟基磷灰石表面聚合制备的复合材料,被用作检测Pb(II)的电极材料。羟基磷灰石取自牛骨,经过三步程序,包括预煅烧、用(NH)HPO进行化学处理和煅烧。使用XRD、FTIR和SEM对原始羟基磷灰石(NHAP)及其功能化对应物(NHAP-CA-β-CD)的结构和形态进行了研究。当以薄膜形式沉积在玻碳电极(GCE)上时,利用NHAP-CA-β-CD的离子交换能力精心制作了一种用于检测铅的灵敏传感器。电分析程序基于开路条件下Pb(II)离子的化学积累,然后使用差分脉冲阳极溶出伏安法检测预富集的物质。基于在含有2μM Pb(II)的溶液中进行的一系列8次测量,该方法的重现性给出了1.27%的变异系数。优化了可能影响Pb(II)溶出响应的重要参数,得到了浓度范围为2×10 mol L - 20×10 mol L的铅的线性校准曲线(R = 0.998)。所提出传感器的检测限(3S/m)和灵敏度分别为5.06×10 mol L和100.80μA.μM。评估了几种预期会影响铅测定的离子的干扰效应,所提出的传感器成功应用于泉水、井水、河水和自来水样品中Pb(II)离子的测定。

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