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钴(II)-酞菁修饰电极电化学催化氧化-多径校准法测定葡萄酒中的酒石酸

Voltammetric determination of tartaric acid in wines by electrocatalytic oxidation on a cobalt(II)-phthalocyanine-modified electrode associated with multiway calibration.

机构信息

Universidade Federal Rural de Pernambuco, Departamento de Química, 52171-900 Recife, Pernambuco, Brazil.

Universidade Federal Rural de Pernambuco, Departamento de Química, 52171-900 Recife, Pernambuco, Brazil; Universidade Católica de Pernambuco, Departamento de Química, 50050-900 Recife, Pernambuco, Brazil.

出版信息

Anal Chim Acta. 2018 May 30;1008:29-37. doi: 10.1016/j.aca.2018.01.005. Epub 2018 Jan 20.

Abstract

The electrocatalytic oxidation of tartaric acid on a carbon paste electrode modified with cobalt (II)-phthalocyanine was demonstrated and applied to the development of a highly sensitive, simple, fast and inexpensive voltammetric sensor to determine tartaric acid. The electrochemical behavior of the modified electrode was investigated by cyclic and square wave voltammetry, and the effect of experimental variables, such as dispersion and loading of cobalt (II)-phthalocyanine, together with optimum conditions for sensing the analyte by square wave voltammetry were assessed. In addition, the absence of a significant memory effect combined with the ease of electrode preparation led to the development of a sensitive and direct method to determine tartaric acid in wines. Interferences from other low molecular weight organic acids commonly present in wines were circumvented by using a multiway calibration technique, successfully obtaining the second order advantage by modeling voltammetric data with unfolded partial least square with residual bilinearization (U-PLS/RBL). A linear response range between 10 and 100 μmol L (r = 0.9991), a relative prediction error of 4.55% and a recovery range from 96.41 to 102.43% were obtained. The proposed method is non-laborious, since it does not use sample pretreatment such as filtration, extraction, pre-concentration or cleanup procedures.

摘要

在碳糊电极上修饰钴(II)-酞菁电化学氧化酒石酸,并将其应用于开发一种高灵敏度、简单、快速且廉价的测定酒石酸的伏安传感器。通过循环伏安法和方波伏安法研究了修饰电极的电化学行为,并评估了实验变量(如钴(II)-酞菁的分散和负载)的影响,以及通过方波伏安法测定分析物的最佳条件。此外,由于不存在显著的记忆效应且电极制备简单,因此开发了一种灵敏且直接的方法来测定葡萄酒中的酒石酸。通过使用多变量校准技术,可以避免来自葡萄酒中常见的其他低分子量有机酸的干扰,成功地通过用无折叠偏最小二乘法与残差双线性化建模(U-PLS/RBL)对伏安数据进行建模获得二阶优势。得到的线性响应范围为 10 到 100 μmol·L(r=0.9991),相对预测误差为 4.55%,回收率范围为 96.41%至 102.43%。该方法不繁琐,因为它不需要使用过滤、提取、预浓缩或净化等样品预处理步骤。

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