Freitas P V, da Silva D R, Beluomini M A, da Silva J L, Stradiotto N R
Departamento de Tecnologia de Alimentos, Centro de Ciências Exatas e Tecnológicas, Universidade Federal de Viçosa, Av. Peter Henry Rolfs s/n, Viçosa, MG, Brazil.
Departmento de Química Analítica, Instituto de Química (IQ/CAr), Universidade Estadual Paulista, R. Prof. Francisco Degni 55, Jardim Quitandinha, 14800-060 Araraquara, SP, Brazil.
J Anal Methods Chem. 2018 Jan 21;2018:4869487. doi: 10.1155/2018/4869487. eCollection 2018.
A reversed-phase liquid chromatographic separation with pulsed amperometric detection of phenolic acids at a glassy carbon electrode is described. Chromatographic separation was carried out in isocratic conditions using 0.20 mol·L acetic acid (pH 5.0)/water (80 : 20, /) as mobile phase under constant working potential mode of 0.80 V. Chromatographic peaks presented high resolution and separation. Calibration curves exhibited excellent correlation coefficients, above 0.995. Linear ranges of the analytes, in mg L, were of 0.018-18 (gallic acid), 0.146-19 (vanillic acid), 0.13-17 (caffeic acid), 0.016-16 (ferulic acid), and 0.008-17 (p-coumaric acid), respectively. Limits of detection ranged from 1.6 to 97 g·L and precision varied in 1.73-3.78% interval. Concentrations of 19 ± 0.51 mg·L and 7.8 ± 2.5 mg·L were found for vanillic and caffeic acids, respectively, in a sugarcane vinasse sample. Gallic, ferulic, and p-coumaric acids were not detected. Recovery results demonstrated that the proposed method is accurate, and it can be used to detect and quantify phenolic acids in sugarcane vinasse without any influence of interferents.
描述了一种在玻碳电极上采用脉冲安培检测法对酚酸进行反相液相色谱分离的方法。色谱分离在等度条件下进行,以0.20 mol·L醋酸(pH 5.0)/水(80 : 20,v/v)作为流动相,在0.80 V的恒定工作电位模式下进行。色谱峰呈现出高分辨率和分离度。校准曲线具有优异的相关系数,高于0.995。各分析物的线性范围(mg/L)分别为:没食子酸0.018 - 18、香草酸0.146 - 19、咖啡酸0.13 - 17、阿魏酸0.016 - 16和对香豆酸0.008 - 17。检测限范围为1.6至97 μg·L,精密度在1.73 - 3.78%区间内变化。在甘蔗酒糟样品中,分别测得香草酸和咖啡酸的浓度为19 ± 0.51 mg/L和7.8 ± 2.5 mg/L。未检测到没食子酸、阿魏酸和对香豆酸。回收率结果表明,所提出的方法准确,可用于检测和定量甘蔗酒糟中的酚酸,不受干扰物的影响。