Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis, SC, 88040-900, Brazil.
Departamento de Farmacociências, Universidade Federal de Ciências da Saúde de Porto Alegre, Porto Alegre, RS, 90050-170, Brazil.
Talanta. 2020 Nov 1;219:121369. doi: 10.1016/j.talanta.2020.121369. Epub 2020 Jul 9.
This study reports a novel and environmentally friendly method based on bar adsorptive microextraction (BAμE) with cork pellet as extraction phase for the determination of methylparaben, ethylparaben, propylparaben and butylparaben in river water samples. This natural approach consists of a cork pellet recycled from wine stoppers used as biosorbent material to replace the traditional BAμE device. The analytical determinations were performed using a high-performance liquid chromatography-diode array detector (HPLC-DAD). Parameters such as type of desorption solvent, desorption and extraction time, sample pH and ionic strength were carefully optimized through univariate and multivariate approaches. Cork pellets of 15 mm length were inserted into vials containing 15 mL of water sample adjusted at pH 3 and 25% (w/v) of NaCl. The extraction step was carried out under agitation for 45 min followed by liquid desorption with 120 μL of methanol:acetonitrile (1:1 v/v) for 30 min. Satisfactory analytical performance was obtained with coefficients of determination ranging from 0.9921 for methylparaben to 0.9994 for propylparaben; intraday precision ranged from 6.7 to 18.3%, and interday precision varied from 7.2 to 20.0%. Accuracy was assessed through relative recovery assays and varied from 53 to 124%.
本研究报告了一种新颖且环保的方法,基于 cork pellet(软木颗粒)的 bar adsorptive microextraction(BAμE),用于测定河水样品中的甲基对羟基苯甲酸酯、乙基对羟基苯甲酸酯、丙基对羟基苯甲酸酯和丁基对羟基苯甲酸酯。这种天然方法使用从葡萄酒瓶塞中回收的 cork pellet(软木颗粒)作为生物吸附材料,替代传统的 BAμE 装置。分析测定采用高效液相色谱-二极管阵列检测器(HPLC-DAD)进行。通过单变量和多变量方法,仔细优化了洗脱溶剂类型、洗脱和萃取时间、样品 pH 值和离子强度等参数。将 15mm 长的 cork pellet(软木颗粒)插入含有 15mL 水样的小瓶中,水样的 pH 值为 3,NaCl 的浓度为 25%(w/v)。在搅拌下进行萃取步骤 45 分钟,然后用 120μL 的甲醇:乙腈(1:1 v/v)进行 30 分钟的液体洗脱。对于甲基对羟基苯甲酸酯的测定,得到了令人满意的分析性能,相关系数范围为 0.9921 至 0.9994;日内精密度范围为 6.7%至 18.3%,日间精密度变化范围为 7.2%至 20.0%。通过相对回收率测定评估了准确性,范围为 53%至 124%。