Microchimica Acta ( IF 5.3 ) Pub Date : 2022-11-24 , DOI: 10.1007/s00604-022-05552-7 Lucía Abad-Gil 1 , Mayte García-Ríos 1 , Carmen Isabel-Cabrera 1 , M Jesús Gismera 1 , M Teresa Sevilla 1 , Jesús R Procopio 1
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New sensing platforms based on screen-printed carbon electrodes modified with composites based on polystyrene sulfonate and oxidized multi-walled carbon nanotubes (PSS/MWCNTs-COOH/SPCE) have been used to develop a novel HPLC method with electrochemical detection (ECD) for the determination of the most used synthetic phenolic antioxidants in cosmetics: butylhydroxytoluene (BHT), butylhydroxyanisole (BHA), tert-butylhydroquinone (TBHQ) and propyl gallate (PG). Optimal separation conditions were achieved using methanol: 0.10 mol L−1 acetate solution at pH 6 as mobile phase with a gradient elution program from 60 to 90% of methanol percentage in 15 min. The electrochemical detection was carried out in amperometric mode using the PSS/MWCNTs-COOH/SPCE at + 0.80 V vs. Ag. Under these optimal separation and detection conditions, the limits of detection (LOD) were between 0.11 and 0.25 mg L−1. These LOD values were better, especially for BHT, than those previously published in other HPLC methods. Linear ranges from 0.37 mg L−1, 0.83 mg L−1, 0.69 mg L−1 and 0.56 mg L−1 to 10 mg L−1 were obtained for PG, TBHQ, BHA and BHT, respectively. RSD values equal or lower than 5% and 8% were achieved for repeatability and reproducibility, respectively. The HPLC-ECD method was successfully applied to analyze different cosmetic samples. Recovery values within 83–109% were obtained in the validation studies.
Graphical Abstract
中文翻译：
MWCNTs-COOH/PSS 纳米复合材料修饰的丝网印刷电极，用于 HPLC 安培检测法测定合成酚类抗氧化剂
基于聚苯乙烯磺酸盐和氧化多壁碳纳米管 (PSS/MWCNTs-COOH/SPCE) 复合材料改性的丝网印刷碳电极的新型传感平台已被用于开发一种具有电化学检测 (ECD) 的新型 HPLC 方法，用于化妆品中最常用的合成酚类抗氧化剂的测定：丁基羟基甲苯 (BHT)、丁基羟基茴香醚 (BHA)、叔丁基对苯二酚 (TBHQ) 和没食子酸丙酯 (PG)。使用甲醇达到最佳分离条件：0.10 mol L −1pH 6 的乙酸盐溶液作为流动相，梯度洗脱程序在 15 分钟内从 60% 到 90% 的甲醇百分比。电化学检测使用 PSS/MWCNTs-COOH/SPCE 在安培模式下在 + 0.80 V vs. Ag 下进行。在这些最佳分离和检测条件下，检测限 (LOD) 介于 0.11 和 0.25 mg L -1之间。这些 LOD 值比以前在其他 HPLC 方法中发表的值更好，尤其是 BHT。线性范围为 0.37 mg L −1、0.83 mg L −1、0.69 mg L −1和 0.56 mg L −1至 10 mg L −1分别获得了 PG、TBHQ、BHA 和 BHT。重复性和再现性的 RSD 值分别等于或低于 5% 和 8%。HPLC-ECD 方法成功应用于分析不同的化妆品样品。在验证研究中获得了 83–109% 的回收率值。
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