Centro de Química Estrutural, Faculdade de Ciências, Universidade de Lisboa, 1749-016 Lisboa, Portugal.
Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade de Lisboa, 1749-016 Lisboa, Portugal.
Molecules. 2020 May 2;25(9):2133. doi: 10.3390/molecules25092133.
In the present work we propose, for the first time, bar adsorptive microextraction coated with carbon-based phase mixtures, followed by microliquid desorption and high performance liquid chromatography-diode array detection (BAμE-μLD/HPLC-DAD) analysis, to enhance the performance of the determination of traces of benzotriazoles (BTRs), benzothiazoles (BTs), and benzenesulfonamide derivatives (BSDs) in environmental water matrices. Assessing six carbon-based sorbents (CA1, CN1, B test EUR, SX PLUS, SX 1, and R) with different selectivity properties allowed us to tailor the best phase mixture (R, 12.5%/CN1, 87.5%) that has convenient porosity, texture, and surface chemistry (pH ~6.5) for trace analysis of benzenesulfonamide, 1-hydroxybenzotriazole, 1-benzotriazole, 5-methyl-1-benzotriazole, benzothiazole, and 1,3-benzothiazol-2-ol chemicals in aqueous media. Optimized experimental conditions provided average recoveries ranging from 37.9% to 59.2%, appropriate linear dynamic ranges (5.0 to 120.0 µg L; ≥ 0.9964), limits of detection between 1.0 and 1.4 μg L, and good precisions (relative standard deviation (RSD) ≤ 9.3%). The proposed methodology (BAμE(R, 12.5%/CN1, 87.5%)-μLD/HPLC-DAD) also proved to be a suitable sorption-based static microextraction alternative to monitor traces of BTRs, BTs, and BSDs in rain, waste, tap, and estuarine water samples. From the data obtained, the proposed approach showed that the BAμE technique with the addition of lab-made devices allows users to adapt the technique to use sorbents or mixtures of sorbents with the best selectivity characteristics whenever distinct classes of target analytes occur simultaneously in the same application.
在本工作中，我们首次提出了基于碳的混合相涂层的棒吸附微萃取（BAμE），随后进行微液解吸和高效液相色谱-二极管阵列检测（HPLC-DAD）分析，以增强痕量苯并三唑（BTRs）、苯并噻唑（BTs）和苯磺酰胺衍生物（BSDs）在环境水样中的测定性能。评估六种具有不同选择性的碳基吸附剂（CA1、CN1、B 测试 EUR、SX PLUS、SX 1 和 R），使我们能够定制最佳的相混合物（R，12.5%/CN1，87.5%），该混合物具有方便的孔隙率、结构和表面化学性质（pH~6.5），适用于痕量分析苯磺酰胺、1-羟基苯并三唑、1-苯并三唑、5-甲基-1-苯并三唑、苯并噻唑和 1,3-苯并噻唑-2-醇等在水介质中的化学物质。优化的实验条件提供了 37.9%至 59.2%的平均回收率、适当的线性动态范围（5.0 至 120.0 µg L；≥0.9964）、检测限在 1.0 和 1.4 µg L 之间，以及良好的精密度（相对标准偏差（RSD）≤9.3%）。所提出的方法（BAμE（R，12.5%/CN1，87.5%）-μLD/HPLC-DAD）也被证明是一种合适的基于吸附的静态微萃取替代方法，可用于监测雨水、废水、自来水和河口水中 BTRs、BTs 和 BSDs 的痕量。从获得的数据来看，所提出的方法表明，BAμE 技术加上自制的装置，允许用户根据不同目标分析物类别同时出现在同一应用中时，使用具有最佳选择性特征的吸附剂或吸附剂混合物来适应该技术。
