Nathan de Souza Coelho, Helvécio Costa Menezes, Zenilda de Lourdes Cardeal
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The proposed technique, termed in-tube extraction, was developed and optimized to effectively retain PAHs and their derivatives in aqueous media, followed by GCxGC/Q-TOFMS determination. Fiber characterization, using techniques such as TG, DTG, FTIR, and SEM, confirmed the hydrophobic compounds retention properties of the PDMS. The determination method was validated, pointing to a significant advancement in the detection and analysis of PAHs in the environment, and proved effective even for traces of these compounds. The results showed that the detection limits (LOD) and quantification limits (LOQ) ranged from 0.07 ng L<sup>-1</sup> to 1.50 ng L<sup>-1</sup> and 0.33 ng L<sup>-1</sup> to 6.65 ng L<sup>-1</sup>, respectively; recovery ranged between 72 % and 117 %; and the precision intraday and interday ranged from 1 % to 20 %. The fibers were calibrated in the laboratory, with exposure times for analysis in the equilibrium region ranging from 3 to 10 days. The partition coefficients between PDMS and water were also evaluated, showing logarithm values ranging from 2.78 to 5.98. The fibers were applied to the analysis of real water samples, demonstrating high capacity. 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引用次数: 0
摘要
鉴于多环芳烃(PAHs)在大气中的扩散以及在水体和土壤中的沉积,多环芳烃污染是一个亟待解决的环境问题。这些化合物及其硝化和含氧衍生物可能表现出很高的毒性,在环境分析中被列为优先考虑的对象。随着对精确分析技术的需求,二维色谱-质谱联用技术(GCxGC/Q-TOFMS)已成为一种前景广阔的工具,尤其是在面临共洗脱等挑战时。本研究采用一种基于聚二甲基硅氧烷(PDMS)的萃取纤维,在多环芳烃的预浓缩和检测方面进行了创新,具有更高的稳定性和多功能性。所提出的技术称为管内萃取,经过开发和优化,可有效保留水介质中的多环芳烃及其衍生物,然后进行 GCxGC/Q-TOFMS 检测。使用 TG、DTG、FTIR 和 SEM 等技术对纤维进行表征,证实了 PDMS 的疏水化合物保留特性。该测定方法经过验证,表明在检测和分析环境中的多环芳烃方面取得了重大进展,即使对痕量的这些化合物也证明是有效的。结果表明,检测限(LOD)和定量限(LOQ)分别为 0.07 ng L-1 至 1.50 ng L-1 和 0.33 ng L-1 至 6.65 ng L-1;回收率为 72 % 至 117 %;日内和日间精密度为 1 % 至 20 %。纤维在实验室中进行了校准,在平衡区进行分析的暴露时间为 3 至 10 天。还对 PDMS 和水之间的分配系数进行了评估,结果显示对数值在 2.78 到 5.98 之间。这种纤维被应用于实际水样的分析,显示出很高的能力。此外,鉴于对可持续方法的需求日益增长,本文介绍的方法结合了绿色化学原理,为当前的化学分析方案提供了一种高效、环保的解决方案。
Development of new PDMS in tube extraction microdevice for enhanced monitoring of polycyclic aromatic hydrocarbons and their derivatives in water.
Contamination by polycyclic aromatic hydrocarbons (PAHs) is an urgent environmental concern, given its atmospheric dispersion and deposition in water bodies and soils. These compounds and their nitrated and oxygenated derivatives, which can exhibit high toxicities, are prioritized in environmental analysis contexts. Amid the demand for precise analytical techniques, comprehensive two-dimensional chromatography coupled with mass spectrometry (GCxGC/Q-TOFMS) has emerged as a promising tool, especially in the face of challenges like co-elution. This study introduces an innovation in the pre-concentration and detection of PAHs using an extraction fiber based on polydimethylsiloxane (PDMS), offering greater robustness and versatility. The proposed technique, termed in-tube extraction, was developed and optimized to effectively retain PAHs and their derivatives in aqueous media, followed by GCxGC/Q-TOFMS determination. Fiber characterization, using techniques such as TG, DTG, FTIR, and SEM, confirmed the hydrophobic compounds retention properties of the PDMS. The determination method was validated, pointing to a significant advancement in the detection and analysis of PAHs in the environment, and proved effective even for traces of these compounds. The results showed that the detection limits (LOD) and quantification limits (LOQ) ranged from 0.07 ng L-1 to 1.50 ng L-1 and 0.33 ng L-1 to 6.65 ng L-1, respectively; recovery ranged between 72 % and 117 %; and the precision intraday and interday ranged from 1 % to 20 %. The fibers were calibrated in the laboratory, with exposure times for analysis in the equilibrium region ranging from 3 to 10 days. The partition coefficients between PDMS and water were also evaluated, showing logarithm values ranging from 2.78 to 5.98. The fibers were applied to the analysis of real water samples, demonstrating high capacity. Additionally, given the growing demand for sustainable methods, the approach presented here incorporates green chemistry principles, providing an efficient and eco-friendly solution to the current chemical analysis scenario.
期刊介绍:
Talanta provides a forum for the publication of original research papers, short communications, and critical reviews in all branches of pure and applied analytical chemistry. Papers are evaluated based on established guidelines, including the fundamental nature of the study, scientific novelty, substantial improvement or advantage over existing technology or methods, and demonstrated analytical applicability. Original research papers on fundamental studies, and on novel sensor and instrumentation developments, are encouraged. Novel or improved applications in areas such as clinical and biological chemistry, environmental analysis, geochemistry, materials science and engineering, and analytical platforms for omics development are welcome.
Analytical performance of methods should be determined, including interference and matrix effects, and methods should be validated by comparison with a standard method, or analysis of a certified reference material. Simple spiking recoveries may not be sufficient. The developed method should especially comprise information on selectivity, sensitivity, detection limits, accuracy, and reliability. However, applying official validation or robustness studies to a routine method or technique does not necessarily constitute novelty. Proper statistical treatment of the data should be provided. Relevant literature should be cited, including related publications by the authors, and authors should discuss how their proposed methodology compares with previously reported methods.