关键词: Dispersive solid phase microextraction Large volume sample stacking Layered double hydroxides α-naphthol β-naphthol

Mesh : Naphthols / chemistry analysis isolation & purification Water Pollutants, Chemical / analysis isolation & purification chemistry Electrophoresis, Capillary / methods Solid Phase Microextraction / methods Limit of Detection Hydroxides / chemistry Isomerism Reproducibility of Results Hydrogen-Ion Concentration

来  源:   DOI:10.1016/j.chroma.2024.465174

Abstract:
The present work describes a quick, simple, and efficient method based on the use of layered double hydroxides (LDH) coupled to dispersive solid phase micro-extraction (DSPME) to remove α-naphthol (α-NAP) and β-naphthol (β-NAP) isomers from water samples. Three different LDHs (MgAl-LDH, NiAl-LDH, and CoAl-LDH) were used to study how the interlayer anion and molar ratio affected the removal performance. The critical factors in the DSPME procedure (pH, LDH amount, contact time) were optimized by the univariate method under the optimal conditions: pH, 4-8; LDH amount, 5 mg; and contact time, 2.5 min. The method can be successfully applied in real sample waters, removing NAP isomers even in ultra-trace concentrations. The large volume sample stacking (LVSS-CE) technique provides limits of detections (LODs) of 5.52 µg/L and 6.36 µg/L for α-naphthol and β-naphthol, respectively. The methodology\'s precision was evaluated on intra- and inter-day repeatability, with %RSD less than 10% in all cases. The MgAl/Cl--LDH selectivity was tested in the presence of phenol and bisphenol A, with a removal rate of >92.80%. The elution tests suggest that the LDH MgAl/Cl--LDH could be suitable for pre-concentration of α-naphthol and β-naphthol in future works.
摘要:
目前的工作描述了一个快速,简单,基于层状双氢氧化物(LDH)耦合分散固相微萃取(DSPME)去除水样中α-萘酚(α-NAP)和β-萘酚(β-NAP)异构体的高效方法。三种不同的LDH(MgAl-LDH,NiAl-LDH,和CoAl-LDH)用于研究层间阴离子和摩尔比如何影响去除性能。DSPME程序中的关键因素(pH,LDH量,接触时间)在最佳条件下通过单变量方法进行优化:pH,4-8;LDH量,5毫克;和接触时间,2.5min.该方法可成功应用于实际样水,即使在超痕量浓度下也能去除NAP异构体。大体积样品堆叠(LVSS-CE)技术为α-萘酚和β-萘酚提供了5.52µg/L和6.36µg/L的检测极限(LOD),分别。该方法的精度是根据日内和日间可重复性进行评估的,在所有情况下%RSD小于10%。在苯酚和双酚A存在下测试了MgAl/Cl--LDH的选择性,去除率>92.80%。洗脱测试表明,LDHMgAl/Cl--LDH可适用于未来的α-萘酚和β-萘酚的预浓缩。
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