Department of Chemistry, Iowa State University, 1605 Gilman Hall, Ames, IA 50011, USA; Ames Laboratory-USDOE, Iowa State University, 1605 Gilman Hall, Ames, IA 50011, USA.
Department of Chemistry, Iowa State University, 1605 Gilman Hall, Ames, IA 50011, USA.
J Chromatogr A. 2022 Oct 11;1681:463429. doi: 10.1016/j.chroma.2022.463429. Epub 2022 Aug 23.
In this work, hydrophobic magnetic deep eutectic solvents (HMDESs) were used in the development of a simple and rapid dispersive liquid-liquid microextraction (DLLME) approach coupled to high performance liquid chromatography with UV detection (HPLC-UV) for the determination of ten organic contaminants including five polycyclic aromatic hydrocarbons, four UV filters, and a pesticide from water at trace levels. The HMDESs were prepared by mixing a hydrogen bond acceptor, metal halide salt, and hydrogen bond donor in suitable molar ratios. Two HMDESs, 2 tetraoctylammonium bromide ([N][Br]): cobalt chloride (CoCl): 4 octanoic acid (OA) and 3 trioctylphosphine oxide (TOPO): neodymium chloride (NdCl): 3 OA, offered the highest analyte extraction efficiency overall and were chosen as suitable solvents for validation of the microextraction method. Under optimized extraction conditions, the method required 30 µL of HMDES as extraction solvent, acetone (87.5 µL) as disperser solvent, a NaCl concentration of 30% (w/v), and an extraction time of 120 s at 20°C. Enrichment factors of the analytes ranged from 44.6 for 3-(4-methylbenzylindene) camphor to 66.0 for 2-ethylhexyl-4-(dimethyl)aminobenzoate. The method provided low limits of detection (LODs) ranging from 0.5 to 4.5 µg L, and acceptable precision, with RSD values lower than 9.6%. Furthermore, the validated method was successfully applied for tap and lake water analysis, resulting in relative recoveries of spiked samples ranging between 94.7 and 119.2%.
在这项工作中，使用了疏水性磁性深共晶溶剂（HMDES）来开发一种简单快速的分散液-液微萃取（DLLME）方法，该方法与高效液相色谱法（HPLC-UV）联用，用于测定痕量水中的十种有机污染物，包括五种多环芳烃、四种紫外线滤光剂和一种农药。HMDES 是通过以合适的摩尔比混合氢键受体、金属卤化物盐和氢键供体制备而成的。两种 HMDES，即 2 四辛基溴化铵([N][Br]): 氯化钴(CoCl): 4 辛酸(OA)和 3 三辛基氧化磷(TOPO): 氯化钕(NdCl): 3 OA，总体上提供了最高的分析物萃取效率，被选为微萃取方法验证的合适溶剂。在优化的萃取条件下，该方法需要 30 μL 的 HMDES 作为萃取溶剂、87.5 μL 的丙酮（分散剂）、30%（w/v）的 NaCl 浓度和 20°C 下 120s 的萃取时间。分析物的富集因子范围为 3-(4-甲基苯亚甲基)樟脑的 44.6 到 2-乙基己基-4-(二甲氨基)苯甲酸酯的 66.0。该方法提供了低检测限（LOD），范围从 0.5 到 4.5μg L，并且具有可接受的精密度，RSD 值低于 9.6%。此外，验证后的方法成功应用于自来水和湖水分析，得到加标样品的相对回收率在 94.7%到 119.2%之间。
