Faculty of Chemistry and Petroleum Sciences, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
Chemistry and Process Department, Niroo Research Institute, Tehran, Iran.
Mikrochim Acta. 2019 Aug 2;186(9):597. doi: 10.1007/s00604-019-3698-9.
The authors describe the synthesis of a magnetic metal-organic framework (MOF) of type MIL-53(Fe) for coextraction of phenols and anilines from various environmental samples. A quick method for dispersive micro-solid phase extraction (D-μ-SPE) was developed for coextraction of the analytes 4-nitrophenol (4-NP), 4-chlorophenol (4-CP), 4-chloroaniline (4-CA), 1-amino-2-naphtol (1-A2N) and 2, 4-dichloroaniline (2, 4-DCA). The MOF was characterized by SEM, TEM, FT-IR, EDS, thermogravimetry, VSM and XRD. The method was optimized by response surface methodology combined with desirability function approach, specifically with respect to pH value of the sample, amount of sorbent, sorption time, salt concentration, sample volume, type and volume of the eluent, and elution time. Following elution with acetonitrile, the analytes were quantified by HPLC with photodiode array detection. Responses are linear in 0.1-2000 μg·L concentration ranges. The limits of detection and relative standard deviations (for n = 5) are in the range of 0.03-0.2 μg·L and 3.5-12.6%, respectively. Enrichment factors are 113, 61, 87, 144 and 114 for 4-NP, 4-CP, 4-CA, 1-A2N and 2,4-DCA, respectively. Recoveries from spiked samples ranged from 39.5 to 93.3%. The magnetic sorbent was successfully applied to the coextraction and determination of the analytes in river, rain and hookah water samples. Graphical abstract Schematic presentation for the synthesis of (a) FeO nanoparticles (NPs) and (b) FeO@MIL-53(Fe). FeO@MIL-53(Fe) was employed as a new nanosorbent in dispersive micro-solid phase extraction of phenols and anilines. The limits of detection are in the range of 0.03-0.2 μg·L.
作者描述了一种磁性金属有机骨架（MOF）MIL-53(Fe) 的合成方法，用于从各种环境样品中同时萃取酚类和苯胺类物质。开发了一种快速的分散固相微萃取（D-μ-SPE）方法，用于同时萃取分析物 4-硝基苯酚（4-NP）、4-氯苯酚（4-CP）、4-氯苯胺（4-CA）、1-氨基-2-萘酚（1-A2N）和 2,4-二氯苯胺（2,4-DCA）。MOF 采用 SEM、TEM、FT-IR、EDS、热重分析、VSM 和 XRD 进行了表征。该方法通过响应面法结合理想函数法进行了优化，具体涉及样品的 pH 值、吸附剂的量、吸附时间、盐浓度、样品体积、洗脱剂的类型和体积以及洗脱时间。用乙腈洗脱后，用高效液相色谱-光电二极管阵列检测法对分析物进行定量。响应值在 0.1-2000μg·L 的浓度范围内呈线性。检测限和相对标准偏差（n=5）的范围分别为 0.03-0.2μg·L 和 3.5-12.6%。4-NP、4-CP、4-CA、1-A2N 和 2,4-DCA 的富集因子分别为 113、61、87、144 和 114。从加标样品中的回收率为 39.5-93.3%。磁性吸附剂成功应用于河流、雨水和水烟水中分析物的同时萃取和测定。
