Controllable synthesis of uniform flower-shaped covalent organic framework microspheres as absorbent for solid-phase extraction of trace 2,4-dichlorophenol

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchimica Acta Pub Date : 2024-01-13 DOI:10.1007/s00604-024-06178-7

Guangping Xia, Haoyun Hu, Yipeng Huang, Guihua Ruan

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Abstract

Controllable synthesis of micro-flower covalent organic frameworks (MFCOFs) with controllable size, monodisperse, spherical, and beautiful flower shape was realized by using 2,5-diformylfuran (DFF) and p-phenylenediamine (p-PDA) as building blocks at room temperature. High-quality MFCOFs (5 − 7 μm) were synthesized by controlling the kind of solvent, amounts of monomers, catalyst content, and reaction time. The synthesized MFCOFs possessed uniform mesopores deriving from the intrinsic pores of frameworks and wide-distributed pores belonging to the gap between the petals. The MFCOFs-packed solid-phase extraction (SPE) column shows adsorption capacity of about 8.85 mg g⁻¹ for 2,4-dichlorophenol (2,4-DCP). The MFCOF-based SPE combined with the HPLC method was established for the determination of 2,4-DCP in environmental water. The linear range of this method is 20–1000 ng mL⁻¹ (R² > 0.9994), and limit of detection (S/N = 3) is 10.9 ng mL⁻¹. Spiked recoveries were 94.3–98.5% with relative standard deviations lower than 2.3%.

Graphical Abstract

Abstract Image

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可控合成均匀的花形共价有机框架微球，作为固相萃取痕量 2,4 二氯苯酚的吸收剂。

以 2,5-二甲酰基呋喃（DFF）和对苯二胺（p-PDA）为构筑基块，在室温下实现了尺寸可控、单分散、球形和美丽花朵形状的微花共价有机框架（MFCOFs）的可控合成。通过控制溶剂种类、单体用量、催化剂含量和反应时间，合成了高质量的 MFCOFs（5 - 7 μm）。合成的 MFCOFs 具有源自框架固有孔隙的均匀中孔和属于花瓣间隙的宽分布孔隙。MFCOFs填料固相萃取（SPE）柱对2,4-二氯苯酚（2,4-DCP）的吸附容量约为8.85 mg g-1。建立了基于 MFCOF 的固相萃取与高效液相色谱相结合的方法，用于测定环境水体中的 2,4-二氯苯酚。该方法的线性范围为 20-1000 ng mL-1 (R2 > 0.9994)，检出限（S/N = 3）为 10.9 ng mL-1。加标回收率为 94.3%-98.5%，相对标准偏差小于 2.3%。

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来源期刊

Microchimica Acta 化学-分析化学

CiteScore

9.80

自引率

5.30%

发文量

410

审稿时长

2.7 months

期刊介绍： As a peer-reviewed journal for analytical sciences and technologies on the micro- and nanoscale, Microchimica Acta has established itself as a premier forum for truly novel approaches in chemical and biochemical analysis. Coverage includes methods and devices that provide expedient solutions to the most contemporary demands in this area. Examples are point-of-care technologies, wearable (bio)sensors, in-vivo-monitoring, micro/nanomotors and materials based on synthetic biology as well as biomedical imaging and targeting.