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FOOD CHEMISTRY · 2024 · IF 8.5

Fabrication of fluorinated magnetic microporous organic network for selective and efficient extraction of benzoylurea insecticides in tea beverages

Hui-Ping Yu,Qian-Qian Xu,Xin Wang,Yuan-Yuan Cui,He-Fang Wang,Cheng-Xiong Yang

In this work, a novel fluorinated magnetic microporous organic network (Fe 3 O 4 @FMON) was exquisitely designed and synthesized for highly efficient and selective magnetic solid phase extraction (MSPE) of fluorinated benzoylurea insecticides (BUs) from complex tea beverage samples. The Fe 3 O 4 @FMON exhibited good extraction for BUs via the pre-designed hydrophobic, π-π stacking, hydrogen bonding and specific F F interactions. A sensitive Fe 3 O 4 @FMON-based MSPE-HPLC-UV method with wide linear range (0.10–1000 μg L −1 , R 2  ≥ 0.996), low limits of detection (0.01–0.02 μg L −1 ), and large enrichment factors (85.6–98.0) for BUs from tea beverage samples was developed. By decorating F elements within MON's networks, the Fe 3 O 4 @FMON characterized good hydrophobicity and chemical stability, which could be reused at least 8 times without decrease of recoveries. This work demonstrated the great prospects of Fe 3 O 4 @FMON for enriching trace BUs from complex substrates and triggered the potential of FMON for sample pretreatment of fluorinated analytes.

研究领域: 分析化学 · 环境科学 · 材料科学 · 食品科学
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JOURNAL OF CHROMATOGRAPHY A · 2022 · IF 4.601

Dispersive solid-phase extraction of non-steroidal anti-inflammatory drugs in water and urine samples using a magnetic ionic liquid hypercrosslinked polymer composite

Pengzhao Han,Kai Hu,Yuanpeng Wang,Lixin Li,Pan Wang,Weixia Zhu,Haiyan Gong,Zhenqiang Zhang,Shusheng Zhang

In this work, Friedel-Crafts alkylation was successfully applied to prepare a magnetic ionic liquid hypercrosslinked polymer composite (Fe 3 O 4 @IL-HCP), which was subsequently employed as magnetic solid-phase extraction (MSPE) adsorbent for the isolation and enrichment of trace non-steroidal anti-inflammatory drugs (NSAIDs). The developed composite was comprehensively characterized using various techniques, with the results indicating that it possessed high saturation magnetization (39.44 em g   −   1 ), large specific surface area (175 m 2 g   −   1 ), and high adsorption capacity for NSAIDs. The adsorption behavior and mechanisms were also investigated in detail. NSAIDs were adsorbed onto the Fe 3 O 4 @IL-HCP sorbent via a heterogeneous multilayer process consisting of hydrogen bonding and π-π and electrostatic interactions. Additionally, the composite's large surface area and multiple active sites enabled extraction equilibrium within 6 min. By coupling with high performance liquid chromatography (HPLC), the developed MSPE/HPLC method was applied for the determination of selected NSAIDs in water and urine samples. The developed method displayed wide linear ranges, low limits of detection (0.12–0.30 ng mL −1 and 0.15–1.5 ng mL −1 in water and urine samples, respectively), sufficient recoveries (92.8–109%), and good precision (relative standard deviations ≤ 4.6%). Thus, the findings of this work provide an appealing alternative for the extraction and determination of trace NSAIDs in environmental water and biological samples.

研究领域: 分析化学 · 环境科学 · 材料科学
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JOURNAL OF CHROMATOGRAPHY A · 2023 · IF 4.1

A magnetic solid phase extraction microfluidic chip coupled with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in aqueous samples

Yangkun Sun,Shengli Ruan,Yuanyuan Zhou,Linhao Zhao,Wenjing Xiong,Chuhui Lin,Jingjing Kuang,Fanghong Ning,Min Zhang,Hongyang Zhang,Ping Hu

In this paper, we designed and manufactured a reliable magnetic solid phase extraction (MSPE) microfluidic chip for determination of polycyclic aromatic hydrocarbons (PAHs) in water combined with gas chromatography-mass spectrometry. Sample loading, washing and elution are implemented with microinjection pump and integrated on a single chip, which reduced manual operation. Magnets were used to fix octadecyl/phenyl bifunctional Fe 3 O 4 @SiO 2 extractant to avoid the design of weir structure in extraction chamber. The whole microfluidic chip was simple and low cost. Based on the microfluidic chip extraction platform, the on-chip MSPE method for the determination of PAHs was optimized and established. The results showed that this method required only 2 mL of sample, 2 mg of extractant, and 50 μL of elution organic solvent for whole on-chip MSPE process, which was environmentally friendly and consistent with green chemistry. Method verification results were displayed which the linear range of five PAHs was between 1-100 ng/mL with good linearity (R 2 ≥ 0.9985), and the detection limits (S/N = 3) were 0.08–0.26 ng/mL. The RSDs of intra-day precision (n=6) and inter-day precision (n=9) for PAHs were less than 6.1 % and 7.2 %, respectively. Enrichment factors were determined to be 31.3–37.7. The recoveries of river water, tap water, bottle water, waste water and urine at three spiked levels were in the range of 89.9% to 113.7% and the matrix effect values were between 83.8% to 109.6%. The extraction platform has the advantages of accurate analysis, simple design and cost-effective, which is conducive to the widespread use of microfluidic chips

研究领域: 分析化学 · 环境科学 · 微流控技术 · 色谱法 · 质谱法
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Analytical Methods · 2019 ·Vol. 12 ·期 4 ·507-513 · IF 2.378

Mesoporous yolk–shell structure molecularly imprinted magnetic polymers for the extraction and detection of 17β-estradiol

Yinpeng Yang,Yuan Sun,Hang Chen,Xueping Dang,Youhong Ai,Xiaolan Liu,Huaixia Chen

Novel mesoporous yolk–shell structure magnetic molecularly imprinted polymers (MYS-MMIPs) were synthesized via surface polymerization using E2 as a template followed by chemical selective etching to remove the inorganic silica interlayer for the rapid, selective extraction and sensitive detection of 17β-estradiol (E2) in milk powder. For MYS-MMIPs, transmission electron microscopy coupled with N2 adsorption experiments confirmed the successful formation of a mesoporous yolk–shell structure. Furthermore, the thermogravimetric and recycling experiments showed the good thermal and adsorption stability of MYS-MMIPs, the magnetic properties experiment confirmed their good magnetic response, and the binding experiment indicated their selective recognition and high binding capacity (39.24 mg g−1) for E2. The obtained polymers were applied as adsorbents for the magnetic solid phase extraction (MSPE) of E2. After optimizing the MSPE conditions, an MSPE-HPLC method was developed for the determination of E2 in milk powder. The linear range was 1–300 μg kg−1 with a limit of detection of 0.33 μg kg−1. The satisfactory recoveries ranged from 88.3–102.4% and the relative standard deviations (RSDs) were lower than 5.5%. Thus, the MSPE-HPLC method has high accuracy and sensitivity for the analysis of E2 in milk samples.

研究领域: 分析化学 · 材料科学 · 环境科学 · 食品科学
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JOURNAL OF HAZARDOUS MATERIALS · 2025 · IF 11.3

Sustainable One-Pot Synthesis of Dual-Mechanism Magnetic HCPs for Classified Extraction of Trace PAHs and Quaternary Ammonium Pesticides in Environmental Waters

Xue Ma,Mengmeng Fu,Kai Hu,Li Gao,Chenchen Song,Shusheng Zhang,Renyong Zhao,Wenjie Zhao

Developing efficient and reliable adsorbents with simplified synthesis and mixed-mode performance is crucial for the accurate quantitative analysis of diverse coexisting environmental pollutants. A magnetic carboxylated hypercrosslinked organic polymer (Fe 3 O 4 /HCP-COOH) with reverse phase/cation exchange mixed-mode performance was synthesized through a two-stage process: (1) Fabrication of HCP-COOH via FeCl 3 -catalyzed Friedel-Crafts alkylation using 1,4-phenylenediacetic acid and 1,4-bis(chloromethyl)benzene; (2) In situ growth of Fe 3 O 4 nanoparticles on HCP-COOH through coprecipitation, utilizing FeCl₃ dually as polymerization catalyst and iron precursor to enhance process efficiency and waste minimization. The nanocomposite functioned as a mixed-mode sorbent for magnetic solid-phase extraction (MSPE), integrating dual retention mechanisms to selectively extract hydrophobic polycyclic aromatic hydrocarbons (PAHs) and cationic quaternary ammonium pesticides (QUATs), with subsequent analysis by GC-MS for PAHs and HPLC-MS/MS for QUATs respectively. Following optimization of adsorption pH, eluent composition, and contact time, the method exhibited high sensitivity with limits of detection (LODs) of 0.80-7.93   ng   L⁻¹ for 15 PAHs and 0.02-16.31   ng   L⁻¹ for 4 QUATs. Validation showed satisfactory recoveries of 89.5-98.3% (RSDs ≤11.2%) in snowmelt and 90.4-101.8% (RSDs ≤11.6%) in lake water (n=3), confirming practicality for simultaneous monitoring of hydrophobic and cationic contaminants in complex environmental water, offering significant advantages in multi-residue analysis for environmental monitoring applications.

研究领域: 环境化学 · 分析化学 · 材料科学 · 污染监测 · 可持续合成
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