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MSPE
ANALYTICAL LETTERS · 2021 · IF 2.329

Reduced Graphene Oxide Nanoribbons for the Magnetic Solid-Phase Extraction (MSPE) of Bisphenol Endocrine Disruptors in Carbonated Beverages with Determination by High-Performance Liquid Chromatography with Ultraviolet Detection (HPLC-UV)

Ya-Wen Ding,Shi-Lan Feng,Juan Chen

A novel magnetic reduced graphene oxide nanoribbons (Fe3O4 @RGONRs) composite was prepared and applied as an adsorbent of magnetic solid-phase extraction (MSPE) for the determination of four bisphenol endocrine disrupters in three carbonated beverages coupled with high-performance liquid chromatography (HPLC). The prepared Fe3O4@RGONRs composite was characterized by transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, vibrating sample magnetometry, nitrogen adsorption-desorption isotherms and zeta potential analysis. Fe3O4@RGONRs composite possessed an abundant π-electron system and interacted with the analytes by π-π stacking, hydrophobic interactions, and hydrogen bond. The MSPE parameters, including the mass of adsorbent, sample solution pH, extraction time, ionic strength, desorption solvent and desorption time, were evaluated. Under the optimal conditions, the proposed Fe3O4@RGONRs-based MSPE method exhibited good linearity with determination coefficients (R2) between 0.9994 and 1000 from 1.6 to 1000 µg L−1, low limits of detection from 0.33 to 0.87 µg L−1, and suitable accuracy with spiked recoveries from 81.88% to 115.73%. The excellent analytical performance, along with suitable batch-to-batch reproducibility and reusability, suggest potential applications in the field of sample pretreatment.

CAS / MDL: 115-39-9 1478-61-1
研究领域: 分析化学 · 环境科学
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Solvent and monomer regulation synthesis of core-shelled magnetic β-cyclodextrin microporous organic network for efficient extraction of estrogens in biological samples prior to HPLC analysis

Chun-Ying Xu,Chang-Qing Zhen,Yu-Jing He,Yuan-Yuan Cui,Cheng-Xiong Yang

The abnormal estrogens levels in human body can cause many side effects and diseases, but the quantitative detection of the trace estrogens in complex biological samples still remains great challenge. Here we reported the fabrication of a novel core-shell structured magnetic cyclodextrin microporous organic network (Fe 3 O 4 @CD-MON) for rapid magnetic solid phase extraction (MSPE) of four estrogens in human serum and urine samples prior to HPLC-UV determination. The uniform spherical core-shell Fe 3 O 4 @CD-MONs was successfully regulated by altering the reactive monomers and solvents. The Fe 3 O 4 @CD-MONs owned high specific surface area, good hydrophobicity, large superparamagnetism, and abundant extraction sites for estrogens. Under optimal conditions, the proposed MSPE-HPLC-UV method provided wide linearity range (2.0–400 μg L −1 ), low limits of detection (0.5–1.0 μg L −1 ), large enrichment factors (183–198), less adsorbent consumption (3 mg), short extraction time (3 min), and good stability and reusability (at least 8 cycles). The established method had also been successfully applied to the enrichment and detection of four estrogens in serum and urine samples with a recovery of 88.4–105.1 % and a relative standard deviation of 1.0–5.9 %. This work confirmed the feasibility of solvent and monomer regulation synthesis of Fe 3 O 4 @CD-MON composites, and revealed the great prospects of magnetic CD-MONs for efficient enrichment of trace estrogens in complex biological samples.

研究领域: 分析化学 · 材料科学 · 生物医学工程
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FOOD CHEMISTRY · 2022 · IF 9.231

Fast extraction of aflatoxins, ochratoxins and enniatins from maize with magnetic covalent organic framework prior to HPLC-MS/MS detection

Dan Wei,Ao Pan,Can Zhang,Ming Guo,Chaoyan Lou,Ju Zhang,Huizhen Wu,Xu Wang

A simple, rapid and sensitive vortex-assisted magnetic solid phase extraction (MSPE) method using core–shell structured magnetic covalent organic frameworks (Fe 3 O 4 /COF-TpBD) as adsorbents was established for simultaneous determination of aflatoxins, ochratoxins and enniatins in maize before high-performance chromatography tandem spectrometry detection. Fe 3 O 4 /COF-TpBD was facilely fabricated, characterized, and applied for simultaneous extraction of ten mycotoxins from maize. Key parameters affecting MSPE efficiency were investigated. The method possessed good linearity (0.05–50 μg/kg), high sensitivity (0.02–1.67 µg/kg for limits of detection), and satisfactory recoveries (73.8–105.3 %), with relative standard deviations less than 8.5 %. The amount of adsorbent used (5 mg) and the time required (0.5 min each for adsorption and for desorption) for MSPE were greatly shortened in comparison with the previous reports. Therefore, the fabricated Fe 3 O 4 /COF-TpBD exhibited a great potential for rapid extraction of common mycotoxins in maize, which can be attributed to its multiple interactions with the target mycotoxins.

研究领域: 分析化学 · 食品安全 · 真菌毒素分析
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MICROCHEMICAL JOURNAL · 2020 · IF 3.594

Facile preparation of novel COFs functionalized magnetic core-shell structured nanocomposites and used for rapid detection of trace polycyclic aromatic hydrocarbons in food

Jian Chen,Na Li,Jianghua Liu,Fuping Zheng

A facile and rapid magnetic solid phase extraction (MSPE) based on magnetic covalent organic framework and coupled with high performance liquid chromatography diode array detection (HPLC-DAD) has been developed for detection of 11 kind of polycyclic aromatic hydrocarbons (PAHs) in food samples. In this paper, the novel magnetic core-shell structured (Fe 3 O 4 @COFs) nanocomposites were consisted with the magnetic Fe 3 O 4 nanoparticles (NPs) as a core, and 1,3,5-tris (4-aminophenyl) benzene (TAPB) and 2,5-dihydroxyterephthalaldehyde (DP) as two ligands for building shell outside of the core. These new nanocomposites were applied as superior adsorbent to enrich the PAHs due to their merits of large specific surface area, highly porosity and excellent thermal stability. The conditions that may affect the enrichment efficiency in MSPE process, including desorption solvent, amount of sorbent , extraction time, desorption time and desorption adsorption volume were investigated systematically. By combining MSPE with HPLC-DAD, an effective method for the detection of trace PAHs was successfully developed, which exhibited good linearity with R 2 ranging from 0.9954 to 0.9988, satisfactory recoveries in the range of 83.2–119.3%, and the relative standard deviations (RSD) was lower than 5.8%. In addition, the proposed MSPE-HPLC-DAD method was shown excellent ability to enrich trace PAHs effectively in food samples and potential application in extract other aromatic compounds .

研究领域: 分析化学 · 材料科学 · 环境科学 · 食品科学
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NEW JOURNAL OF CHEMISTRY · 2022 ·Vol. 46 ·期 24 ·11927-11933 · IF 3.925

Preparation, characterization and application of double yolk–shell structure magnetic molecularly imprinted polymers for extraction of 17β-estradiol

Hui Lyu,Xinze Wu,Yinpeng Yang,Huaixia Chen,Xueping Dang,Xiaolan Liu

Novel double yolk–shell structure molecularly imprinted polymers were synthesized by surface polymerization with 17β-estradiol as the template, followed by chemical etching. The prepared polymers were characterized by transmission electron microscopy, nitrogen adsorption–desorption experiments, thermal gravimetric analysis and magnetic property experiments. For 17β-estradiol, the double yolk–shell structure showed a 60% improvement in the binding capacity compared to the single layer structure, and the cycle life was at least 18 times. The obtained polymers were applied as the adsorbent for magnetic solid-phase extraction (MSPE) for 17β-estradiol. Under the optimal conditions, an MSPE-HPLC method was developed for the detection of 17β-estradiol in milk powder. A wide linearity range of 0.3–300 μg kg−1 (R2 = 0.9997) for 17β-estradiol was obtained, and the limit of detection was 0.1 μg kg−1. Satisfactory recoveries ranged from 92.50% to 101.1% and relative standard deviations were lower than 6.1%. The established MSPE-HPLC method has been proven to be accurate for the analysis of 17β-estradiol in milk powder.

研究领域: 材料科学 · 分析化学 · 环境科学 · 食品科学
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Synthesis of magnetic covalent organic framework composites for effective extraction of benzimidazole fungicides from food samples

Jie Zhao,Zi-Yu Li,Ting Cheng,Yan-Xin Chen,Cong Dai,Jia-Hui Zhu,Yu-Shen Liu,Lu-Liang Wang

Benzimidazoles (BZDs) are widely applied and easily accumulated through the food chain and endanger human health. Effective sample pre-treatment technology is the key procedure for trace BZDs analysis. Herein, magnetic covalent organic frameworks (Fe 3 O 4 @TRITER) nanospheres , as magnetic solid-phase extraction (MSPE) adsorbent, were synthesized and well characterized. The efficient extraction of BZDs residues depended on large specific surface of COFs and π-π and hydrophobic interactions between TRITER shell and BZDs. Under the optimal MSPE conditions, the developed MSPE-HPLC based on Fe 3 O 4 @TRITER method for BZDs residues afforded good linearities (0.01–1 μg mL −1 ) with R 2 (≥0.996) and low limit of detections (3 ng mL −1 ). The developed Fe 3 O 4 @TRITER based MSPE-HPLC method was evaluated and successfully applied to determine BZDs residues in orange juice, mixed juice drink and cucumber with satisfactory recoveries (76.9–117 %) and relative standard deviations (0.10–7.90 %).

研究领域: 分析化学 · 食品科学 · 材料科学
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JOURNAL OF CHROMATOGRAPHY A · 2019 · IF 3.858

Solid phase “on-situ” quadraplex isotope dimethyl labeling for the analysis of biogenic amines in beers by liquid chromatography-high resolution mass spectrometry

Enming Miao,Nazhen Zhang,Shiwei Lu,Yufeng Hu,Lin Fu,Hao Zhou,Jingjing Zhan,Minghuo Wu

A simple magnetization method was developed for the preparation of magnetic materials from conventional solid phase packing though coprecipitation and solvothermal approaches. And the prepared magnetic materials were used for magnetic solid phase extraction (MSPE) of biogenic amines (BAs) from beers. Furthermore, to improve the analytical throughput, a solid phase “on-situ” quadraplex isotope dimethyl labeling method was developed for the quantification of BAs by liquid chromatography-high resolution mass spectrometry (LC HRMS). Compared to conventional in-solution labeling, the “on-situ” labeling could simplify the sample preparation procedure and efficiently remove the residuals such as inorganic salts and excessive labeling reagents. The quadraplex labeling, which enabled three real samples and one internal standard sample to be analyzed simultaneously in a single LC HRMS run. For the tested 8 BAs (cadaverine, phenethylamine, spermine, spermidine, tyramine, histamine, putrescine and tryptamine), LODs of 0.02–0.05 μg/L and LOQs of 0.05–0.1 μg/L were achieved at good reproducibility (RSD of 0.5–4.6% and 2.2–7.0% for intra- and inter-day reproducibility, respectively). With this method, six beer samples were analyzed, and these 8 BAs were all detected in the range of low μg/L to 2.9 mg/L, which were lower than maximal residual level (MRL) required in the regulations of China and EU.

研究领域: 分析化学 · 食品科学 · 质谱分析
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BIOINORGANIC CHEMISTRY AND APPLICATIONS · 2022 · IF 4.724

Synthesis of the Magnetically Nanoporous Organic Polymer Fe3O4@SiO2-NH2-COP and Its Application in the Determination of Sulfonamide Residues in Surface Water Surrounding a Cattle Farm

Yuqin Yang,Junjie Miao,Zhendong Yin,Weili Hao,Hongmei Shi,Ling Ma,Tiesheng Shi

Efficient extractions of trace antibiotic residues in the environment are a key factor for accurate quantification of the residues. A new nanoporous material, namely, magnetically covalent organic polymer (MCOP, Fe3O4@SiO2-NH2-COP) was synthesized in this work and was used for magnetic solid-phase extraction (MSPE). The combination of MSPE with high-performance liquid chromatography separation together with ultraviolet detection (HPLC-UV) was established as an effective method for the determination of four sulfonamide (SA) residues in surface water surrounding a cattle farm. The synthesized magnetic material was characterized by SEM, TEM, FT-IR, magnetic properties measurement system (MPMS), and nitrogen gas porosimetry. The material possessed many attractive features, such as a unique microporous structure, a larger specific surface area (137.93 m2·g−1) than bare Fe3O4 (24.84 m2·g−1), high saturation magnetization (50.5 emu·g−1), open adsorption sites, and high stability. The influencing parameters, including pH, the used amount of MCOPs, the type of eluent, adsorption solution, and desorption time, were optimized. Under the optimized conditions, the method conferred good linearity ranges (R2 ≥ 0.9990), low detection limits (S/N = 3, LOD, 0.10–0.25 μg·L−1), and satisfactory recoveries (79.7% to 92.2%). The enrichment factor (EF) for the four SAs was 34.13–38.86. The relative standard deviations of intraday (n = 5) and of interday (n = 3) were less than 4.8% and 8.9%, respectively. The equilibria between extraction and desorption for SAs could be reached within 150 s. The proposed method was sensitive and convenient for detecting SA residues in complex environmental matrices, and the successful application of the new MCOPs as an adsorbent was demonstrated.

研究领域: 环境科学 · 分析化学 · 材料科学 · 水质
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JOURNAL OF CHROMATOGRAPHY A · 2019 · IF 3.858

Preparation of magnetic porous covalent triazine-based organic polymer for the extraction of carbamates prior to high performance liquid chromatography-mass spectrometric detection

Xiaolan Wang,Tao Feng,Juntao Wang,Lin Hao,Chun Wang,Qiuhua Wu,Zhi Wang

A magnetic porous covalent triazine-based organic polymer (M-PCTP) was synthesized by co-precipitation method. The M-PCTP combined both the properties of the PCTP and the magnetism of Fe 3 O 4 nanoparticles, possessing highly porous structure and good magnetism. It was used as a magnetic solid phase extraction (MSPE) adsorbent to extract carbamate pesticides (propoxur, carbaryl, isoprocarb, fenobcarb and diethofencarb) from lemonade and grape juice samples prior to high performance liquid chromatography-mass spectrometric detection. Under the optimal conditions, a good linearity for the real samples was received in the range from 0.10–0.90 to 80.00 ng mL −1 with the correlation coefficients of 0.9882–0.9983. The method recoveries for the five carbamates were 86.3–108.0%. The limits of detection were 0.02–0.20 ng mL −1 for lemonade sample, and 0.04-0.30 ng mL −1 for grape juice sample. The M-PCTP also demonstrated good extraction capabilities for other different kinds of organic compounds including chlorophenols and polycyclic aromatic hydrocarbons.

研究领域: 分析化学 · 环境科学 · 材料科学 · 食品科学
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MICROCHEMICAL JOURNAL · 2025 · IF 5.1

An environmentally friendly cucurbit[7]uril-mediated magnetic-assisted matrix solid-phase dispersion extraction combined with HPLC-MS/MS for multiple analysis of pharmaceuticals and personal care products in aquatic organisms

Huiyu He,Rui Wang,Rongbin Nie,Nan Dong

Trace amounts of pharmaceuticals and personal care products (PPCPs) in aquatic environment poses a non-negligible risk to human health. Here, an environmentally friendly cucurbit[7]uril-mediated magnetic-assisted matrix solid phase dispersion (Q[7]- m -MSPD) extraction method was developed for extracting PPCPs from complex aquatic organisms. The extraction of PPCPs were achieved via the host-guest interaction between Q[7] and targets, significantly reducing the matrix interference. Gold magnetic nanoparticles (AuMNPs) were chelated to Q[7]-target complexes and used for purification and enrichment via magnetic solid-phase extraction (MSPE), effectively replacing the complex operation of sample loading and elution on SPE columns in MSPD. Coupled with high performance liquid chromatography-tandem mass spectrometry, multiple analysis of 14 PPCPs in 3 aquatic plants and an aquatic animal were achieved, with detection limits ranging from 0.0015 to 0.0179 μg/kg, recoveries ranging from 71.06 to 113.6 %, and enrichment factors within 46 to 152. The green chemistry assessment confirmed the environmental friendliness, economic feasibility, and application potential of the Q[7]- m -MSPD, with an AGREE score of 0.63 and a BAGI score of 72.5. By integrating the merits of MSPD and MSPE, the proposed approach exhibited high sensitivity and anti-interference capability, simple operation, and great environmental friendliness. Therefore, the approach provided a green method for simultaneously detecting multiple hazardous residues in complex matrices owing to the broad-spectrum molecular recognition capability of Q[7] , which has a good application prospect in food safety and environmental monitoring.

研究领域: 分析化学 · 环境科学 · 绿色化学 · 食品安全 · 药物分析 · 生物分析化学
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TALANTA · 2020 · IF 5.339

Determination of estrogens by solid-phase quadruplex stable isotope dansylation coupled with liquid chromatography-high resolution mass spectrometry in environmental samples

Minghuo Wu,Enming Miao,Wenxue Xu,Weiping Xu,Yufeng Hu,Jingjing Zhan,Hao Zhou

Estrogens distribute widely in the environment as endocrine-disrupting chemicals (EDCs), which have to be monitored to evaluate their environmental impact. Aim to improve the analytical throughput of liquid chromatography-high resolution mass spectrometry (LC-HRMS), a quadruplex stable isotope dansylation method was developed, with which three real samples could be quantitatively analyzed in one injection. As the estrogens were at trace level in complex matrices, magnetic solid-phase extraction (MSPE) was applied to enrich these analytes and remove the interfaces. By integrating MSPE and quadruplex stable isotope dansylation, a solid-phase quadruplex labeling method was developed for the LC-HRMS analysis of estrogen analogues . For the tested seven estrogens, the developed method showed low detection limits (0.1–0.5 ng/L for pond water and 0.01–0.05 μg/kg for poultry manure), good precision (RSD < 5.5%) and accuracy (96.8–108.3%). The method was applied in the determination of estrogens in environmental samples, and the results revealed that all the tested estrogens were present in the estuary water (unquantifiable to 71.2 ng/L) and chicken manure (undetectable to 25.43 μg/kg).

研究领域: 环境科学 · 分析化学 · 环境监测
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FOOD CHEMISTRY · 2024 · IF 8.5

Hydrophilic molecularly imprinted thermal-responsive polymers based sorbent for ambient ionization mass spectrometric analysis of sulfonamide antibiotics from food samples

Yaxin Hao,Minli Yang,Na Li,Yanfang Zhao,Yunshan Wang,Xiangfeng Chen,Feng Zhang

The thermal-responsive magnetic molecularly imprinted polymer (TrMMIP) sorbent was synthesized by surface imprinting method, and then used for magnetic solid-phase extraction (MSPE) and subsequent integrated into the ion source for elution and ionization. The shrinking-strength states change of the thermal-responsive polymer chain on TrMMIP alters the wettability of the sorbent when the working temperature crosses the lower critical solution temperature (LCST) of the polymer, and thus affects its behavior of in the extraction and clean-up process. The targeted analytes could be effectively extracted due to the high selectivity of MIPs and well dispersibility of polymer chain under the open state. Additionally, a hydrophilic polymer chain wrapped on the sorbent surface further protected target substances from co-elution during cleanup. Analytical methods for sulfonamide antibiotics (SAs) detection in complex food samples (milk, honey, fish) were developed, demonstrating potential for rapid and sensitive SAs analysis in diverse food and biological samples.

CAS / MDL: 78-10-4 100-68-5
研究领域: 分析化学 · 材料科学 · 环境科学 · 食品科学
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