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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2023 · IF 4.3

Magnetic solid phase extraction for the determination of Pb(II) and Cd(II) in high salt foods

Dian-Bing Zhou,Hai-Tao Zhu,Yu-Zhu Hou,Gui-Lan Shen,Can Shi,Ya-Jie Zhu,Ya-Bing Xiao,Wei Song,Yu-Xin Liu,Fang Han,Ping Zheng,Xiao-Feng Yu

The conventional method for the determination of heavy metals in food is acid digestion followed by atomic absorption spectrometry or induced coupled plasma mass spectrometry . However, for high salt foods, due to the strong matrix effect, the detection results are seriously inaccurate. In this work, sulfur-functionalized magnetic metal-organic frameworks (Fe 3 O 4 @UiO-66-SH) were synthesized by coating Fe 3 O 4 nanospheres with sulfydryl-functionalized UiO-66. The Fe 3 O 4 @UiO-66-SH possesses both the magnetic properties of Fe 3 O 4 and the diverse properties of metal-organic framework (MOF) in one material, which has the superiority of high surface area, easy-operation and strong adsorb ability with Pb (II) and Cd(II), is used to separate and determine Pb (II) and Cd(II) in high salt foods by magnetic solid phase extraction-induced plasma mass spectrometry. The detection limits (LODs) for Pb (II) and Cd(II) were 0.17 and 0.21 µg/kg, respectively, and the quantification limits (LOQs) were 0.56 and 0.66 µg/kg. Analyzing the certified reference material of soy sauce (CFAPA-QC1728–4, P41839) and estimating the spiked recoveries proved the accuracy and precision of the proposed method. The determined values agreed well with the reference values, and the recoveries for spiking sample varied from 85.8–100.5%.

CAS / MDL: 10026-11-6
研究领域: 分析化学 · 食品安全
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JOURNAL OF CHROMATOGRAPHY A · 2017 · IF 3.981

Magnetic solid–phase extraction of tetracyclines using ferrous oxide coated magnetic silica microspheres from water samples

Lili Lian,Jinyi Lv,Xiyue Wang,Dawei Lou

A novel magnetic solid–phase extraction approach was proposed for extraction of potential residues of tetracyclines (TCs) in tap and river water samples, based on Fe 3 O 4 @SiO 2 @FeO magnetic nanocomposite. Characterized results showed that the received Fe 3 O 4 @SiO 2 @FeO had distinguished magnetism and core–shell structure. Modified FeO nanoparticles with an ∼5 nm size distribution were homogeneously dispersed on the surface of the silica shell. Owing to the strong surface affinity of Fe (II) toward TCs, the magnetic nanocomposite could be applied to efficiently extract three TCs antibiotics, namely, oxytetracycline, tetracycline and chlortetracycline from water samples. Several factors, such as sorbent amount, pH condition, adsorption and desorption time, desorption solvent, selectivity and sample volume, influencing the extraction performance of TCs were investigated and optimized. The developed method showed excellent linearity (R > 0.9992) in the range of 0.133–333 μg L −1 , under optimized conditions. The limits of detection were between 0.027 and 0.107 μg L −1 for oxytetracycline, tetracycline and chlortetracycline, respectively. The feasibility of this method was evaluated by analysis of tap and river water samples. The recoveries at the spiked concentration levels ranged from 91.0% to 104.6% with favorable reproducibility (RSD < 4%).

研究领域: 环境科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Amidoxime covalent organic framework@Fe3O4 based magnetic solid-phase extraction for rapid and sensitive determination of trace uranium in seafood

Fan Bai,Xu Yang,Cheng Yang,Hai-Long Qian,Xiu-Ping Yan

The unintentional dissemination of uranium into environment poses substantial risks to both food sources and human populations. An advanced method for convenient and accurate detection of uranium in food is thus a pressing need. Herein, a novel magnetic amidoxime functionalized covalent organic framework (TpDb-AO@Fe 3 O 4 ), prepared with 2,5-dinitrobenzonitrile, 1,3,5-triformylphloroglucinol and hydroxylamine hydrochloride, was synthesized as adsorbent for magnetic-solid phase extraction (MSPE) of UO 2 2+ . Furthermore, a TpDb-AO@Fe 3 O 4 based MSPE coupled with UV–vis spectrophotometer was successfully developed to realize the determination of uranyl ions with low limit of detection of 1.63 μg L −1 , wide linear range of 10 − 200 μg L −1 . The spiking recoveries in real seafood samples (tuna, yesso scallop, kelp, eel, hairtail) ranged from 94.1 % − 106.8 %. The intraday ( n = 5) and interday ( n = 5) relative standard deviation (RSD) for determination of UO 2 2+ were 3.33 % and 6.23 %, respectively. This approach represents an advancement in the rapid extraction and sensitive quantification of trace uranium contaminants in food matrices, thereby contributing to enhanced environmental monitoring and public health safeguards.

研究领域: 环境科学 · 分析化学
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JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY · 2020 ·Vol. 324 ·期 3 ·1329-1337 · IF 1.137

Magnetic solid-phase extraction of U(VI) in aqueous solution by Fe3O4@hydroxyapatite

Zeng Dejun,Dai Ying,Zhang Zhibing,Wang Youqun,Cao Xiaohong,Liu Yunhai

In this work, the magnetic hydroxyapatite composite (Fe 3 O 4 @HAP) was prepared and used to remove of U(VI). The characterizations of transmission electron microscope and vibrating sample magnetometer indicated that the average size and saturation magnetizations ( M s ) of Fe 3 O 4 @HAP was about 360 nm and 20.89 emu g −1 , respectively. The results of solid-phase extraction indicated that at pH 5.0, the removal efficiency of Fe 3 O 4 @HAP was more than 95% within 20 min. The maximum adsorption capacity ( q m ) of Fe 3 O 4 @HAP was 789.58 mg g −1 . Therefore, Fe 3 O 4 @HAP may be a rapid and highly efficient magnetic adsorbent to remove of U(VI) from water.

CAS / MDL: 151-21-3
研究领域: 环境科学 · 材料科学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2013 ·Vol. 28 ·期 7 ·1110-1117 · IF 3.155

Ionic liquid-based magnetic solid phase extraction coupled with inductively coupled plasma-optical emission spectrometry for the determination of Cu, Cd, and Zn in biological samples

Chao Cui,Bin Hu,Beibei Chen,Man He

Ionic liquids of methyltrioctylammonium chloride modified magnetic nanoparticles were prepared, and a new method of magnetic solid phase extraction combined with inductively coupled plasma-optical emission spectrometry was established for the determination of Cu, Zn, and Cd in human hair and urine samples. The effect of pH on the extraction of Cu, Zn, and Cd was investigated. The results show that the ionic liquid played a key role in the extraction of target analytes. The magnetic nanoparticles served as the carriers of the ionic liquid and the base of the phase separation. Several parameters affecting the extraction and desorption of the target analytes were investigated including the sample volume, extraction time, eluent concentration and volume, desorption time, sedimentation time, amount of the ionic liquid and Fe3O4@Si–OH, and the optimized conditions were established. Under the optimized conditions, the detection limits of Cu, Zn, and Cd were 0.54, 0.56, and 0.33 μg L−1, respectively, and the relative standard deviations (n = 7) were 4.9% (c = 2 μg L−1), 3.7% (c = 2 μg L−1), and 5.1% (c = 1 μg L−1), respectively. To validate the accuracy of the proposed method, it was applied to analyze certified reference materials of GBW07601 human hair and GBW09103 human urine. The determined values agree with the certified values. The developed method was also employed to analyze human hair and urine, and the recoveries for the spiked samples were in the range of 89.1% to 120%. The developed method was simple, highly sensitive, solvent-free, chelate-free, and could be considered as a green analytical technique.

CAS / MDL: 5137-55-3
研究领域: 分析化学 · 环境科学
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JOURNAL OF FOOD SCIENCE · 2025 ·Vol. 90 ·期 4 ·e70215 · IF 3.4

Novel Room-Temperature-Prepared Covalent Organic Framework as Adsorbent for Rapid Extraction of Aromatic Esters in Baijiu

Yongqing Zhang,Zhen Fan,Xiaolong Shang,Ling Ao,Miao Liu,Feng Lin,Baoguo Sun,Wei Dong,Xiaotao Sun,Yanfei Xiong,Bo Deng

Developing a rapid, efficient, and environmentally friendly analytical methodology for the determination of aromatic esters (AREs) in Baijiu presents a significant challenge. In this study, we developed a room-temperature method to synthesize core-shell Fe 3 O 4 @TPB-Dha in 1 h using pre-prepared Fe 3 O 4 nanoparticles, enabling rapid and sensitive detection of AREs. The Fe 3 O 4 @TPB-Dha demonstrated exceptional adsorption capabilities (52.63–58.82 mg/g) with a brief adsorption duration (4 min) for four AREs as magnetic solid phase extraction (MSPE) adsorbent. Moreover, density functional theory (DFT) calculations revealed the key adsorption mechanisms to be hydrogen bonds, van der Waals forces, and π–π interactions. Ultimately, the method enabled the rapid and accurate quantification of the four AREs in real Baijiu samples, with concentrations spanning from 0.17 ± 6 × 10 −4 to 2.40 ± 0.03 mg/L, and exhibited relative standard deviations below 6.57% ( n = 3). These findings suggest that Fe 3 O 4 @TPB-Dha holds promise as an effective adsorbent for efficient extraction and precise quantification of aromatic esters in Baijiu.

CAS / MDL: 10025-77-1 127-09-3
研究领域: 分析化学 · 材料科学
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CHROMATOGRAPHIA · 2017 ·Vol. 80 ·期 3 ·463-471 · IF 1.402

Synthesis of Fe3O4@m-SiO2/PSA@Zr-MOF Nanocomposites for Bifenthrin Determination in Water Samples

Xu Mei,Chen Kun,Luo Chen,Song Guoxin,Hu Yaoming,Cheng Hefa

Abstract In this paper, a simple but efficient method for the extraction and analysis of bifenthrin in water samples was proposed. The Fe 3 O 4 -based nanocomposites (Fe 3 O 4 @m-SiO 2 /PSA@Zr-MOF) were successfully synthesized and developed as adsorbents for magnetic solid-phase extraction. With the solvothermal reaction and sol–gel method, the resultant adsorbents exhibited excellent characteristics of large surface areas, homogeneous pore size, strong magnetic responsivity and high hydrophilicity. The parameters affecting the extraction performance including adsorbent amounts, adsorption time, species of eluents and desorption time were investigated. Under the optimal conditions, validation experiments such as recovery, reproducibility and limits of detection (LOD) were carried out and showed satisfactory results. The LOD of the targeted analytes was found to be 0.5 μg L −1 . The average recovery was 103.2% with the intra-day and inter-day relative standard deviations of 2.0 and 3.5%, respectively. Ultimately, the novel magnetic adsorbents were successfully applied to detect the bifenthrin compound in real water samples. Graphical Abstract

研究领域: 环境科学 · 分析化学
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TALANTA · 2016 · IF 4.035

Sensitive determination of As (III) and As (V) by magnetic solid phase extraction with Fe@polyethyleneimine in combination with hydride generation atomic fluorescence spectrometry

Qingxiang Zhou,Zhenwen Zheng,Junping Xiao,Huili Fan

The magnetic nanomaterial Fe@polyethyleneimine (Fe@PEI) was successfully synthesized and used as an effective adsorbent material for magnetic solid phase extraction(MSPE) of As(III) and As(V) from water samples. Fe@SiO 2 nanoparticles were prepared by one pot synthetic method using a borohydride reduction method, then modified with (3-chloropropyl)trimethoxysilane to obtain Fe@SiO 2 -Cl by chloropropylation, which was reacted with PEI to achieve Fe@polyethyleneimine (Fe@PEI). The microstructure and morphology of Fe@PEI were characterized by transmission electron microscoscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD). The experimental results showed that Fe@PEI demonstrated excellent adsorption for As(III) and As(V). Based on this fact, the determination method for these two arsenic species earned good limits of detection (LODs) of 0.002   μg   L −1 and wide calibration curves in the concentration range from 0.008 to 0.2   μg   L −1 . The precisions of As (III) and As (V)were 1.95% and 2.55% (RSD, n =6), respectively. The proposed method was validated with real samples and the spiked recoveries were in the range of 82.7–98.3% and the accuracies were in the range of 2–13.3%. The results demonstrated that the developed MSPE method had good advantages such as simplicity, rapid separation, low cost, easy to reuse and high-quality analytical performances, which made it attractive for rapid and efficient extraction of inorganic arsenic species in the environmental water samples.

CAS / MDL: 2530-87-2 9002-98-6
研究领域: 分析化学 · 环境科学
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MICROCHEMICAL JOURNAL · 2021 · IF 4.821

Magnetic solid phase extraction based on Fe3O4@SiO2@CTS nano adsorbent for the sensitive detection of trace polychlorinated biphenyls in environmental water samples

Yu Tian,Zhigang Xu,Yuming Yang,Dan Wang,Zhimin Liu,Xiaoxi Si

In this study, a magnetic composite material was developed by bonding the modified natural polysaccharide chitosan (CTS) with SiO 2 on the surface of magnetic Fe 3 O 4 nanoparticles to detect polychlorinated biphenyls (PCBs). The structural, porosity, and magnetic properties of Fe 3 O 4 @SiO 2 @CTS were characterized by scanning electron microscopy, infrared spectroscopy, X-ray diffraction, nitrogen sorption, and vibrating sample magnetometry. Various experimental parameters affecting the extraction capacity were investigated, including extraction time, desorption time, desorption solvent, solution pH value, and salt ion concentration. Results showed that Fe 3 O 4 @SiO 2 @CTS exhibited excellent selectivity, easy separation by magnet, and reusability (at least 10 cycles). Under optimized experimental condition, this magnetic solid phase extraction material was applied to detect three PCBs with low limits of detection of 0.02–0.15 μg·L −1 . The linear correlation coefficient was higher than 0.998, while the recoveries ranged between 90.34% and 106.99% with the relative standard deviation less than 11.31%. The practical application of Fe 3 O 4 @SiO 2 @CTS was verified through quantitative analysis of PCB residues in environmental water, supporting its promising role in simple, convenient, and low-cost detection of PCBs in real environmental samples.

研究领域: 分析化学 · 环境科学
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MICROCHIMICA ACTA · 2020 ·Vol. 187 ·期 7 ·1-8 · IF 6.232

Caramelized carbonaceous shell-coated γ-Fe2O3 as a magnetic solid-phase extraction sorbent for LC-MS/MS analysis of triphenylmethane dyes

Li Nianlu,Li Ruohan,Song Yinshuang,Ma Long,Gao Cuiling,Li Lili,Cheng Shi-Bo,Zhang Xiaoli,Chen Jing,Zhan Jinhua

Carbonaceous shell-coated γ-Fe 2 O 3 nanoparticles (γ-Fe 2 O 3 @CNM) were synthesized from glucose caramelization and used as a novel magnetic solid-phase extraction medium for malachite green and crystal violet in environmental water. Malachite green and crystal violet were absorbed on to γ-Fe 2 O 3 @CNM by electrostatic and π-interactions. The morphologies, pore structures, surface functional groups, and magnetic properties of γ-Fe 2 O 3 @CNM were characterized by TEM, FTIR, hysteresis regression, Brunauer-Emmet-Teller analysis, zeta potential, XPS, and XRD. The magnetic solid-phase extraction procedure was optimized by extraction pH, absorption time, desorption solvent, and desorption time. The absorption capacities (q max values) for malachite green and crystal violet were 34.2 and 27.9 mg g −1 , respectively. After magnetic solid-phase extraction, malachite green and crystal violet were determined by LC-MS/MS. The analytical method was validated with a linear range of 0.02–20 ng mL −1 , enrichment factor of 25.8 and 25.4, method detection limit of 0.004 ng mL −1 , and intra-day precisions of 2.1% and 2.6% for malachite green and crystal violet, respectively. The relative recovery was found to be 73.4–101.5% for malachite green and 83.1–102.7% for crystal violet upon the application of the magnetic solid-phase extraction method to real water samples from lake, spring, sea, fishpond, and industrial waste. Caramelized-carbon-coated magnetic nanoparticles are used as novel extraction medium based on electrostatic and π-interactions. It is porous, amphiphilic, electronegative, magnetically strong, and features abundant absorption site. These characteristics stimulate mass transfer and result in a useful MSPE method in environmental analysis.

研究领域: 分析化学 · 环境科学
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TALANTA · 2016 · IF 4.035

Metal organic frameworks (MOFs) for magnetic solid-phase extraction of pyrazole/pyrrole pesticides in environmental water samples followed by HPLC-DAD determination

Jiping Ma,Zhidan Yao,Liwei Hou,Wenhui Lu,Qipeng Yang,Jinhua Li,Lingxin Chen

Magnetic metal-organic frameworks (MOFs, [MIL-101]) were prepared and used as magnetic solid-phase extraction (MSPE) adsorbents for preconcentration of four kinds of pyrazole/pyrrole pesticides (flusilazole, fipronil , chlorfenapyr , and fenpyroximate) in environmental water samples, followed by high-performance liquid chromatography-diode-array detector (HPLC-DAD) determination. Several variables affecting MSPE efficiency were systematically investigated, including amount of MIL-101, extraction time, sample pH, salt concentration, type of desorption solvent and desorption number of times. Under optimized conditions, excellent linearity was achieved in the range of 5.0–200.0   μg/L for flusilazole and fipronil, and 2.0–200.0   μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients r >0.9911. Limits of detection and quantification were 0.3–1.5   μg/L and 1.0–5.0   μg/L, respectively. The intra-day and inter-day precision (relative standard deviation, n =6, %) at three spiked levels were 1.1–5.4% and 3.9–7.8% in terms of peak area, respectively. The method recoveries at three fortified concentration levels ranged from 81.8% to 107.5% for reservoir water samples, 81.0–99.5% for river water samples, and 80.2–106.5% for seawater samples. The developed MOFs based MSPE coupled with HPLC method proved to be a convenient, rapid and eco-friendly alternative to the sensitive determination of pyrazole/pyrrole pesticides with high repeatability and excellent practical applicability.

CAS / MDL: 68-12-2
研究领域: 环境科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2017 · IF 3.981

Magnetic solid phase extraction of typical polycyclic aromatic hydrocarbons from environmental water samples with metal organic framework MIL-101 (Cr) modified zero valent iron nano-particles

Qingxiang Zhou,Man Lei,Yalin Wu,Yongyong Yuan

Metal-organic framework material has been paid more attention because of its good physical and chemical properties. Nanoscale zero valent iron is also in the center of concern recently. Combination of their merits will give impressive results. Present study firstly synthesized a new magnetic nanomaterial nano-scale zero valent iron-functionalized metal-organic framworks MIL-101 (Fe@MIL-101) by co-precipitation method. The morphology and structure of the as-prepared Fe@MIL-101 were characterized by transmission electron microscopy and X-ray diffraction, etc. The experimental results showed that Fe@MIL-101 earned good adsorption ability to polycyclic aromatic hydrocarbons. The limits of detection of developed magnetic solid phase extraction were all below 0.064   μg   L −1 and precision can be expressed as relative standard deviation (RSD, %) and which was better than 4.4% (n   =   6). The real water analysis indicated that the spiked recoveries were satisfied, and Fe@MIL-101 earned excellent reusability. All these demonstrated that Fe@MIL-101 exhibited excellent adsorption capability to polycyclic aromatic hydrocarbons and would be a good adsorbent for development of new monitoring methods for environmental pollutants.

研究领域: 环境科学 · 材料科学
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