Analytical Methods
·
2014
·Vol. 6
·期 19
·7842-7847
·
IF 1.938
Guan-Hua Wang,Yong-Qian Lei,Hua-Can Song
Metal–organic frameworks (MOFs), a novel class of hybrid inorganic–organic materials, possess high surface area, good thermal stability and selectivity, and thus have great potential for use as sorbent materials. MOF-177 is attractive for its large pores, high adsorptivity and selectivity, which has rarely been used in analytical science. Herein a facile magnetization of MOF-177 for rapid magnetic solid phase extraction of phenols from environmental water samples was studied, with analysis using gas chromatography-mass spectrometry. The magnetization of MOF-177 microcrystals as well as solid-phase extraction (SPE) of phenols was achieved simultaneously by mixing MOF-177 and Fe3O4@SiO2 microparticles in the water sample under sonication. Under the optimized conditions, the developed method showed good linearity within the range of 1–200 μg L−1, low detection limits (16.8–208.3 ng L−1) and quantitation limits (56.0–694.2 ng L−1). The recoveries are between 83.3 and 108.7% with the spiked level of 25 μg L−1. The results demonstrated that the Fe3O4@SiO2–MOF-177 magnetic microspheres are promising sorbents in the MSPE field in environmental samples.
研究领域:
分析化学
·
环境科学
✓ 已验证
DOI
高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 6
·661-671
·
IF 3.532
Ming Gao,Xiaofan Zhang,Sai Ma,Junxia Wang,Marcus Mammah,Liyang Du,Xuedong Wang
Herein, an ionic-liquid-based effervescence-enhanced magnetic solid-phase extraction (ILE-MSPE) approach for the extraction/concentration of organophosphorus pesticides in waters is reported with high stability and portability for rapid sample pretreatment in the field. The ionic-liquid-based magnetic effervescent tablet, composed of magnetic nanoparticles (Fe3O4), sodium carbonate (Na2CO3) as an alkaline source, and an ionic liquid ([C6MIM][PF6]), played triple functions: extractant, dispersant, and retrieving agent. Based on the one-factor-at-a-time method, the important variables for the ILE-MSPE approach were optimized as follows: as an extractant, 70 μL of [C6MIM][PF6]; molar ratio of alkaline to acidic sources (Na2CO3 : H2C4H4O6) as 1 : 1; and mass of magnetic nanoparticles (MNPs) of 30 mg. By integrating HPLC-DAD detection, the ILE-MSPE approach offered the limits of detection of 0.14–0.22 μg L−1 and fortified recoveries of 81.4–97.6% for three representative species (methamidophos, phoxim, and parathion) in water samples. The relative standard deviations were lower than 4.9% for both the intra-day and inter-day precision. Overall, the newly developed method is environmentally benign, time-saving, and feasible for outdoor application.
研究领域:
分析化学
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环境科学
✓ 已验证
DOI
高影响因子
FOOD CHEMISTRY
·
2017
·
IF 4.529
Wenhua Ji,Mingming Zhang,Wenjuan Duan,Xiao Wang,Hengqiang Zhao,Lanping Guo
Phytic acid-stabilized Fe 3 O 4 -graphene oxide (GOPA@Fe 3 O 4 ) was assembled by microwave-enhanced hydrothermal synthesis and super-amphipathicity was demonstrated by measurement of dynamic oil and water contact angles. GOPA@Fe 3 O 4 was used as a sorbent for enrichment of eight polycyclic aromatic hydrocarbons (PAHs) from vegetable oils by magnetic solid-phase extraction (MSPE). The extraction-desorption factors were systematically investigated and, under optimum conditions, the super-amphiphilic sorbent achieved wide linear ranges (0.2–200 ng g −1 ), satisfactory precision (3.44–6.64% for intra-day and 5.39–8.41% for inter-day) and low limits of detection (LODs, 0.06–0.15 ng g −1 ) for PAHs. Excellent recoveries (85.6–102.3%) for spiked PAHs were obtained with genuine vegetable oil samples. These results indicate that MSPE using GOPA@Fe 3 O 4 as the sorbent, coupled with high performance liquid chromatography (HPLC), is an efficient and simple method for the detection of low concentrations of PAHs in vegetable oils.
研究领域:
分析化学
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环境科学
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食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 3
·e70118
·
IF 2.8
Yu Jiang,Hong Pan,Menghong Xie,Huifeng Deng,Guihua Ruan,Yipeng Huang
In this study, magnetic Fe 3 O 4 -coated metal-organic framework composites, CONH 2 -MIL-101(Cr)/Fe 3 O 4 , were synthesized by depositing Fe 3 O 4 particles on the surface of amidated MIL-101(Cr). The scanning electron microscope images show that the MIL-101(Cr) crystals were uniformly coated by Fe 3 O 4 particles. The magnetic hysteresis curve of CONH 2 -MIL-101(Cr)/Fe 3 O 4 reveals a saturated magnetization value of 23.47 emu/g. The water contact angle decreases from 61.00° to 12.88° after amidation and Fe 3 O 4 coating. The magnetic solid-phase extraction (MSPE) efficiency of CONH 2 -MIL-101(Cr)/Fe 3 O 4 for benzoic acid derivatives was studied. Under optimal conditions, the adsorption and desorption processes can be completed within 5 min, and the maximum adsorption capacity to protocatechuic acid (PCA) and vanillic acid (VA) is 10.31 and 17.30 mg/g. Coupling the MSPE with high-performance liquid chromatography-ultraviolet detection, the detection limit for PCA and VA was 0.29 and 0.58 ng/mL, respectively. The mean recoveries of PCA and VA in spiked samples ranged from 82.85%–91.27% with relative standard deviations lower than 0.33%–5.33%. This study provides inspiration for the fabrication of novel magnetic sorbents, and a reliable method for the adsorption and analysis of benzoic acid derivatives.
研究领域:
分析化学
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材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Sustainable Food Systems
·
2024
·
IF 3.7
Ai-Jun Huang,Xiu-Xiu Dong,Shu Tan,Kai Chen,Meiling Zhang,Bingrong Li,Hao Deng,Fan He,Hui Ni,Hongwu Wang,Zi-Jian Chen
Sample pretreatment is an essential procedure in pesticide analysis, as the matrix effect can significantly influence the results. In this study, a covalent organic framework (COF) was synthesized using 1,2,4,5-tetrakis-(4-formylphenyl)benzene (TFPB) and benzidine (BD) to mitigate the matrix effect in vegetable and fruit samples. This COF was then used to develop a solid-phase extraction (CSPE) method. In addition, the COF was used to create a magnetic COF (MCOF) for use in magnetic solid-phase extraction (MSPE). The synthesized COF and MCOF were thoroughly characterized using scanning electron microscopy (SEM) for morphological analysis, Fourier-transform infrared spectroscopy (FT-IR) for chemical bond identification, and N2 adsorption–desorption measurements for porosity and surface area assessment. Key pretreatment parameters such as buffers, dilution rate, sorbent dosage, extraction time, elution solvent, and reuse number were optimized. The developed CSPE and MSPE showed excellent purification ability for the matrix of vegetable and fruit samples. The reuse test demonstrated that the synthesized COF and MCOF can be reused up to 15 times. Moreover, the developed CSPE and MSPE showed acceptable recoveries in spiked recovery tests, suggesting that these pretreatment methods were feasible for sample purification in pesticide analysis.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2021
·Vol. 45
·期 21
·9382-9393
·
IF 3.591
Xiangzhi Feng,Yuanyuan Li,Yuanyuan Yang,Yulong Ma,Wenxin Ji,Yonggang Sun,Tong Chen,Yang Chen
In order to achieve rapid and effective analysis of praziquantel and pymetrozine residues in food, a new magnetic solid phase extraction (m-SPE) material based on GO and ZIF-67 was synthesized. Because the release of ZIF and GO materials may lead to secondary environmental pollution and their separation from solutions is difficult, ZIF-67 loaded on sheet-like MGO@PDA, a magnetic porous nano-composite, was fabricated by a convenient method at room temperature. The poly-dopamine (PDA) layer can improve the hydrophilicity of the material. The resultant MGO@PDA@ZIF-67 preserved the properties of ZIF-67 and MGO. The adsorbent material was characterized by XRD, VSM, TEM, SEM, TGA, XPS and FTIR experiments. An m-SPE technique was developed to selectively enrich two pyridine ring insecticides (praziquantel and pymetrozine) using high performance liquid chromatography (HPLC). The adsorption mechanism was investigated. Results showed that the maximum adsorption capacities of the new material for praziquantel and pymetrozine are 22.68 and 24.27 mg g−1, respectively. The method was successfully applied to the analysis of praziquantel and pymetrozine in vegetable samples with satisfactory recoveries (92.3%–102.8%) and precisions. Due to the advantages of easy preparation, high efficiency, and renewability, the prepared hydrophilic magnetic porous nano-composite is an excellent candidate for adsorption and separation and provides a promising magnetic ZIF-67 material for multi-component system separation.
研究领域:
食品科学
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环境科学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY
·
2020
·
IF 1.431
Jiahui Yang,Kaixuan Ma,Nan Li,Xinyue Gu,Shengchao Miao,Meixing Zhang,Jing Yang,Shihai Cui
Novel magnetic CoFe2O4-embedded MIL-101(Cr) with tetramethylammonium hydroxide (CoFe2O4/MIL-101T) was prepared through the facile hydrothermal method. Tetramethylammonium hydroxide acts as a template molecule and avoids the recrystallisation of terephthalic acid. The material was applied as the adsorbent in the magnetic solid-phase extraction (MSPE) process coupled with high-performance liquid chromatography to detect the five flame retardants in environmental water samples. Several parameters affecting MSPE efficiency were systematically investigated, such as MIL-101T content, material amount, desorption solvents, adsorption time, solution pH, theoretical maximum enrichment factor (EFmax) and the reusability. Under optimised conditions, good linearities were achieved for five flame retardants with correlation coefficients R2 > 0.9961. The limits of detections for analytes at the signal-to-noise ratio of three were 0.013–0.071 μg·L−1. This method was applied to the analysis of tap, pond, lake and river waters. The recoveries were in the range of 81.5 ± 3.2–107.0 ± 2.3% with the relative standard deviations ranging from 0.11% to 8.66% in four real water samples. The adsorption mechanism was the hydrophobic interaction between the material and the analytes besides pore adsorption action of the material.
研究领域:
材料科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Hui Chen,Chuanhui Huang,Wenming Zhang,Qingqing Ding,Jia Gao,Lan Zhang
An easy-prepared adsorbent with high stable and good dispersibility is especially valuable for the development of magnetic solid-phase extraction (MSPE) techniques. In this study, magnetic nitrogen-doped carbon nanotube cages (N-CNTCs) were synthesized via direct carbonization of cobalt (II)-containing metal-organic frameworks. During carbonization, cobalt ions inside the MOFs were converted into magnetic functional nanoparticles of N-CNTCs. Simultaneously, large amounts of nitrogen, originating from the organic ligands, were doped into the carbon framework. This unique structure gave the N-CNTCs excellent chemical stability, high affinity, and good dispersibility. The synthesized magnetic N-CNTCs were then used for MSPE of okadaic acid (OA) from aquatic samples. A simple, efficient, and sensitive method for detecting and quantitating OA was developed by combining the above sample pretreatment technique with high-performance liquid chromatography -tandem mass spectrometry (HPLC-MS/MS). The resulting method boasts a linear dynamic range of 3.0–1000.0 pg mL −1 with good linearity (R 2 ≥ 0.9994). The limit of detection (LOD) and limit of quantification (LOQ) were 1.3 pg mL −1 and 3.0 pg mL −1 , respectively. Several shellfish and seafood samples were analyzed using the developed method, showing satisfactory recoveries (82.0–107.0%) and relative standard deviations (<4.5%). The developed method was also used to investigate the OA distribution in crab tissues. Our results demonstrate that magnetic N-CNTCs are promising adsorbents for providing reliable support for the early warning and tracing to the source of algae toxins.
研究领域:
分析化学
·
环境科学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2981-2990
·
IF 4.58
Wang Ting,Liu Siyu,Gao Guihua,Zhao Pan,Lu Nan,Lun Xiaowen,Hou Xiaohong
The authors describe a method for magnetic solid phase extraction (MSPE) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the quantitation of eight non-steroidal anti-inflammatory drugs (NSAIDs) in wastewater and environmental water samples. Specifically, the NSAIDs were directly extracted by using a magnetic nanocomposite of type Fe 3 O 4 /MIL-101(Cr) (Matérial Institute Lavoisier, MIL) from 50 mL water samples without any further cleanup. The effects of the amount of adsorbent, pH value, salt concentration, ultrasonic extraction time, desorption solvent nature and volume and desorption time were investigated. Under the optimal conditions, UPLC-MS/MS based detection resulted in the following figures of merit: (a) Linear calibration plots that typically extend from 0.1 (0.2, 0.05, 0.02) to 50 μg·L −1 , depending on the compound; (b) detection limits between 3 to 60 ng·L −1 ; and (c), recoveries varying from 81.2% to 116.8% with relative standard deviations between 0.4% and 10.8%. The adsorption of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was characterized by adsorption isotherms, kinetics and thermodynamics studies and provides a deeper insight into the adsorption mechanism. Compared to other method for pretreatment and preconcentration of NSAIDs, the new method is more rapid, sensitive, accurate and eco-friendly. The method was successfully applied to the determination of the NSAID residues in a variety of real environmental and wastewater samples.
Schematic of a method for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in environmental water by magnetic solid phase extraction based on Fe 3 O 4 /MIL-101(Cr) combined with UPLC-MS/MS. The adsorption mechanism of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was studied.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 4
·1029-1036
·
IF 4.58
Zhou Qingxiang,Lei Man,Li Jing,Liu Yongli,Zhao Kuifu,Zhao Danchen
Metal organic frameworks of type MOF-5 exhibit good adsorption capacity for many organic compounds. The authors have used nanoscale silica-coated zerovalent iron and MOF-5 to prepare, by co-precipitation, a novel magnetic nanomaterial of type Fe@MOF-5. Its morphology and structure were characterized by transmission electron microscopy and X-ray diffraction. The nanomaterial is shown to be well suited for magnetic solid phase extraction for five kinds of N- and S-containing polycyclic aromatic hydrocarbons prior to quantitation by HPLC. The limits of detection are in the 25 to 33 ng⋅L −1 concentration range. Four real water samples were used to validate the method, and the recoveries of spiked samples with concentrations of 5 and 10 ppb were found to be in the range between 92.6 and 97.3% ( n = 3). The Fe@MOF-5 sorbent obviously has excellent adsorption capability for such compounds, can be fairly easily synthesized, displays sensitivity, simplicity, ease of operation, and can be prepared at low costs. In our perception, it has a large potential in terms of monitoring such environmental pollutants.
A metal organic framework of type Fe@MOF-5 is found to exhibit good adsorption capacity for N- and S-containing polycyclic aromatic hydrocarbons. A sensitive magnetic solid phase extraction method with Fe@MOF-5 was developed for the determination of N- and S-containing polycyclic aromatic hydrocarbons from the water samples.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 12
·1-7
·
IF 5.705
Pang Yachao,Zang Xiaohuan,Wang Mengting,Chang Qingyun,Zhang Shuaihua,Wang Chun,Wang Zhi
A fibrous magnetic boron nitride nanocomposite was synthesized and is shown to be a viable adsorbent for the magnetic solid phase extraction of pesticides prior to their quantitation by gas chromatography with electron capture detection. The optimum conditions were obtained by both single factor optimization and response surface analysis (Box-Behnken design). Under the optimized conditions, the response to the ten pesticides (dicofol, α-endosulfan, p,p’ -DDE, nitrofen, β -endosulfan, p,p’ -DDD, p,p’ -DDT, bifenthrin, permethrin and fenvalerate) is linear in the 0.03–40 ng·mL −1 concentration range with the coefficients of determination ranging from 0.9970 to 0.9992. The relative standard deviations at concentration levels of 0.5 ng·mL −1 , 20 ng·mL −1 and 40 ng·mL −1 were below 8.7%. The recoveries of the analytes from spiked tea water and tea beverage samples varied between 84.5% and 122%, with relative standard deviations ranging from 4.8 to 12%. The limits of detection are between 0.01 and 0.05 ng·mL −1 . The adsorbent can be reused over 50 times without significant loss of extraction efficiency.
A novel fibrous-shape magnetic boron nitride nanocomposite (Fe 3 O 4 @ f -BN) was used as the adsorbent for the magnetic solid phase extraction (MSPE) of ten pesticides from tea water and tea beverage samples prior to their determination by gas chromatography (GC).
研究领域:
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Yifu Jiang,Le Lang,Jingwen Zhang,Yining Ji,Chenglong Zhang,Ruiqin Yang,Xuwen Li
This study combined the structural characteristics of amanita peptide toxins to prepare a Fe 3 O 4 /P4VPBA/PPy/GO composite material as a magnetic solid-phase extraction adsorbent. The experimental results indicated that this adsorbent showed excellent selectivity for the extraction of amatoxins and phallotoxins from mushroom samples. Compared with traditional dispersive solid-phase extraction, this adsorbent enables rapid separation in the enrichment and elution recovery stages through the application of a magnetic field . Simultaneously, the study optimized the conditions for ultraperformance liquid chromatography–mass spectrometry (UPLC–MS/MS), ensuring both separation efficiency and accuracy while reducing the analysis time. The researchers established the MSPE–UPLC–MS/MS method for the determination of amanita peptide toxins in wild mushrooms. This method not only simplified and expedited the sample pretreatment process but also achieved qualitative and quantitative analyses in a short period, thus demonstrating high detection sensitivity and outstanding recovery rates. Furthermore, the developed method was successfully applied to analyze toxic mushrooms discovered in Nanjing, China. The potential for extensive utilization of this method is highlighted in the field of food analysis and detection.
研究领域:
分析化学
·
食品科学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）