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FOOD CHEMISTRY · 2025 · IF 9.8

Metal-organic framework UiO-66-NH2 functionalized polydopamine-modified magnetic multi-walled carbon nanotubes for convenient magnetic solid-phase extraction of sixteen quinolones

Lin Lv,Hongmei Liu,Lei Wang,Sikai Wang,Yue Li,Guoqi Zhang,Yan Zhao

In this study, an innovative magnetic solid-phase extraction adsorbent based on metal-organic framework UiO-66-NH 2 functionalized polydopamine-modified magnetic multi-walled carbon nanotubes (Fe 3 O 4 @MWCNTs@PDA@UiO-66-NH 2 ) was developed for the selective extraction of trace amounts of quinolones (QNs) from milk and honey. Under optimal conditions, when coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), the developed approach demonstrated excellent linearity in the concentration range of 0.1–100 μg kg −1 (R 2  ≥ 0.9916). The recoveries for sixteen QNs ranged from 72.4 % to 108.9 %, with relative standard deviations less than 9.40 %. The limits of detection were 0.012–0.450 μg kg −1 for milk and 0.023–0.690 μg kg −1 for honey. Finally, the method was successfully applied to the quantification of QNs in milk and honey samples.

研究领域: 分析化学 · 食品科学 · 环境科学
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ANALYTICAL LETTERS · 2016 · IF 1.088

Preconcentration and Determination of Cadmium, Lead, and Cobalt in Moringa Oleifera (Moringaceae) Using Magnetic Solid-Phase Extraction and Flame Atomic Absorption Spectrometry

Shuangqiao Ju,Mousheng Liu,Yaling Yang

Magnetic solid-phase extraction was used for the preconcentration of cadmium, lead, and cobalt in Moringa Oleifera with determination by flame atomic absorption spectrometry. Fe3O4 nanoparticles were modified by oleic acid to form the sorbent for magnetic solid-phase extraction. The modified sorbent was characterized by transmission electron microscopy, infrared spectroscopy, and X-ray diffraction. The preconcentration was optimized for the mass of nanoparticles, pH, adsorption time, the presence of coexisting ions, solution volume, eluent, and reuse. The optimized limits of detection were 0.09, 0.26, and 0.54 µg/L for Cd(II), Pb(II), and Co(II) with relative standard deviations below 4.3%. The method was employed for the analysis of Moringa oleifera and recoveries between 90.0 and 102.0% were obtained.

研究领域: 分析化学 · 环境毒理学 · 植物营养学 · 食品安全 · 重金属检测
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 42 ·期 5 ·1058-1066 · IF 2.516

Fe3O4/reduced graphene oxide-carbon nanotubes composite for the magnetic solid-phase extraction and HPLC determination of sulfonamides in milk

Yingying Feng,Xiaopeng Hu,Faqiong Zhao,Baizhao Zeng

A novel magnetic adsorbent Fe 3 O 4 /reduced graphene oxide-carbon nanotubes, was prepared by one-pot solvothermal synthesis method. It was characterized by scanning electron microscopy, X-ray powder diffraction and vibrating sample magnetometry. The diameter of Fe 3 O 4 microparticles was about 350 nm, which were covered by carbon nanotubes and reduced graphene oxide sheets, while carbon nanotubes inserted between the reduced graphene oxide sheets effectively prevented their aggregation. The composite had large surface area and good magnetic property, suiting for magnetic solid-phase extraction and the determination of sulfonamides, by coupling with high-performance liquid chromatography. Under the optimized conditions (including extraction time, amount of adsorbent, solution pH, ionic strength and desorption conditions), a good linear was achieved in the concentration range of 5–500 μg/L and the low limits of detection and low limits of quantification were 0.35–1.32 and 1.16–4.40 μg/L, respectively. The enrichment factors were estimated to be 24.72 to 30.15 fold. The proposed method was applied for the detection of sulfonamides in milk sample and the recoveries were 88.4–105.9%, with relative standard deviations of 0.74–5.38%.

研究领域: 分析化学 · 材料科学 · 食品安全
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FOOD CHEMISTRY · 2019 · IF 5.399

Reversed-phase/weak anion exchange magnetic mesoporous microspheres for removal of matrix effects in lipophilic marine biotoxins analysis by ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry

Fei Xu,Feng Liu,Chaozhan Wang,Yinmao Wei

Magnetic solid-phase extraction (MSPE), using a new reversed-phase/weak anion exchange mix-mode mesoporous magnetic SiO 2 adsorbent, was assessed as an approach for reducing matrix effects in the analysis of six lipophilic marine biotoxins in shellfish using ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The adsorbent showed greater adsorption capacity and selectivity for the analytes and, thus, the MSPE microspheres reduced the matrix effects significantly in the subsequent analysis. In the UPLC-MS/MS analysis, precursor and product ions of the analytes were monitored quantitatively and qualitatively using multiple reaction monitoring and product ion confirmation modes. The proposed method exhibited a linear correlation of 0.9980–0.9991 in the working range for azaspiracids (2.0–200.0 ng/mL) and okadaic acid and its derivatives dinophysistoxins (4.0–200.0 ng/mL) with satisfactory recoveries (82.8–118.6%, RSD < 12%), lower LODs (0.4–1.0 μg/kg) and LOQs (1.0–4.0 μg/kg) than existing methods. In addition, consumption of the adsorbent was reduced, and the MSPE operation is simple and rapid relative to alternatives. These results suggest the proposed method has potential for use in the analysis of lipophilic marine biotoxins in shellfish samples.

CAS / MDL: 3069-42-9
研究领域: 分析化学 · 海洋生物学 · 毒理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2021 · IF 3.205

Determination of six parabens in biological samples by magnetic solid-phase extraction with magnetic mesoporous carbon adsorbent and UHPLC-MS/MS

Qianchun Zhang,Yongzhi Zhi,Linchun Bao,Yuguo Zheng,Xingyi Wang,Li Jiang,Yun Wu

Although parabens are useful due to their antiseptic properties, their widespread use has caused concerns regarding their potential toxicological effects. In this study, a novel magnetic solid-phase extraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (MSPE-UHPLC-MS/MS) was developed, based on ordered magnetic mesoporous carbon (MMC), for paraben analysis. The MMC was prepared by soft-template synthesis, with a unique pore structure and a highly specific surface response, indicating potential as an excellent adsorbent. Several parameters affecting the paraben extraction efficiency were investigated and a novel method for paraben analysis in serum and urine samples using MSPE-UHPLCMS/MS was developed. The concentrations of methylparaben, ethylparaben, isopropylparaben, and propylparaben in these samples were 0.0380–4.36, 0.460–9.65, 0.0118–0.770, and 0.0363–0.641 μg/L, respectively, whereas isobutylparaben and butylparaben were not detected. Furthermore, satisfactory recoveries of 76.4–121% with relative standard deviations (n = 5) of 1.9–8.6% were obtained. Therefore, the developed MSPE-UHPLC-MS/MS method was efficient, highly sensitive, and reliable for analysing parabens in complex biological samples.

研究领域: 分析化学 · 环境科学 · 毒理学
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RSC Advances · 2016 ·Vol. 6 ·期 61 ·56240-56248 · IF 3.289

Magnetic solid-phase extraction based on ferroferric oxide nanoparticles doubly coated with chitosan and β-cyclodextrin in layer-by-layer mode for the separation of ibuprofen

Pengfei Chen,Hang Song,Lu Zhou,Jun Chen,Jiyang Liu,Shun Yao

A novel and environmentally-friendly magnetic adsorbent consisting of ferroferric oxide (Fe3O4) nanoparticles, β-cyclodextrin and chitosan was successfully fabricated by layer-by-layer methodology and applied in the magnetic solid phase extraction (MSPE) of ibuprofen. The adsorption results demonstrated that ibuprofen extraction was significantly pH dependent and the optimal pH value was 5.0, which was mainly ascribed to the electrostatic interaction and inclusion complexes between the adsorbent and ibuprofen. The adsorption kinetics of ibuprofen was found to follow a pseudo-second-order kinetic model. Thermodynamic data for ibuprofen adsorption were fitted well by the Freundlich model and the Freundlich constant indicated it was a favorable process. The thermodynamic parameters suggested that the adsorption process was endothermic and spontaneous in nature. Based on the adsorption research, the main factors affecting the MSPE procedure were optimized, including desorption conditions, amount of adsorbents and eluent volume. Under the optimal conditions, the enrichment factor was 182.56. Moreover, the feasibility of the proposed procedure was demonstrated with the extraction and enrichment of ibuprofen from an environmental water sample, and the results indicated that the complex composition of the investigated object did not significantly affect the selectivity of the extraction process.

研究领域: 分析化学 · 环境科学
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ANALYST · 2014 ·Vol. 139 ·期 8 ·1938-1944 · IF 3.906

Ultrasound-assisted magnetic solid-phase extraction based ionic liquid-coated Fe3O4@graphene for the determination of nitrobenzene compounds in environmental water samples

Xiaoji Cao,Lingxiao Shen,Xuemin Ye,Feifei Zhang,Jiaoyu Chen,Weimin Mo

An ultrasound-assisted magnetic solid-phase extraction procedure with the [C7MIM][PF6] ionic liquid-coated Fe3O4-grafted graphene nanocomposite as the magnetic adsorbent has been developed for the determination of five nitrobenzene compounds (NBs) in environmental water samples, in combination with high performance liquid chromatography-photodiode array detector (HPLC-PDA). Several significant factors that affect the extraction efficiency, such as the types of magnetic nanoparticle and ionic liquid, the volume of ionic liquid and the amount of magnetic nanoparticles, extraction time, ionic strength, and solution pH, were investigated. With the assistance of ultrasound, adsorbing nitrobenzene compounds by ionic liquid and self-aggregating ionic liquid onto the surface of the Fe3O4-grafted graphene proceeded synchronously, which made the extraction achieved the maximum within 20 min using only 144 μL [C7MIM][PF6] and 3 mg Fe3O4-grafted graphene. Under the optimized conditions, satisfactory linearities were obtained for all NBs with correlation coefficients larger than 0.9990. The mean recoveries at two spiked levels ranged from 80.35 to 102.77%. Attributed to the convenient magnetic separation, the Fe3O4-grafted graphene could be recycled many times. The proposed method was demonstrated to be feasible, simple, solvent-saving and easy to operate for the trace analysis of NBs in environmental water samples.

CAS / MDL: 7783-85-9 7783-83-7
研究领域: 分析化学 · 环境科学
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TALANTA · 2019 · IF 4.916

Facile magnetization of covalent organic framework for solid-phase extraction of 15 phthalate esters in beverage samples

Yue-Hong Pang,Qi Yue,Yu-ying Huang,Cheng Yang,Xiao-Fang Shen

Phthalate esters (PAEs), a category of widely used plasticizers , are tend to migrate from plastic packaging to drinks. In this paper, we develop a simple and rapid coprecipitation method for synthesis of a magnetic covalent organic framework (COF) adsorbent. The fabricated COF-(TpBD)/Fe 3 O 4 was applied to magnetic solid phase extraction (MSPE) of 15 phthalate esters (PAEs) for subsequent GC-MS/MS determination in beverage samples. The as-synthesized magnetic adsorbent exhibited great potential in PAEs analysis with a limit of detection of 15 PAEs ranged from 0.005 to 2.748 μg L −1  (S/N = 3). The intra-day and inter-day relative standard deviations (RSD) value of the PAEs were less than 8.8% and 9.9%, respectively. The adsorbent can be reused after washing with methanol. The developed method was successfully applied for the determination of trace PAEs in eight beverages with recoveries ranging from 79.3% to 121.8% and RSDs were less than 11.9%. This work provides a simple magnetization process, which facilitates the application of COFs for enrichment and separation of PAEs in beverages with different matrices.

CAS / MDL: 108-67-8
研究领域: 分析化学 · 环境科学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2018 · IF 2.441

Magnetic metal-organic frameworks for fast and efficient solid-phase extraction of six Sudan dyes in tomato sauce

Xin-Ran Shi,Xue-Lei Chen,Yu-Lan Hao,Li Li,Hou-Jun Xu,Man-Man Wang

Magnetic solid-phase extraction is an effective and useful technique to preconcentrate trace analytes from food samples. In this study, a magnetic trimeric chromium octahedral metal-organic framework (Fe 3 O 4 -NH 2 @MIL-101) was fabricated and characterized. Fe 3 O 4 -NH 2 @MIL-101 was applied as an adsorbent of magnetic solid-phase extraction combined with high performance liquid chromatography to effectively isolate and simultaneously determine six Sudan dyes (Para Red, Sudan I–IV, and Sudan Red 7B) from tomato sauce. Potential factors affecting the MSPE were investigated in detail, and adsorption efficiency of Fe 3 O 4 -NH 2 @MIL-101 was compared with those of conventional adsorbents, such as neutral alumina, HLB, and C 18 . The developed method facilitated the extraction with using only 3 mg of adsorbent in 2 min. In addition, enhancement factors of 50, linear range of 0.01–25 μg/mL, and detection limit (S/N = 3) of 0.5–2.5 μg/kg were obtained. The intra-day and inter-day recoveries for spiked Sudan dyes were in the range of 72.6%–92.9% and 69.6%–91.6%, respectively, with relative standard deviations of ≤9.2%.

研究领域: 食品科学 · 分析化学
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MICROCHEMICAL JOURNAL · 2022 · IF 5.304

Deep eutectic solvent - loaded Fe3O4@MIL-101(Cr) with core–shell structure for the magnetic solid phase extraction of non-steroidal anti-inflammatory drugs in environmental water samples

Li Yang,Shuang Wang,Zhongshui Xie,Rongrong Xing,Runqin Wang,Xuan Chen,Shuang Hu

A novel deep eutectic solvent - loaded magnetic solid phase extraction (DES-L-MSPE) method was proposed, which was based on the direct loading of a hydrophobic DES composed of L-menthol and lactic acid (1:2) into the pores of core–shell magnetic Fe 3 O 4 @MIL-101(Cr) nanoparticles. The function of DES was to condition the Fe 3 O 4 @MIL-101(Cr) and promote liquid phase microextraction for the analytes. Through coupling with HPLC-UV analysis, this method was utilized for the determination of six non-steroidal anti-inflammatory drugs (NSAIDs), including ketoprofen, naproxen, flurbiprofen, diclofenac sodium, ibuprofen, and mefenamic acid in environmental water samples. The influencing parameters such as type and ratio of DES, amount of adsorbent, sample solution pH, salt concentration, extraction time, elution solvent and time were investigated and optimized in detail. Under the optimal conditions, the method exhibited good linearity (5.0–1000 μg/L for ketoprofen, ibuprofen, 1.5–600 μg/L for flurbiprofen, mefenamic acid, 2.5–1000 μg/L for naproxen and 3.0–600 μg/L for diclofenac sodium with the correlation coefficients ranging from 0.9972 to 0.9993), low limits of detection (0.20–1.1 μg/L), and high precision (RSD < 8.2 %). Besides, the recoveries in spiked lake and river water samples were 89.8 %–110.4 % and 83.8 %–109.0 %, respectively. Taken together, the established method was proved to be simple, fast, highly sensitive and accurate for the determination of NSAIDs from aqueous matrices.

CAS / MDL: 2216-51-5
研究领域: 分析化学 · 环境科学
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MICROCHEMICAL JOURNAL · 2022 · IF 5.304

A low-cost, efficient and selective detection method of acaricide residues: Adsorption study

Jiaxuan Fan,Jing Li,Wenfeng Zhou,Haixiang Gao,Runhua Lu

Acaricide residues (ARs) have high toxicity and pose a significant chronic dietary risk to humans. In this work, a low-cost and efficient selective detection method for ARs was developed. Meanwhile, to reduce the matrix effects of samples, a novel and fast pretreatment technology called magnetic solid phase extraction is used. After the optimization and validation of the method, the method’s limit of detection and quantitation were calculated as 0.5–0.9 and 1.7–3.1 μg L −1 , respectively. Additionally, the adsorption experiment between sorbents and ARs was thoroughly investigated in terms of adsorption behavior, mechanism, and selectivity. Finally, two environmental water samples were selected to verify the feasibility of the proposed method. The relative recovery ranged from 87 % to 116 % with a relative standard deviation ranging from 0.27 % to 9.41 %. These results demonstrated that the proposed method was low-cost and efficient and had the ability to selectively detect multiple ARs.

研究领域: 分析化学 · 环境科学 · 食品科学
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MOLECULES · 2023 ·Vol. 29 ·期 1 ·45 · IF 4.6

Magnetic Persimmon Leaf Composite: Preparation and Application in Magnetic Solid-Phase Extraction of Pesticides in Water Samples

Yuyue Zang,Na Hang,Jiale Sui,Senlin Duan,Wanning Zhao,Jing Tao,Songqing Li

In recent years, the utilization of biomass materials for the removal and detection of water pollutants has garnered considerable attention. This study introduces, for the first time, the preparation of Fe3O4/persimmon leaf magnetic biomass composites. The magnetic composites were employed in a magnetic solid-phase extraction method, coupled with gas chromatography-electron capture detection (GC-ECD), for the analysis of four pesticides (trifluralin, triadimefon, permethrin, and fenvalerate) in environmental water samples. The innovative magnetic persimmon leaf composites were synthesized by in situ generation of Fe3O4nanoparticles through coprecipitation and loaded onto persimmon leaves. These composites exhibit superparamagnetism with a saturation magnetization of 12.8 emu g−1, facilitating rapid phase separation using a magnetic field and reducing the extraction time to 10 min. Desorption can be achieved within 30 s by aspirating 20 times, eliminating the need for time-consuming and labor-intensive experimental steps like filtration and centrifugation. The specific surface area of the magnetic composite adsorbent increased from 1.3279 m2g−1for the original persimmon leaf to 5.4688 m2g−1. The abundant hydroxyl and carboxyl groups on the composites provide ample adsorption sites, resulting in adsorption capacities ranging from 55.056 mg g−1to 73.095 mg g−1for the studied pesticides. The composites exhibited extraction recoveries ranging from 80% to 90% for the studied pesticides. Compared to certain previously reported MSPE methods, this approach achieves equivalent or higher extraction recoveries in a shorter operation time, demonstrating enhanced efficiency and convenience. Good linearity of the target analytes was obtained within the range of 0.75–1500 μg L−1, with a determination of coefficient (R2) greater than 0.999. These findings contribute to the use of magnetic persimmon leaf biomass materials as effective and environmentally friendly adsorbents for pollutant determination in water samples.Keywords:biomass adsorbent;Fe3O4/persimmon leaf magnetic composite;magnetic solid-phase extraction;pesticides;water

研究领域: 环境科学 · 分析化学
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