ANALYST
·
2012
·Vol. 137
·期 22
·5411-5419
·
IF 4.23
Xiang-Feng Chen,Hao Zang,Xia Wang,Jian-Guang Cheng,Ru-Song Zhao,Chuan-Ge Cheng,Xiao-Qing Lu
In this paper, the potential applications of metal–organic framework (MOF) materials as fiber coatings for the solid-phase microextraction (SPME) of polycyclic aromatic hydrocarbons (PAHs) in water samples were explored. Fibers coated with MIL-53(Al, Cr, Fe) materials were fabricated by an adhesive method for SPME. The quantitation was performed by gas chromatography–tandem mass spectrometry (GC–MS/MS) using the multiple reaction monitoring mode. Among the three MIL-53(M) coatings, MIL-53(Al) showed the highest extraction efficiency towards PAHs under the current fabrication procedure. Under optimized conditions, the MIL-53(Al)-coated fiber showed good precision (relative standard deviation <12.5%), low detection limits (0.10 ng L−1 to 0.73 ng L−1, S/N = 3), and good linearity (R2 > 0.98) for aqueous solutions containing 16 PAH . The fiber also offered high thermal and chemical stability. The method developed based on MIL-53(Al) SPME–GC–MS/MS was successfully applied in the analysis of real water samples. Based on the simulation results, the PAHs were adsorbed on MIL-53(Al) primarily through the hydrophobic and π–π interactions between PAHs and the organic linker of the material. The results presented in this paper indicate that water-stable MOF materials have great potential for the SPME of aromatic compounds in water samples.
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COLLOIDS AND SURFACES A-PHYSICOCHEMICAL AND ENGINEERING ASPECTS
·
2025
·
IF 5.4
Zhengang Bu,Jianhua Li,Siqi Fang,Yuanlin Zhan,Wenzhuo He,Yibin Huang
The uniform and stable deposition of metal-organic frameworks (MOFs) onto membranes without compromising their performance presents a significant challenge. This study reports the fabrication of a photocatalytic self-cleaning membrane using hydrothermal and photochemical substitution methods. These methods enabled the uniform and stable deposition of β-FeOOH nanorods, m-MIL-100(Fe), and Ag nanoparticles (NPs) not only on the members surface but also throughout the interior of polyvinylidene fluoride (PVDF) membrane pores. The synergistic effect of these materials and their uniform and stable distribution within the PVDF membrane resulted in superior photocatalytic efficacy. The membrane's excellent photocatalytic performance facilitated the degradation of most pollutants, ensuring prolonged usage. Unlike other photocatalytic membranes requiring additional cocatalysts, our membrane degraded over 90% of various dyes without H 2 O 2 , demonstrating a greener usage mode and higher photocatalytic efficiency. The valence band (VB) and conduction band (CB) of β-FeOOH nanorods and m-MIL-100(Fe) were calculated, confirming the existence of a type-II heterojunction for the first time. Free radical trapping experiments identified hydroxyl radicals (·OH) as the primary reactive species in the degradation process. This research provides a novel approach to uniformly and stably load MOFs on membranes, enhancing their properties and offering insights into fabricating multifunctional photocatalytic membranes.
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TALANTA
·
2024
·
IF 5.6
Xueyun Wei,Zhuomin Zhang,Gongke Li
Aromatic disinfection by-products (DBPs) have garnered considerable interest in recent years for their potential carcinogenicity. However, efficient separation and enrichment of DBPs in complex samples is a challenge due to the extremely low content of aromatic DBPs and the complexity of sample matrices. In this study, a MIL-101(Cr)–NH 2 @TAPB-DVA-COF hybrid material was prepared as the enrichment medium of membrane solid-phase extraction (M-SPE) to efficiently determine trace emerging aromatic DBPs. This medium exhibited excellent enrichment capacity and selectivity for aromatic DBPs because of the strong hydrogen bonding, π-π stacking and hydrophobic interactions. An efficient analytical method for five aromatic DBPs in juice drinks was successfully established by use of this hybrid material as the enrichment medium for M-SPE in combination with liquid chromatography tandem mass spectrometry (LC-MS/MS). The limits of detection of the established method were from 0.50 to 3.00 ng/L. Moreover, the method had been successfully used in real juice drinks to determine trace five aromatic DBPs with the spiked recoveries ranging from 84.1% to 125%. The method possessed high analytical sensitivity and accuracy for these five aromatic DBPs in juice drinks with the aid of the efficient M-SPE technology proposed.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Yun Wu,Yanqun Yang,Ming Wen,Jing Xie,Linchun Bao,Shuting Yang,Xiangming Luo,Xingyi Wang,Qianchun Zhang
Monoamine neurotransmitters play vital roles in cognitive and various physiological and pathophysiological processes, but their trace levels, small sample volumes, and complex biological matrices in biological samples pose significant analytical challenges. This study developed a novel method for the simultaneous quantification of six monoamine neurotransmitters—tyrosine, vanillylmandelic acid, tryptophan, 3,4-dihydroxyphenylacetic acid, 5-hydroxyindole-3-acetic acid, and homovanillic acid—in human serum and urine. The method utilizes magnetic solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A multifunctional magnetic composite, polyethylenimine@polymer dopamine hydrochloride@NH 2 -MIL-53(Al)-SiO 2 @Fe 3 O 4 , was synthesized, exhibiting high extraction selectivity and capacity and achieving an extraction range of 9.61–25.4 nmol/mg for the target neurotransmitters. The analytical method, optimized for the aforementioned composite, exhibited robust linearity for all six monoamine neurotransmitters, with correlation coefficients ( R 2 ) exceeding 0.998. The limits of detection (S/N = 3) ranged from 1.1 to 22 ng/L, indicating high sensitivity. Recovery rates for the targeted analytes varied between 94.5 % and 112 %, and relative standard deviations remained within the range of 1.5–9.4 %. These findings confirm that the developed methodology is sensitive, accurate, selective, and reliable for the quantitative determination of trace monoamine neurotransmitters in complex biological samples.
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JOURNAL OF COLLOID AND INTERFACE SCIENCE
·
2019
·
IF 6.361
Jiping Ma,Shuang Li,Gege Wu,Shasha Wang,Xiaotong Guo,Liyan Wang,Xiaoyan Wang,Jinhua Li,Lingxin Chen
Novel mixed-matrix membranes (MMM) were prepared from metal-organic frameworks (MOF) (MIL-53) and poly (vinylidene fluoride) (PVDF), viz MIL-53–PVDF MMM, for the simultaneous dispersion membrane extraction (DME) of seven sulfonylurea herbicides (SUs) in aqueous environments followed by high performance liquid chromatography (HPLC) determination. The MIL-53–PVDF MMM was well characterized and major factors influencing DME performances were systematically investigated including membrane type, MOF dosage, eluent type, solution pH, extraction/elution time and salinity, etc. Under optimal conditions, the MIL-53–PVDF MMM based DME coupled with HPLC exhibited excellent linearity within 0.03–10 μg L −1 for chlorimuronethyl and 0.01–10 μg L −1 for other six SUs individual. High enrichment factor of 250 was obtained, as well as low detection limits and quantification limits ranged from 3.75 to 10.30 ng L −1 and 12.49–34.30 ng L −1 , respectively. Furthermore, the method attained high recoveries of 77.20–111.00% at three spiking levels of SUs, with relative standard deviations of 1.28–14.67% in tap water, seawater and surface water samples. Additionally, the MMM was readily separated from water and well regenerated, and could keep about 80% recovery after 25 cycles. Compared to that reported extraction materials, the MIL-53–PVDF MMM possessed the advantages of high enrichment ability, excellent reusability, good practicality and easy separation, indicating it was a promising alternative for the enrichment of SUs from aqueous environments.
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CRYSTAL GROWTH & DESIGN
·
2018
·
IF 3.972
Wei Zhang,Run-Zhi Zhang,Yong-Qing Huang,Ji-Min Yang
Herein, we report that the surface charge status and size of the metal–organic framework (MOF) MIL-101(Cr) can be tailored by varying the concentration of tetramethylammonium hydroxide. The adsorption capacity of MIL-101(Cr)-2 toward the anionic dye Congo red (CR) was found to be significantly higher than that of other MIL-101(Cr) adsorbents, although MIL-101(Cr)-3 microcrystals exhibited the highest adsorption capacity toward the anionic dye methyl orange (MO) due to the different adsorption mechanisms involved. This is the first demonstration of the synergetic interplay between the electrostatic and π–π interactions, adsorption spaces and sites, and size of the dye molecules, in terms of the uptake capacity of an adsorbent. In addition, the obtained results shed new light on the adsorption mechanism toward organic dyes over MOFs. Moreover, the MIL-101(Cr) microparticles exhibited excellent adsorption capabilities toward CR, achieving a maximum capacity of 1367.1 mg g–1, which is higher than the majority of reported values for other materials. Therefore, these results indicate that the MIL-101(Cr) nanostructure exhibits potential for application in the treatment of anionic dye-containing wastewater.
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TALANTA
·
2016
·
IF 4.035
Xinpeng Dai,Xiuna Jia,Pan Zhao,Ting Wang,Jian Wang,Peiting Huang,Lu He,Xiaohong Hou
As a novel kind of materials, metal-organic frameworks (MOFs) have great potential for the preconcentration of trace analytes. In our work, MIL-101(Cr) was prepared and applied as a solid phase extraction (SPE) sorbent for the pretreatment of sulfadiazine (SDA), sulfamethazine (SMZ), sulfachloropyridazine (SCP) and sulfamethoxazole (SMX) in different environmental water samples coupling with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection. Experimental parameters, such as SPE materials, pH of water sample, volume of sample, flow rate , and type and volume of elution solvent, were properly optimized. Under the optimum conditions, good sensitivity levels were achieved with the detection limits of 0.03–0.08 μg/L and the quantitation limits of 0.11–0.27 μg/L. The linear ranges were from 0.2–40 or 0.5–100 μg/L ( r 2 >0.996) for the analytes, and the relative recoveries were in the range from 83.5% to 107.3% with the relative standard deviations (RSD) between 0.2% and 8.0% ( n =6). In addition, computational simulation was primarily used to predict the adsorption of MIL-101(Cr) toward sulphonamides (SAs), and also demonstrated the molecular interactions and free binding energies with the molecular modeling method. The results revealed that the combination of experimental and computational study not only accurately recognized the adsorption of MIL-101(Cr) on SAs, but also provided a new strategy on the trace contaminant analysis.
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MICROCHIMICA ACTA
·
2022
·Vol. 189
·期 11
·1-10
·
IF 6.408
Fan Ru,Tian Jinrong,Wang Huili,Wang Xuedong,Zhou Peipei
By employing NH 2 -MIL-88 as a template, we synthesized the intermediate Fe@CN under high-temperature calcination and further fabricated the FeS 2 @CN nanocomposites in the presence of sulfur powder. Under varying temperatures (300–600 °C) and Fe@CN-to-S ratios (1:3–6), FeS 2 @CN 500-5 nanocomposites had the highest peroxidase-mimetic activity. Under optimized conditions (incubation temperature 40 °C; solution pH 4.0 and nanocomposite concentration 10 μg/mL; 652-nm absorption), the Michaelis-Menten constant ( K m ) of FeS 2 @CN was much lower than that of horseradish peroxidase (HRP), therefore demonstrating that it had a higher affinity for both chromogenic substrates than conventional HRP. The limits of detection for H 2 O 2 and glucose were 0.15 and 0.30 μmol/L, respectively, and the recoveries for glucose were 91.8–103% with RSDs <5.2%. The novelty of this study lies in (1) the FeS 2 @CN was confirmed to possess stronger enzyme-mimetic activity than its precursors (NH 2 -MIL-88 and Fe@CN); (2) the enhanced activity resulted from the unsaturated sites of N and S doping and the plentiful defects on the porous carbon surface; and (3) free radical trapping experiments evidenced that •OH played a major role in the catalytic reaction, while h + and •O 2 − simultaneously participated in the catalytic process. These convincing performance metrics lead us to postulate that the FeS 2 @CN-based colorimetric biosensor provides a promising approach for several real-world applications, such as point-of-care diagnosis and workplace health evaluations. Graphical abstract
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LANGMUIR
·
2023
·
IF 3.9
Suyun Wang,Yuanbo Fang,Wuli Han,Qiang Li,Xiao Luo
For the first time, MIL-100(Fe)-derived microspheres with a hollow structure were perfectly constructed and used as a photocatalyst to decompose organic dyes under visible light irradiation. The prepared MIL-100(Fe)-NH2(20) could boost the separation, migration, and transfer of photoinduced carriers effectively, together with efficient photocatalytic performance. In simulated sunlight, the MIL-100(Fe)-NH2(20) exhibits the best degradation efficiency as well as excellent reusability and stability, and the degradation rate for rhodamine B (RhB) can be more than 99.5% within 80 minutes. Structural analysis proves that the porous MIL-100(Fe)-NH2(20) catalyst reaps an amazing hollow structure, large specific surface areas (2784.9 m2·g–1), and uniform distribution of Fe and N active phases. Besides, the enhanced visible light response and lower recombination rate of e––h+ pairs are both confirmed, and the band gap is significantly reduced to 2.53 eV. Finally, the photocatalytic mechanism and the possible degradation pathway were suggested. Owing to the enhanced photocatalytic activity, good tolerance to pH and water quality, and excellent stability, the MIL-100(Fe)-NH2(20) catalyst can be potentially used in a wide range of dye wastewater purifications.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 6
·1-11
·
IF 5.479
Chen Zhipeng,Yu Chen,Xi Jiangbo,Tang Sheng,Bao Tao,Zhang Juan
A hybrid material was synthesized by growing a covalent organic framework (COF) in-situ on the surface of functionalized metal organic framework (MOF). Specifically, the amino-modified MOF (type MIL-68) was obtained by reacting indium(III) nitrate and 2-aminoterephthalic acid. Subsequently, it was reacted with tris(4-formylphenyl)amine and tris(4-aminophenyl)amine to obtain the final hybrid COF. This material overcomes the disadvantage of MOF concerning poor stability in aqueous solution and it combines the advantages of MOF and COF. This MOF@COF hybrid material is shown to be a viable adsorbent for the extraction of sulfonamides by pipette tip solid-phase extraction). Following elution with acetonitrile, the sulfonamides were quantified by high performance liquid chromatography using variable wavelength detection (HPLC-VWD). The structure and morphology of the material was characterized by various techniques. Extraction parameters such as amount of adsorbent, sampling rate, sample pH, elution solvent and sample volume were investigated. Under the optimum conditions, the sulfonamides tested (sulfadimethoxine sulfamethoxazole, sulfamonomethoxine, sulfamethazine, sulfamerazine and sulfadiazine) can be determined over a wide linear range (10–2000 ng·mL −1 ), with low limits of detection (1 ng·mL −1 ) and high precision (RSD <5.2%). The method was applied the determination of sulfonamide residues in (spiked) environmental water, milk and meat samples and gave recoveries in the range from 68.9–103.8%, with RSDs of <6.6%. The packed pipette tip column exhibits excellent stability, reproducibility and high adsorption capacity.
A hybrid sorbent was prepared by controlled growth of a covalent organic framework on amino-modified MIL-68 and packed into a pipette tip for sulfonamide extraction. The sensitivity was dramatically increased after optimized extraction, with limit of detection as low as 1 ng·mL -1
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TALANTA
·
2016
·
IF 4.035
Xialin Luo,Gongke Li,Yufei Hu
In this work, a novel NH 2 -MIL-53(Al) incorporated poly(styrene-divinylbenzene-methacrylic acid) (poly(St-DVB-MAA)) monolith was prepared via chemical fabrication. Moreover, it has been efficiently applied to the in-tube solid-phase microextraction (SPME) for online coupling with high-performance liquid chromatography (HPLC) to the direct determination of five estrogens in human urine samples. The NH 2 -MIL-53(Al)-polymer monolith was suitable for in-tube SPME owing to its good permeability, high extraction efficiency, chemical stability, good reproducibility and long lifetime. The extraction conditions including extraction solvent, pH of sample solution, flow rate of extraction and desorption, and desorption volume were investigated. Under the optimum conditions, the enrichment factors were 180–304 and saturated amounts of extraction were 2326–21393 pmol for estriol , 17β-estradiol, estrone , ethinyl estradiol and progesterone , respectively. The adsorption mechanism was also explored which contributed to its strong extraction to target compounds. The proposed method had low limit of detection (2.0–40 ng/L) and good linearity (with R 2 between 0.9908 and 0.9978). Four endogenous estrogens were detected in urine samples and the recoveries of all five analytes were ranged from 75.1–120% with relative standard deviations (RSDs) less than 8.7%. The results showed that the proposed online SPME-HPLC method based on NH 2 -MIL-53(Al)-polymer monolithic column was highly sensitive for directly monitoring trace amount of estrogens in human urine sample.
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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.
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