TALANTA
·
2023
·
IF 6.1
Haoyu Long,Yanhao Jiang,Yanjuan Liu,Yuefei Zhang,Wei Chen,Sheng Tang
In this work, 2,4,6-tris(4-aminophenyl)-1,3,5-triazine (TAPT) and 1,3,5-tris(4-formylphenyl)benzene (TFPB) were used as monomers to construct a triazine-containing imine-linked covalent organic framework (COF), which was then bonded onto the surface of aldehydized silica (SiO 2 –CHO), and finally a COF@silica composite material (TAPT-TFPB COF@SiO 2 ) was successfully prepared. The chromatographic separation performance of SiO 2 –CHO, TAPT-TFPB COF@SiO 2 and TAPT-TFPB COF@SiO 2 /SiO 2 –CHO (80/20, mass ratio) was evaluated and compared. It was found that separation efficiency was obviously enhanced by adding an appropriate amount of SiO 2 –CHO into TAPT-TFPB COF@SiO 2 . The obtained TAPT-TFPB COF@SiO 2 /SiO 2 –CHO showed more favorable separation ability than SiO 2 –CHO and TAPT-TFPB COF@SiO 2 . Various aromatic compounds including alkylbenzenes , polycyclic aromatic hydrocarbons , environmental endocrine disruptors , foodborne stimulants and phenyl ketones were effectively separated on the TAPT-TFPB COF@SiO 2 /SiO 2 –CHO column in reversed phase chromatography mode. The silica microspheres surface-modified with triazine-containing imine-linked COFs proved to be a new type of promising chromatographic packing materials.
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Food Analytical Methods
·
2023
·Vol. 16
·期 6
·1131-1144
·
IF 2.9
Yu Chen,Luo Xiaogang,Wu Fengshou,Zhang Juan
A covalent organic framework/reduced graphene oxide composite (COF/rGO) was fabricated by facile ultrasonic self-assembly strategy and further coated onto stainless-steel wire by physically adhesion for headspace solid-phase microextraction (HS-SPME) of polycyclic aromatic hydrocarbons (PAHs) prior to their determination by gas chromatography-flame ionization detection (GC-FID). Compared with the individual porphyrin-based COF and GO, the as-prepared COF/rGO composite effectively prevented the stacking of GO nanosheets and exhibited enhanced extraction efficiency due to the synergistic effect, with the enrichment factor up to 8816 for phenanthrene. The morphology, structure, and stability of COF/rGO composite was characterized by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, and N 2 adsorption–desorption. Effective adsorption and desorption parameters including extraction temperature, extraction time, desorption temperature, desorption time, agitation speed, and ionic strength were optimized. The established HS-SPME/GC-FID method based on COF/rGO composite fiber was evaluated in terms of linear ranges from 0.5 to 250.0 ng mL −1 with R 2 ≥ 0.9985, limits of detection in the range of 0.09–0.59 ng mL −1 , and limits of quantitation in the range of 0.31–1.97 ng mL −1 . The intra-day, inter-day, and fiber-to-fiber relative standard deviations (RSDs) were in the range of 1.86–4.37%, 2.48–5.40%, and 3.51–7.81%, respectively. The established method was employed to determine trace level of PAHs in honey with good recoveries (62.99–128.8%) and reliable reproducibility (0.51–7.63%).
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TALANTA
·
2023
·
IF 6.1
Li Xu,Wei Hu,Fengshou Wu,Juan Zhang
In this work, a novel spherical metal organic framework (MOF) was first in situ grown on the surface of iron wire (IW), in which IW served as the substrate and metal source for MOF (type NH 2 -MIL88) growth without adding additional metal salts in the process, while spherical NH 2 -MIL88 provided more active sites for further construction of multifunctional composites. Subsequently, a covalent organic framework (COF) was covalently bonded to the surface of the NH 2 -MIL88 to obtain the IW@NH 2 -MIL88@COF fibers, which were used for headspace solid-phase microextraction (HS-SPME) of polycyclic aromatic hydrocarbons (PAHs) in milk samples prior to determination by gas chromatography-flame ionization detection (GC-FID). Compared with the fiber prepared by physical coating, the IW@NH 2 -MIL88@COF fiber prepared by in situ growth and covalent bonding exhibits better stability and possesses more uniform layer. The extraction mechanism of the IW@NH 2 -MIL88@COF fiber for PAHs was discussed, which mainly owed to π-π interactions and hydrophobic interactions. After optimization of the primary extraction conditions, the SPME-GC-FID method was established for five PAHs with a wide linear range (1–200 ng mL −1 ), good linearity coefficient (0.9935–0.9987) and low detection limits (0.017–0.028 ng mL −1 ). The relative recoveries for PAHs detection in milk samples ranged from 64.69 to 113.97%. This work not only provides new ideas for the in situ growth of other types of MOF, but also provides new methods for the construction of multifunctional composites.
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MOLECULES
·
2023
·Vol. 28
·期 8
·3542
·
IF 4.6
Qing Liu,Chao Yan,Yan Wang
Applications of submicron-scale particles are of rising interest in separation science due to their favorable surface-to-volume ratio and their fabrication of highly ordered structures. The uniformly dense packing beds in columns assembled from nanoparticles combined with an electroosmotic flow-driven system has great potential in a highly efficient separation system. Here, we packed capillary columns using a gravity method with synthesized nanoscale C18-SiO2particles having diameters of 300–900 nm. The separation of small molecules and proteins was evaluated in the packed columns on a pressurized capillary electrochromatography platform. The run-to-run reproducibility regarding retention time and peak area for the PAHs using a column packed with 300 nm C18-SiO2particles were less than 1.61% and 3.17%, respectively. Our study exhibited a systematic separation analysis of small molecules and proteins based on the columns packed with submicron particles combined with the pressurized capillary electrochromatography (pCEC) platform. This study may provide a promising analytical approach with extraordinary column efficiency, resolution, and speed for the separation of complex samples.Keywords:submicron scale particles;pressurized capillary electrochromatography;separation
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JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Ning Zhang,Lishen Su,Suning Man,Xiaoyun Lei,Ting Huang,Chunling Zhu,Lan Zhang,Xiaoping Wu
A direct immersion solid-phase microextraction (DI-SPME) approach for gas chromatography-mass spectrometry (GC–MS) based on hybrid fiber coating of ionic liquid and polyhedral oligomeric silsesquioxane (POSS) is presented. To fabricate the task-specific coating for the enrichment of polycyclic aromatic hydrocarbons (PAHs), 1-butyl-3-vinylimidazolium bis[(trifluoromethyl)sulfonyl]imide (IL) and POSS were rapidly photoinitiated copolymerized within 5 min on a stainless steel fiber. The high efficient extraction of target analytes can be attributed to a combined result of multiple interactions including the strong C F⋯H C pseudohydrogen bonding, π-π stacking, hydrophobic force, and molecular sieve effect. A wide linear range (0.04–400 ng L −1 ) with low detection limits in the range of 0.004 and 0.5 ng L −1 were obtained for PAHs by GC–MS. The applicability of this coupling method was successfully demonstrated by the analysis of trace PAHs in real river water and soil samples, with satisfied recoveries (84.2–108.6%) and relative standard deviations (<8.1%). Compared to the other commercial fiber-based SPME methods, the IL/POSS hybrid coating-based SPME is much cheaper, thermally stable and capable of eliminating possible deleterious effects as well.
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JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Zi-Yuan Zhao,Lei Qin,Xu-Hui Huang,Yu-Ying Zhang,Ming Du,Xian-Bing Xu,Da-Yong Zhou,Bei-Wei Zhu
The coated direct inlet probe (CDIP) is a new laboratory-made low-cost technology developed from a direct inlet probe (DIP), which has the advantage of quick enrichment/cleanup of an analyte from liquid samples. A capillary probe is coated with hydroxy-terminated polydimethylsiloxane (OH-PDMS), divinylbenzene (DVB), and β-cyclodextrin (β-CD) by a sol-gel method. This probe can be directly coupled with a commercialized atmospheric-pressure chemical ionization (APCI) ion source and high-resolution mass spectrometry, which are widely applicable, reliable, and durable. The ability to perform quantitative analyses with the use of a stable-isotope-labeled internal standard (SIL-IS) was tested by using different concentrations of acenaphthylene (ACY), acenaphthene (ACP), fluorene (FLR), fluoranthene (FLT), phenanthrene (PHE), and benzo[a]pyrene (B[a]P). Calibration curves with a coefficient of determination of R 2 ≥ 0.9982 for different polycyclic aromatic hydrocarbons (PAHs) were obtained. A limit of detection (LOD) of 0.008–0.04 ng mL −1 for PAHs was determined. The entire workflow is solvent-free and can be completed in less than 5 min, which demonstrates the advantages of this technique for quantitative analysis.
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JOURNAL OF SEPARATION SCIENCE
·
2018
·Vol. 42
·期 4
·888-896
·
IF 2.415
Tianfu Wei,Gongke Li,Zhuomin Zhang
Covalently cross-linked microporous polymers are a new class of highly cross-linked porous network materials with large surface area and potential superiority in sample pretreatment. In this work, a covalently cross-linked microporous polymer was well designed and synthesized by condensation of acylhydrazines in terephthalic dihydrazide with aldehyde groups in 1,3,5-benzenetricarboxaldehyde. The adsorption mechanism was explored and discussed based on π-π stacking interaction and steric effect. Then, a covalently cross-linked microporous polymer was employed as the adsorbent of online micro-solid-phase extraction coupled with high-performance liquid chromatography for the enrichment and analysis of trace pesticide residues in citrus fruits. The method was successfully applied to the online analysis of sugar orange and Huangdigan samples with the detection limits of 0.10–0.30 μg/kg. It was satisfactory that chlorpifos and triazophos in real sugar orange and Huangdigan samples could be actually found and quantified at concentrations of 0.20 and 0.51 mg/kg, respectively. The recoveries of sugar orange and Huangdigan samples were in the range of 70.0–103 and 74.0–119% with relative standard deviations of 0.4–9.7 and 0.5–9.2% ( n = 3), respectively. The proposed method was accurate, reliable, and convenient for the online simultaneous analysis of trace pesticide residues in citrus fruits.
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SENSORS AND ACTUATORS B-CHEMICAL
·
2018
·
IF 5.667
Bin Qiao,Yansong Li,Pan Hu,Yu Sun,Zhaozhao Si,Shiying Lu,Honglin Ren,Zengshan Liu,Ying Zhang,Lei Meng,Yu Zhou
Fluorene is a priority pollutant in water listed by U.S. Environmental Protection Agency. A fluorescent probe using Eu(III)-marked polystyrene nanoparticles (EuNPs) labelled with a monoclonal antibody (MAb) was synthesized and an immunochromatographic assay (ICA) based on the probe (EuNPs-MAb) was developed for rapid and sensitive detection of fluorene in water samples. The concentration of fluorene was inversely proportional to fluorescence intensity values of T-line in the range 0.98–62.50 ng/mL. The limit of detection (LOD) for quantitative detection of fluorene was 0.09 ng/mL. Recoveries of fluorene in various water samples ranged from 81.50% to 103.00% and coefficients of variation (CVs) were below 13%, which were in a good agreement with those of traditional ELISA (R 2 = 0.99). The assay can be performed within 30 min. The integrated ICA strip gave higher sensitivity and reliable reproducibility. It could be a potential method for rapid and sensitive detection of fluorene in water samples.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2018
·
IF 3.412
Ning Li,Di Wu,Na Hu,Guangsen Fan,Xiuting Li,Jing Sun,Xuefeng Chen,Yourui Suo,Guoliang Li,Yongning Wu
The present study reported a facile, sensitive, and efficient method for enrichment and determination of trace polycyclic aromatic hydrocarbons (PAHs) in food samples by employing new core–shell nanostructure magnetic covalent organic framework hybrid microspheres (Fe3O4@COF-(TpBD)) as the sorbent followed by HPLC-DAD. Under mild synthetic conditions, the Fe3O4@COF-(TpBD) were prepared with the retention of colloidal nanosize, larger specific surface area, higher porosity, uniform morphology, and supermagnetism. The as-prepared materials showed an excellent adsorption ability for PAHs, and the enrichment efficiency of the Fe3O4@COF-(TpBD) could reach 99.95%. The obtained materials also had fast adsorption kinetics and realized adsorption equilibrium within 12 min. The eluent was further analyzed by HPLC-DAD, and good linearity was observed in the range of 1–100 ng/mL with the linear correlation being above 0.9990. The limits of detection (S/N = 3) and limits of quantitation (S/N = 10) for 15 PAHs were in the range of 0.83–11.7 ng/L and 2.76–39.0 ng/L, respectively. For the application, the obtained materials were employed for the enrichment of trace PAHs in food samples and exhibited superior enrichment capacity and excellent applicability.
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Analytical Methods
·
2018
·Vol. 10
·期 41
·5014-5024
·
IF 2.073
Xuexiang Shi,Ning Li,Di Wu,Na Hu,Jing Sun,Xuxia Zhou,Yourui Suo,Guoliang Li,Yongning Wu
A novel magnetic covalent organic framework (Fe3O4@COF(TpDA)) material possessing a large surface area and high and regular porosity was constructed via a facile strategy and applied as a magnetic solid phase extraction sorbent for the determination of trace polycyclic aromatic hydrocarbons in edible oil and grilled meats prior to high performance liquid chromatography with diode array detection. The obtained materials were characterized by transmission electron microscopy, scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, N2 adsorption–desorption isotherms and vibrating sample magnetometry. The prepared Fe3O4@COF(TpDA) materials showed some attractive features including a large surface area (180.20 m2 g−1) and high saturation magnetization (62.28 emu g−1). The experimental parameters affecting the extraction performance including the type of eluent, amount of sorbent, and adsorption and desorption times were optimized. Under the optimized conditions, the adsorption equilibrium for polycyclic aromatic hydrocarbons could be achieved in only 10 min. The proposed method achieved low limits of detection (0.03–0.73 μg L−1 for LODs and 0.10–2.43 μg L−1 for LOQs) and good linearity (R ≥ 0.9937). The obtained materials were successfully applied to enrich polycyclic aromatic hydrocarbons in edible oil and grilled meats and showed good accuracy with recoveries in the range of 85.5–104.2%. Furthermore, the proposed method was also evaluated by different adsorption kinetic theories, and the pseudo-second-order model can explain the adsorption kinetics. The proposed method is facile, rapid, effective and selective for determination of PAHs in food samples.
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CHEMOSPHERE
·
2017
·
IF 4.208
Yong Li,Ling Long,Jing Ge,Li-xuan Yang,Jin-jin Cheng,Ling-xiang Sun,Changying Lu,Xiang-yang Yu
Polycyclic aromatic hydrocarbons (PAHs) accumulated in agricultural soils are likely to threaten human health and ecosystem though the food chain, therefore, it is worth to pay more attention to soil contamination by PAHs. In this study, the presence, distribution and risk assessment of 16 priority PAHs in rice-wheat continuous cropping soils close to industrial parks of Suzhou were firstly investigated. The concentrations of the total PAHs ranged from 125.99 ng/g to 796.65 ng/g with an average of 352.94 ng/g. Phenanthrene (PHE), fluoranthene (FLT), benzo [a] anthracene (BaA) and pyrene (PYR) were the major PAHs in those soil samples. The highest level of PAHs was detected in the soils around Chemical plant and Steelworks, followed by Printed wire board, Electroplate Factory and Paper mill. The composition of PAHs in the soils around Chemical plant was dominated by 3-ring PAHs, however, the predominant compounds were 4, 5-ring PAHs in the soils around other four factories. Meanwhile, the concentration of the total PAHs in the soils close to the factories showed a higher level of PAHs in November (during rice harvest) than that in June (during wheat harvest). Different with other rings of PAHs, 3-ring PAHs in the soils around Chemical plant and Steelworks had a higher concentration in June. The results of principal component analysis and isomeric ratio analysis suggested that PAHs in the studied areas mainly originated from biomass, coal and petroleum combustion. The risk assessment indicated that higher carcinogenic risk was found in those sites closer to the industrial park.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Li-Shun Zhang,Pei-Yao Du,Wen Gu,Qing-Li Zhao,Yan-Ping Huang,Zhao-Sheng Liu
A new lanthanide metal-organic frameworks NKU-1 have successfully incorporated into poly (BMA- co -EDMA) monolith and evaluated by capillary electrochromatography (CEC). Lanthanide metal-organic frameworks [Eu 2 (ABTC) 1.5 (H 2 O) 3 (DMA)] (NKU-1) were synthesized by self-assembly of Eu(III) ions and 3,3′,5,5′-azo benzene tetracarboxylic acid ligands have been fabricated into poly(BMA- co -EDMA) monoliths. 1-Butyl-3-methylimidazolium tetrafluoroborate and N , N -dimethylformamide were developed as binary porogen obtaining homogeneous dispersibility for NKU-1 and high permeability for monolithic column. The successful incorporation of NKU-1 into poly(BMA- co -EDMA) was confirmed and characterized by FT-IR spectra, scanning electron microscopy, X-ray diffraction, energy dispersive spectrometer area scanning, and transmission electron microscopy. Separation ability of the NKU-1-poly (BMA- co -EDMA) monoliths was demonstrated by separating four groups of analytes in CEC, including alkylbenzenes, polycyclic aromatic hydrocarbon, aniline series and naphthyl substitutes. Compared with bare monolithic (column efficiency of 100,000 plates/m), the NKU-1-poly (BMA- co -EDMA) monoliths have displayed greater column efficiency (maximum 210,000 plates/m) and higher permeability, as well as less peak tailing. The results showed that the NKU-1-poly (BMA- co -EDMA) monoliths are promising stationary phases for CEC separations.
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