ANALYTICA CHIMICA ACTA
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2024
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IF 5.7
Yiwen Han,Aikun Han,Yaqiong Qin,Yuan Tian,Bin Peng,Lijun He,Wenfen Zhang,Wenjie Zhao,Shusheng Zhang
Background Edible oils are susceptible to contamination with polycyclic aromatic hydrocarbons (PAHs) throughout production, storage, and transportation processes due to their lipophilic nature. The necessity of quantifying PAHs present in complex oil matrices at trace levels, which bind strongly to impurities in oil matrices, poses a major challenge to the accurate quantification of these contaminants. Therefore, the development of straightforward and effective methods for the separation and enrichment of PAHs in oil samples prior to instrumental analysis is paramount to guaranteeing food safety. Results A pyrazine embedded hyper-crosslinked porous polymer, HCP Pz-TPB , was synthesized via a Friedel-Crafts reaction, utilizing triphenylbenzene (TPB) as the monomer and 2,5-dibromomethylpyrazine as the cross-linking reagent. The material was combined with polydimethylsiloxane (PDMS) using the sol-gel method, and applied as a coating to a dumbbell-shaped stir bar prepared in-house. Using stir bar sorptive extraction (SBSE) combined with gas chromatography-mass spectrometry (GC-MS), 15 PAHs in edible oils were successfully quantified. Optimal conditions for the extraction of PAHs were experimentally investigated, with factors such as stirring rate, extraction time, extraction temperature, desorption solvent, and desorption time systematically optimized. The final method demonstrated a broad linear range (0.12–150 ng g −1 ), and low limits of detection (0.04–0.28 ng g −1 ). The recoveries of PAHs in real edible oil samples ranged from 83.14 % to 128.01 %, with relative standard deviations (RSDs) below 13.47 %. Significance This method simplifies PAH extraction by eliminating steps such as saponification, liquid-liquid extraction, drying, and re-dissolution, thus reducing potential analyte loss and errors associated with the inclusion of multiple pretreatment steps typical of conventional methods reported in the literature. Notably, the adsorbent materials prepared in this study can be reused up to 30 times, underscoring its sustainability. The proposed research broadens the diversity of coating choices for SBSE applications while offering a streamlined, cost-effective, and greener alternative for PAH determinations in edible oils via SBSE/GC-MS.
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JOURNAL OF HAZARDOUS MATERIALS
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2024
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IF 12.2
Sitao Wang,Xiaolan Zhang,Qingqing Zhou,Zhimin Liu,Zhigang Xu
Polycyclic aromatic hydrocarbons (PAHs) have long been globally distributed, and almost worldwide people are exposed to varying degrees of PAHs. Aqueous medium is an important transmission route of PAHs, but the detection of PAHs in aqueous environment has been a challenge. Herein, a magnetic hypercrosslinked polymer microsphere (Fe 3 O 4 @SiO 2 -PS@HCP) was developed for the effective detection of PAHs. Under the effect of multiple factors (hydrophilicity, intermolecular force and molecular volume), Fe 3 O 4 @SiO 2 -PS@HCP shows excellent performance on the enrichment of five PAHs in aqueous environment. Fe 3 O 4 @SiO 2 -PS@HCP was used to capture PAHs in city river of plateau lake. In-depth data analysis showed that factory activities and traffic emissions are the main pollution sources of PAHs. Ecological, carcinogenic and non-carcinogenic risks are almost within the safe range. The carcinogenic and non-carcinogenic risks of PAHs in children are higher than adults, which needs to be taken seriously. This method breaks the dilemma that it is difficult to enrich weakly hydrophilic pollutants in aqueous media, and complements important pathways for tracing sources of pollutants and assessing associated risks. It brings methodological enlightenment into the development of environmental pollution and human health risk assessment methodology.
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APPLIED CLAY SCIENCE
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2024
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IF 5.3
Yun Li,Xuechi Liu,Meng Han,Zhouhua Wang,Ruixin Shi,Haoqi Liao,Bao Yuan,Pengfei Wang,Songbai Han,Jinlong Zhu
To understand the occurrence of natural gas hydrates in seabed sediments, it is crucial to examine the mechanisms of methane (CH 4 ) hydrate formation in sodium montmorillonite (Na-Mt) systems in the presence of amino acid. Accordingly, this study employed kinetics experiments and molecular dynamics simulations to investigate CH 4 hydrate nucleation and growth in an Na-Mt system containing alanine (Ala), leucine (Leu), and phenylalanine (Phe), respectively. Kinetics and Raman experiments showed that, compared with Ala, Leu and Phe enhanced hydrogen bonding between water molecules surrounding Na-Mt. This enhancement was due to the long carbon chain of Leu and the phenyl ring of Phe and facilitated CH 4 hydrate formation. Moreover, in the Na-Mt system, Ala reduced CH 4 consumption, whereas Leu and Phe increased CH 4 consumption. Molecular dynamics simulations revealed that the strength of electrostatic interactions between the negatively charged Na-Mt surface and the functional groups of amino acids affected the distribution of amino acids, thereby altering CH 4 aggregation and CH 4 hydrate nucleation processes. The strong interaction between Na-Mt and Ala significantly disrupted interfacial interactions between Na-Mt and water molecules. In contrast, the weaker interactions between Na-Mt and Leu and Phe, respectively, meant that these amino acids affected CH 4 hydrate nucleation in the bulk-like solution by influencing the arrangement of water molecules. These findings indicate that interfacial interactions between Na-Mt and amino acids play a crucial role in CH 4 hydrate formation. Overall, this study generated insights into the formation kinetics and nucleation properties of CH 4 hydrates in clay mineral–amino acid complexes that may increase understanding about the occurrence of natural gas hydrates in marine sediments.
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JOURNAL OF CHROMATOGRAPHY A
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2025
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IF 4
Zichen Zhao,Ruiyang Ma,Juntao Wang,Qing Zhang,Miao Jing,Chun Wang,Qiuhua Wu,Zhi Wang
A boric acid functionalized hyper-crosslinked polymer (HCP), designated as NPCBA/TBM-HCP, was successfully synthesized via Friedel-Crafts reaction by copolymerizing N-phenylcarbazole-2-boronic acid (NPCBA) and 2,4,6-Tris(bromomethyl)mesitylene (TBM). The NPCBA/TBM-HCP showed a large surface area and a good adsorption property for phenylurea herbicides (PUHs). A method with NPCBA/TBM-HCP based solid phase extraction and high-performance liquid chromatographic detection was developed for the simultaneous analysis of PUHs in lake water, green tea drink and tomato samples. Under the optimized experimental conditions that the amount of the NPCBA/TBM-HCP was 30 mg, sample solution was 100 mL, sample loading rate was 4 mL min -1 , and eluent was 0.3 mL acetonitrile, the linear response for the PUHs was in the range of 0.06–80.0 ng mL -1 , 0.6–80.0 ng mL -1 and 0.9–200 ng g -1 for lake water, green tea drink and tomato samples, respectively, with a good linearity (the coefficients of determination ( r 2 ) ≥ 0.9916). The detection limits (S/N = 3) for lake water, green tea drink and tomato samples were 0.02–0.03 ng mL -1 , 0.2 ng mL -1 and 0.3–0.5 ng g -1 , respectively. The method recoveries for spiked samples were 80.0 %-119.1 % and RSDs were lower than 9.9 % for the determination. The method provides a new and feasible approach for the determination of phenylurea herbicide in real samples.
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Journal of Analysis and Testing
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2025
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IF 7
Li Han,Cui Yuanyuan,Zhen Changqing,Lin Xiaohui,Li Ke,Yang Chengxiong
Microporous organic network (MON) has emerged as efficient stationary phases for high-performance liquid chromatographic (HPLC) separation. Nevertheless, the inherent superhydrophobic networks made their applications limited in the reversed-phase (RP) mode. In this work, a novel amino acid L-cysteine (L-Cys) modified core-shelled microsphere MON@SiO 2 -L-Cys was synthesized via the efficient thiol-yne “click” reaction for hydrophilic interaction chromatography /reversed-phase liquid chromatography (HILIC/RPLC) mixed-mode chromatographic separation. Baseline separation of various hydrophilic and hydrophobic compounds including aromatic ketones, phthalate esters, alkylbenzenes, amines, polycyclic aromatic hydrocarbons, phenols, nucleosides, nucleic acid bases, sulfonamides, water-soluble vitamins, cephalosporin antibiotics, and estrogens was realized on MON@SiO 2 -L-Cys packed column based on the predesigned mixed-mode retention mechanisms. The MON@SiO 2 -L-Cys packed column also exhibited higher selectivity compared to bare SiO 2 , MON@SiO 2 without L-Cys, and C 18 packed columns, revealing the synergistic interactions of MON’s networks and the modified L-Cys molecules. This work provided a feasible way to construct a novel amphipathic MON-based stationary phase, broadened the application scope of MON for hydrophilic analytes, and uncovered the prospects of MON in mixed-mode HPLC.
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LANGMUIR
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2024
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IF 3.7
Chunyang Liu,Yanrong Cheng,Delan Ge,Ju Xie,Xia Guo
Aqueous two-phase systems (ATPS) are considered a new type of green separation system, but their low selectivity to target molecules limits their practical application. In this study, we used surfactant@MWCNT as an adjuvant to improve the selectivity of PEG/(NH4)2SO4 ATPS. The surfactants used include Triton X-100 (TX-100), Tween 80, sodium dodecyl sulfate (SDS), sodium dodecyl benzenesulfonate (SDBS), and bis(2-ethylhexyl)sulfosuccinate sodium salt (AOT). Nine aromatic compounds, including syringic acid, vanillin, tryptophan, phenylalanine, tyrosine, mandelic acid, theophylline, theobromine, and cephalexin, were selected as model extracts. The results showed that the use of the surfactant@MWCNT composite as an adjuvant significantly improved the selectivity of the ATPS toward syringic acid among the nine extracts. Moreover, the selectivity of the ATPS for syringic acid with the TX-100/MWCNT composite as the adjuvant is better than that with the Tween 80/MWCNT composite as the adjuvant, followed by that with the anionic surfactant/MWCNT composite as the adjuvant. The enhanced selectivity of ATPS by the surfactant/MWCNT composite is ascribed to the spatial effect and the electrostatic and hydrophobic interactions between the extract and the surfactant adsorbed on the MWCNT.
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Journal of Environmental Chemical Engineering
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2025
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IF 7.2
Guangyu Dong,Liushan Jiang,Linchun Nie,Jiawei Liao,Xiaodie Geng,Wenjing Liu,Dejing Meng,Meiling Xu,Na Liu,Qingxiang Zhou,Chunmao Chen
In this study, a magnetic covalent organic framework composite (Fe 3 O 4 @COF-BTCA-TMB) was conceived and synthesized with benzene-1,3,5-tricarbaldehyde and 3,3’,5,5’-tetramethyl benzidine as monomers. The modification of COF endowed the magnetic composite with a large number of functional groups and benzene rings, which exhibited high affinity to polycyclic aromatic hydrocarbons (PAHs) attributed to π-π conjugation and hydrophobic interaction. Based on these properties, it was utilized to conceive a highly efficient magnetic solid phase extraction method to enrich PAHs from water samples prior to high performance liquid chromatography analysis. The key factors that affect the extraction efficiencies of six PAHs in water samples were explored. Under the optimized conditions, six PAHs obtained good linearity in wide concentration ranges of 0.2–80 μg L −1 , 0.2–180 μg L −1 , and 0.2–240 μg L −1 , respectively. The limits of detection (LODs) ranged from 0.03 to 0.09 μg L −1 , and the enrichment factors were in the range of 107–149. The adsorption of PAHs on Fe 3 O 4 @COF was consistent with the quasi-second-order kinetic model, and Freundlich adsorption isotherm model. The conceived method was evaluated with real water samples and satisfactory recoveries (73.8 % ∼ 100.5 %) were obtained, indicating that it was simple, robust and efficient, and could be optioned for monitoring trace PAHs in environment.
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JOURNAL OF MOLECULAR LIQUIDS
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2024
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IF 5.3
Lei Tian,Mengni Pan,Cuiping Ye,Hongbo Hao,Wenying Li
Phenanthrene (Phe) and fluorene (Flu) are crucial chemical intermediates with applications in materials, medicine, and pesticides. However, conventional separation methods struggle to effectively isolate phenanthrene from fluorene due to their similar physical properties. To address this challenge, a reaction–separation coupling technique was employed to convert fluorene into 9-fluorenone (9-Fluo), followed by the separation of phenanthrene from 9-fluorenone using solvent-cooling crystallization. Initially, the relative solubilities of phenanthrene and 9-fluorenone in 2072 solvents were calculated using COSMO-RS for preliminary screening. Among various conventional short-chain aliphatic alcohols and low-carbon saturated hydrocarbons, methanol, and cyclohexane were identified as the most effective solvents based on their solubility selectivity (SS). The molecular interactions between phenanthrene or 9-fluorenone and these solvents were analyzed using theoretical methods such as σ-potential/profile, infinite dilution activity coefficients in COSMO-RS, and Hansen solubility parameters, with further confirmation from FTIR tests. The optimal liquid–solid ratios were determined using both phase diagram measurements and solubility calculations. The reaction conversion of fluorene to 9-fluorenone was complete regardless of the raw material used. Phenanthrene and 9-fluorenone were effectively separated using methanol and cyclohexane with optimum liquid–solid mass ratios of 1.6:1 and 2.8:1, respectively. In the model mixture, the contents of phenanthrene and 9-fluorenone exceeded 98 wt%, with yields above 91 wt%. For anthracene residue, the content of 9-fluorenone reached 93.98 wt% with a yield of 84.52 wt%, while its content was only 76.58 wt% due to the accumulation of other components in phenanthrene.
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PEDOSPHERE
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2024
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IF 5.2
Xiaonuo ZHANG,Yaxi DENG,Goujian CHI,Hong LÜ,Hongxia ZHAO
ABSTRACT Rhizoremediation has emerged as a burgeoning approach for the removal of petroleum hydrocarbons (PHCs) from soil, with a primary emphasis on terrestrial plant systems. However, the mechanism on how soil microbiomes influence the dissipation of PHCs within a hygrophyte planting system has yet to be fully elucidated. This work concentrated on investigating the potential evolution of soil microbiomes and their effect on the PHCs dissipation within the Suaeda salsa (L.) Pall. planting system using the pot experiment. Two representative compounds, namely polycyclic aromatic hydrocarbons (PAHs) and n-alkanes, were used as target PHCs. The findings revealed a significant efficiency in the dissipation of petroleum hydrocarbons (PHCs) in soil, particularly with respect to n-alkanes. The high dissipation efficiency of PHCs was the synergistic result of both the root accumulation and the microbial biodegradation. The key microbes involved in PHCs dissipation were revealed, with the dominant phylum of Protobacteria and genus of Salinimicrobium . The alterations in microbial diversity and abundance were closely associated with the root exudation and PHCs exposure. Significant differences in enzyme activity, which serves as an indicator of soil health and fertility, were observed between the rhizospheric and non-rhizospheric soil, attributed to root exudation. This study offers novel insights into the phytoremediation potential for Suaeda in PHC-contaminated soil and serves as a valuable scientific reference for the phytoremediation of such soils.
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CHEMICAL ENGINEERING SCIENCE
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2024
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IF 4.1
Ze-Min Zhao,Yu Zhang,Yu Chen,Jieying Jing,Wen-Ying Li
Nickel–aluminum (Ni–Al) spinel catalysts with distinct Ni/Al molar ratios were synthesized to construct Ni 2+ coordination sites. Owing to the favorable distribution of Ni 2+ coordination sites and the presence of suitable concentration of Ni 2+ in octahedral sites, Ni/Al-0.725 catalyst achieved an 86.1 % average yield of perhydrophenanthrene, which was higher than that obtained with Ni/Al-0.25 (6.3 %). Characterization results indicated that Ni 2+ of the Ni/Al-0.725 catalyst was present in octahedral sites and ∼ 40.4 % Ni 2+ was reduced to Ni, whereas the active Ni metal of Ni/Al-0.25 catalyst mainly comprised Ni 2+ occupying tetrahedral sites as precursors. Furthermore, the Ni/Al-0.725 catalyst exhibited the smallest Ni particle size (2.82 nm) and the largest Ni available surface (19.62 m 2 /g sample ), which helped alleviate competitive adsorption among aromatic hydrocarbons. The Ni reduced by the spinel catalysts was in an electron-deficient state, which enhanced the adsorption of polycyclic aromatic hydrocarbons.
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Journal of Environmental Chemical Engineering
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2024
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IF 7.4
Liwei Ma,Shihua Zheng,Guoqiang Li,Xuejun Wang,Kangdi Chen,Guojie Zhang
Fe(II)EDTA can remove NO efficiently, but it has not been industrially applied. This is because the oxygen present in the flue gas will oxidize Fe(II)EDTA and Fe(II)EDTA-NO to Fe(III)EDTA and deactivate them. In order to solve this problem, this paper innovatively proposes to use NaHS to reduce Fe(III) EDTA, because NaHS has high reducing ability and low price. Therefore, a series of experimental conditions were explored in order to obtain the best reaction setup. The results indicate that increasing the concentrations of NaHS, temperature, and pH enhances the rate of NaHS reduction. The mechanism of the increase in reduction rate was studied in depth using potentiometric titration. It was found that an increase in OH - concentration will generate S 8 precipitate, which is beneficial to the forward progress of the reaction and promotes the large-scale production of the active component Fe 2+ . Oxygen is an inevitable factor in actual flue gas, so this study innovatively proposed a kinetic model under aerobic conditions and used this model to predict the trend of Fe(III)EDTA reduction by NaHS. On this basis, NO removal experiments were conducted under high oxygen conditions. After 15 cycles, the reduction performance of NaHS was still very high, and the NO removal rate was higher than 70%. The reason for this phenomenon is that the stabilizer exists in a form that is conducive to the removal of NO by the active component Fe 2+ . Therefore, this study provides theoretical guidance for promoting the industrial application of Fe(II) EDTA technology for NO removal.
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APPLIED CATALYSIS A-GENERAL
·
2024
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IF 4.7
Meng Xia,Shuai Zhang,Kaihao Xu,Chengxue Zhang,Xiaocong Wang
In arid and semi-arid areas, the remediation of saline-alkaline soils polluted by organic contaminants is challenging. In this study, the adsorption–photocatalysis synergistic removal of organic contaminants was realised using the MIL-88A(Fe) catalyst, and the saline-alkaline soils were remediated simultaneously. The adsorption isotherm of catalyst conformed to Langmuir model, and the photocatalytic degradation of PHE in an optimal visible light system achieved a PHE degradation efficiency of up to 86.2 % within 30 min. Based on the identification of active oxygen species, the PHE photocatalytic degradation was primarily driven by holes (h + ) and superoxide radicals (·O 2 - ), followed by hydroxyl radicals (·OH) and singlet oxygen ( 1 O 2 ). Furthermore, the determined physical and chemical properties of the saline-alkaline soils indicated that the soil pH value decreased to 6.82, effectively increasing the absorbable nitrogen content and improving soil fertility. This study offers a new strategy for the removal of organic contaminants under special soil medium conditions.
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