MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 7
·2171-2180
·
IF 4.58
Wu Tong,Wang Juntao,Liang Weiqian,Zang Xiaohuan,Wang Chun,Wu Qiuhua,Wang Zhi
The authors describe a three-dimensional single layer graphitic carbon nitride-modified graphene composite (g-C 3 N 4 @G) deposited on a stainless steel wire by a sol-gel technique. The coated fiber was applied to direct immersion solid-phase microextraction of trace levels of polycyclic aromatic hydrocarbons (PAHs) from cosmetics samples prior to their determination by gas chromatography with mass spectrometry (GC-MS). Due to π stacking interaction and hydrophobic interaction between the g-C 3 N 4 @G coating and the analytes (naphthalene, acenaphthene, fluorene, phenanthrene, fluoranthene and pyrene), the fiber displays an excellent adsorption capability for the analytes. Under optimized conditions, the method has a wide linear range, low LODs (from 1.0 to 2.0 ng L −1 ), good repeatability and high recoveries. It was successfully applied to the determination of PAHs in cosmetics. The g-C 3 N 4 @G fiber also exhibited good durability.
Schematic of a three-dimensional single layer graphitic carbon nitride-modified graphene composite (g-C 3 N 4 @G) that was coated onto a stainless steel wire for the direct-immersion solid phase microextraction of trace levels of polycyclic aromatic hydrocarbons prior to gas chromatography-mass spectrometric detection.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Nan Dong,Tao Li,Yujie Luo,Lin Shao,Zhu Tao,Chun Zhu
A novel solid-phase microextraction coating that contains perhydroxy cucurbit[6]uril((OH) 12 Q[6]) was prepared by a sol–gel method. (OH) 12 Q[6] was used as a starting coating material with hydroxy-terminated poly(dimethylsiloxane) (OH-PDMS) to bond chemically to a fused-silica substrate using 3-(2-cyclooxypropoxyl)propyltrimethoxysilane as cross-linking agent; hydrolysis and polycondensation reactions then led to the formation of a (OH) 12 Q[6]/PDMS-coating. The coating has a high thermal stability (360 °C), long lifetime and can withstand organic and inorganic solvent rinsing because of the chemical binding between the coating and silica substrate. Its performance was tested by headspace (HS) solid-phase microextraction fiber coupled with gas chromatography to determine polycyclic aromatic hydrocarbon (PAHs) compounds in water samples. The (OH) 12 Q[6]/PDMS-coated fiber exhibited higher enrichment factors from fourfold for naphthalene to tenfold for pyrene compared with commercial PDMS fiber, and the enrichment factors increased with the number of condensed PAH rings. The strong adsorption affinity is believed to be attributed to hydrogen bonding and C H⋯π interactions between PAHs and (OH) 12 Q[6], according to the results of quantum chemical calculations. In the PAH analysis, the (OH) 12 Q[6]-coated fiber showed a good repeatability (< 4.7%) and reproducibility between fibers (< 9.4%), low detection limits (0.03–0.15 μg L −1 ), and a wide linearity (0.1–1000 μg L −1 ) under optimized conditions. This method was used for the simultaneous determination of seven PAHs with satisfactory recoveries of 90.56%–107.4% for Huaxi river water samples and 90.23%–109.5% for local wastewater samples, respectively.
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SCIENCE OF THE TOTAL ENVIRONMENT
·
2024
·
IF 8.2
Qian Zhang,Xinyan Xu,Chenzhuo Song,Dengke Zhang,Yi Kong,Xinyi Cui
Tire wear particles (TWP), as an emerging type of microplastics, are a significant source of contaminants in roadside soils due to their high concentration of pollutants, including polycyclic aromatic hydrocarbons (PAHs). This study explored the impact of ultraviolet (UV) exposure and natural aging on the in vitro bioaccessibility of PAHs associated with TWP in soil on a China-wide scale. Our findings suggested that UV exposure amplified the negative charge of TWP by 75 % and increased the hydrophobic groups on the particle surface. The bioaccessibility of 3- and 4-ring PAHs in TWP was significantly ( p < 0.05) heightened by UV exposure. After 20 types of soils containing 2 % UV-exposed TWP underwent natural aging, the bioaccessibility of PAHs saw a significant decrease ( p < 0.05) to 16–48 %, compared to 28–96 % in the unaged group. Soil pH and electrical conductivity (EC) were the two primary soil properties positively influencing the reduction of in vitro PAHs concentration and PAHs bioaccessibility. According to the prediction results, soils in southern China presented the highest potential region for the release of bioaccessible PAHs from TWP, highlighting the regional specificity of environmental impact. Our study provides valuable insights into the biological impact of PAHs associated with TWP on a regional scale, and offers scientific evidence for targeted soil risk management strategies.
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Chemosensors
·
2024
·Vol. 12
·期 10
·220
·
IF 3.7
Ting Hu,Yitao Xia,You Wang,Li Lin,Rong An,Ling Xu,Xiangdong Qing
Polycyclic aromatic hydrocarbons (PAHs) are a group of organic compounds that are both toxic and hazardous to human health and ecological systems. In recent work, a novel analytical strategy based on the chemometric-assisted HPLC-DAD method was proposed for the quantification and source apportionment of eight PAHs in PM10 samples. Compared to traditional chromatographic methods, this approach does not require the purification of complex PM10 samples. Instead, it utilizes a mathematical separation method to extract analytes’ profiles from overlapping chromatographic peaks, enabling precise quantification of PAHs in PM10. Firstly, 40 PM10 samples collected in Loudi city during two sampling periods were used for analysis. Subsequently, the second-order calibration method based on alternating trilinear decomposition (ATLD) was employed to handle the three-way HPLC-DAD data. Finally, the pollution sources of PAHs were analyzed by the feature component analysis method according to the obtained relative concentration matrix. For the validation model, the average recoveries of eight PAHs were between (88.8 ± 7.6)% and (105.6 ± 7.5)%, and the root-mean-square errors of prediction ranged from 0.03 μg mL−1to 0.47 μg mL−1. The obtained limits of quantification for eight PAHs were in the range of 0.0050 μg mL−1to 0.079 μg mL−1. For actual PM10 samples, results of the feature component analysis indicated that the main source of PAHs in PM10 may be traffic emissions and coal combustion. In summary, the proposed method provided a new and rapid analysis method for the accurate determination and source apportionment of PAHs in atmospheric aerosols.
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JOM
·
2024
·
IF 2.1
Yu Shi,Pan Hong,Ju Jianbin,Xia Guangping,Huang Yipeng,Ruan Guihua,Jiang Fuyang
In this study, carbon spheres decorated with nickel nanoparticles (ACS@Ni NPs) were prepared through arginine-assisted hydrothermal treatment, followed by high-temperature carbonization in a nitrogen atmosphere. ACS@Ni NPs displayed uniform size and excellent monodispersity. The specific surface area increased from 9.03 m 2 /g to 428.69 m 2 /g after carbonization. The ACS@Ni NPs were employed as adsorbents in dispersive magnetic solid phase extraction (d-MSPE) to extract methylnaphthalene and acenaphthene. The adsorption capacities of ACS@Ni NPs for methylnaphthalene and acenaphthene were 1592.75 μg g −1 and 1652.83 μg g −1 , respectively. In addition, ACS@Ni NPs sustained adsorption efficiencies > 90% even after ten reuse times. Coupled with high-performance liquid chromatography-ultraviolet detection technology, under the optimum experimental conditions, the detection limits of methylnaphthalene and acenaphthene were 0.58 and 0.12 ng mL −1 . The recoveries of methylnaphthalene and acenaphthene in all samples remained > 95%, with relative standard deviations < 4.5%. The results indicated that ACS@Ni NPs could be applied in environmental pollution treatment and sample preparation.
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ANALYTICA CHIMICA ACTA
·
2025
·
IF 6
Ting Wang,Yuan-Yuan Cui,Cheng-Xiong Yang
Background As a class of boomingly developed porous material, microporous organic networks (MONs) demonstrated great prospects in HPLC because of their unique structures and excellent stabilities. However, the agglomerated, irregular, and sub-micron sized MONs obtained via the traditional synthesis methods inevitably cause high column pressure and low column efficiency, rendering the main obstacles for their applications in HPLC. Monolithic column has the characteristics of continuous porous structure, fast mass transfer rate, excellent permeability, and low column pressure. Therefore, the integration of MONs with monolithic column should be a potential way to extend the widespread applications of MONs in HPLC. Results In this work, we reported the first example of fabricating MON incorporated monolithic columns by employing methacrylic acid as the monomer, ethylene dimethacrylate as the cross-linking agent, and polyethylene glycol-6000 as the porogen for the improved HPLC separation of small organic molecules. Effects of preparation conditions for MON incorporated monolithic column, sample loading mass, column temperature, and mobile phase composition were studied in detail. MON monolithic column after MON incorporation exhibits improved permeability, column efficiency, hydrophobicity, and specific surface area. Diverse small organic molecules such as polycyclic aromatic hydrocarbons, alkylbenzenes, acidic phenols, basic amines, phenylurea herbicides, parabens, phthalates, and flavonoids were successfully separated on MON incorporated monolithic column (50.0 mm length × 4.6 mm i.d.). MON incorporated monolithic column also provided better resolution and selectivity than C18 packed column. Significance This work reported the first combination of MON and monolithic column for efficient HPLC separation of variety small organic compounds with good resolution, selectivity, and precisions based on typical reversed phase mechanism. The experimental results demonstrated the great potential of MON incorporated monolithic column for enhanced HPLC separation of small organic compounds and could extend the new applications of MONs in separation science.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Xiaomin Li,Mingxia Sun,Yang Feng,Yanming Liu,Yanli Wang,Juanjuan Feng,Min Sun
A covalent organic framework (COF) was gown on porous silica with 1,3,5-tri(4-aminophenyl)benzene and 2,5-divinyl-1,4-phenyldiformaldehyde as monomers, and two ionic liquids were grafted to COF by a click reaction. The materials before and after the modification of ionic liquids were separately packed into solid-phase extraction columns (10 × 4.6 mm, i.d.), which were coupled with liquid chromatography to construct online analysis systems. The extraction mechanisms of polycyclic aromatic hydrocarbons, bisphenols, diphenylalkanes and benzoic acids were investigated on these materials. There were π-π, hydrogen-bond and electrostatic interactions on ionic liquid-functionalized sorbents. After the comparison among these materials, the best sorbent was used, and the analytical method was established and successfully applied to the detection of some estrogens from actual samples. For the analytical method, the detection limit was as low as 0.005 μg L −1 , linear range was as wide as 0.017–10.0 μg L −1 , and enrichment ratio was as high as 3635. The recoveries in actual samples were 70 %-129 %.
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JOURNAL OF APPLIED POLYMER SCIENCE
·
2024
·Vol. 141
·期 27
·e55594
·
IF 2.7
Zhen Zhang,Yue Wang,Shuai Lv,Hailin Cong,Youqing Shen,Bing Yu
In this work, a two-step activated swelling technique was effectively employed to successfully synthesize monodisperse porous poly(styrene-divinylbenzene) (PS-DVB) particles. Diazoresin (DR) transform an ionic bond into a covalent bond by photoreaction. Under ultraviolet irradiation, DR was used to covalently attach dichlorophenyl isocyanate to sulfonated PS-DVB microspheres. The novel photo-crosslinking reaction effectively overcomes the toxicity issues associated with conventional coupling agents and enables green production of chromatographic fillers. Modified PS-DVB particles were indeed commonly used as filler material for the separation of chiral compounds by high performance liquid chromatography (HPLC). The porous modified microspheres designed effectively separate benzoone, DL-mandelic acid, 2-phenylcyclohexanone, ibuprofen, 2-hydroxyl flavone, DL-cysteine, chloraniline maleate, hesperidin, and other chiral compounds by 100 mm column. It is noteworthy that the isocyanate-chitin modified microspheres are effective in separating chiral drugs (1000 μg/mL) within 5 min. Compared with ordinary microspheres, porous isocyanate-chitin modified microspheres showed better separation efficiency under the same conditions. The enhancement is attributed to the increase in their specific surface area. Consequently, they are a better choice of chromatographic packing matrix.
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Journal of Analysis and Testing
·
2025
·
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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JOURNAL OF MOLECULAR LIQUIDS
·
2024
·
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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Water
·
2024
·Vol. 16
·期 17
·2537
·
IF 3
Bo Li,Hulong Liu,Xiaona Liu,Li Han,Jing Yang,Lingke Kang,Liuyuan Tang,Tianwei Qian
Bioremediation is a promising technique owing to its effectiveness, low cost, and environmental friendliness. Previous studies have focused on the degradation efficiency of polycyclic aromatic hydrocarbons (PAHs) in soil and water. However, the expression of PAH-catabolic genes in organisms involved in the degradation process has been rarely and unsystematically reported. In this study, a PAH-degrading strain—Pseudomonas aeruginosa(PQ249631)—was successfully isolated from coking-contaminated soil and used for PAH degradation in soil and water. Furthermore, the degradation of PAHs (naphthalene, fluorene, phenanthrene, anthracene, and pyrene) was investigated in single, binary, and mixture systems to explore the interaction of substrates. The results showed that when naphthalene was used as a cometabolite carbon source, the removal rates of fluorene, phenanthrene, anthracene, and pyrene increased from 14.33%, 17.25%, 6.61%, and 4.47% to 72.08%, 100.00%, 15.63%, and 6.63%, respectively. In a PAH mixture, the degradation rate of each PAH was higher when naphthalene, rather than glucose, was used as the cometabolite carbon source. Transcriptome analysis revealed significant differential expression of PAH-catabolic genes and ATP-binding cassette transporter-related genes under naphthalene stress. The enhanced degradation of PAHs could be attributed to the augmentation of the PAH metabolic pathway and membrane transportation, facilitating the transfer of PAHs to bacteria. These findings underscore the effectiveness ofP. aeruginosaas a PAH degrader and provide molecular insights into enhancing PAH degradation.
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JOURNAL OF HAZARDOUS MATERIALS
·
2024
·
IF 12.2
Yixin Kuang,Suxin Zhou,Yuefan Liu,Xiaoying Feng,Luyi Chen,Juan Zheng,Gangfeng Ouyang
The size of the adsorbent has the potential to influence extraction performance, but the size effect at the nanoscale is still poorly understood. In this study, organic-inorganic hybrid nanospheres (OIHNs) with controllable nanoscale sizes of 30, 50, and 100 nm were successfully prepared. These materials were further fabricated as solid phase microextraction (SPME) coatings with similar thicknesses, and coupled with gas chromatography-mass spectrometry (GC-MS) to investigate their extraction performance. The results showed that the extraction capacities of OIHNs for chlorobenzenes (CBs) and polycyclic aromatic hydrocarbons (PAHs) were much better than those of their corresponding derived carbon materials, despite the smaller specific surface areas and lower porosities of them. In addition, the enrichment performance increased significantly with decreasing particle size, and the OIHN-30 coating demonstrated the best performance, with enrichment factors ranging from 1098 to 6853 for CBs. Finally, a highly sensitive and practical analytical method was established with a wide linear range of 0.5–5000 ng·L −1 , and the limits of quantification (LOQs) were 0.43–1.7 ng·L −1 . The determinations of ultratrace CBs in five marine water samples and five fresh water samples were realized successfully. This study is expected to contribute to a deep understanding of the environmental effects of nanoparticles and the design of high-performance adsorbents.
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