Scientific Reports
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2026
·
IF 4.9
Zhang Kaige,Wang Jing,Chen Yanrong,He Lijun,Zhang Qianchun
Ferrofluids are innovative functional media combing magnetic nanoparticles with liquid fluidity. In this study, a hydrophobic deep eutectic solvent-ferrofluid was prepared by dispersing oleic acid-coated magnetic nanoparticles in hydrophobic deep eutectic solvent composing of DL-menthol and lauric acid, and applied for magnetic assisted liquid–liquid microextraction of trace polycyclic aromatic hydrocarbons (PAHs) from water and food samples. Following microextraction, phase separation was achieved rapidly using an external magnetic field, eliminating the need for time-consuming steps such as centrifugation or ice baths. The material’s structure was characterized by X-ray diffraction and infrared spectroscopy, while its magnetic properties were examined with a vibrating sample magnetometer. Extraction parameters were systematically screened and optimized using Plackett–Burman and Central Composite design experiments. Under optimized conditions, the limits of detection and quantification were 0.05–0.2 µg L − 1 and 0.1–0.5 µg L − 1 , respectively, with intra-day and inter-day relative standard deviations ( n = 5) below 1.6% and 1.7%. The extraction mechanism was further explored using density functional theory. Then, this method was successfully applied to determine of PAHs from environmental water and food samples, achieving spiked recoveries of 85.9–103.0%. Its greenness and practical applicability demonstrate its potential for food analysis and environmental monitoring.
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ANALYTICA CHIMICA ACTA
·
2026
·
IF 6.1
Yali Yang,Hui Ding,Kaijun Quan,Hongwei Zhao,Mingxia Sun,Zhimin Yang,Xiuhui Liu,Hongdeng Qiu,Jia Chen
Background To address the limitations of traditional single-mode stationary phases in separating complex samples, mixed-mode or multi-mode chromatographic stationary phases, which can provide two or more interaction mechanisms, have attracted extensive research interest. Among them, sulfonated pyrene derivatives present a promising candidate ligand, as they synergistically retain the hydrophobicity and π-π interaction capability of the pyrene moiety along with the hydrophilicity and strong cation-exchange capacity provided by the sulfonic acid groups. This synergistic multi-mechanism design significantly enhances separation selectivity for diverse and complex components. Results A pyrene trisulfonic acid-functionalized silica stationary phase (Sil-PyTSa) was successfully prepared and evaluated. In hydrophilic interaction liquid chromatography (HILIC) mode, Sil-PyTSa could efficiently separate nucleobases and nucleosides, ginsenosides, and alkaloids. For nucleobases and nucleosides, it utilized hydrophilic, electrostatic, and π-π interactions, showing superior retention and selectivity over a control HILIC column. In reversed-phase liquid chromatography (RPLC) mode, favorable separation of PAHs was achieved via hydrophobic and π-π interactions, enabling faster analysis and lower solvent consumption than a C18 column. In ion-exchange chromatography (IEC) mode, baseline separation of 14 rare earth elements (REEs) and removal of Fe/U impurities were accomplished. The column efficiency reached 95,920 N/m for naphthalene. Additionally, Sil-PyTSa achieved effective separation for REEs and iron (Fe) in a simulated NdFeB leaching solution and detected nucleobases and nucleosides in Angelica, indicting promising potential for analyzing complex matrices. Significance and novelty This work developed a novel multi-mode chromatographic stationary phase with multiple interactions mechanisms to enable high-performance separations in HILIC, RPLC, and IEC modes. It demonstrates good separation efficiency and selectivity, low solvent consumption, and high stability. This offers a versatile and green solution for the separation of complex samples with diverse analytes.
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Journal of Water Process Engineering
·
2025
·
IF 6.7
Xianxian Sheng,Tianliang Wang,Guilu Zeng,Xiang Zhang,Mudassir Habib,Shuguang Lyu
In the advanced oxidation process (AOPs) induced by sodium percarbonate (SPC), reactive oxygen species (ROS) can be scavenged by a large amount of dissolved Fe(II) released within a short time. To address this issue, a slow-release Fe(II) process is proposed in this study, thereby enhancing the degradation of contaminants. SPC/Fe(III)/amorphous boron (B) and SPC/Fe(III)/citric acid (CA) procedures were employed to remove polycyclic aromatic hydrocarbons (PAHs), with B as the reductant and CA as the chelator. Fluoranthene (FLT) removal in SPC/Fe(III)/B process contributed to HO•, while HO• and O 2 − • were responsible for FLT degradation via SPC/Fe(III)/CA system. SPC/Fe(III)/CA system exhibits more adaptability to intricate water quality circumstances compared to SPC/Fe(III)/B system. The bio-toxicity of FLT and their degradation intermediates was evaluated via the Toxicity Estimation Software Tool (T.E.S.T.), revealing a reduction in oral rat LD50, developmental toxicity, mutagenicity, and bioconcentration factor of the degradation intermediates relative to FLT. Both amorphous B- or CA-assisted SPC/Fe(III) processes were shown to be eco-friendly through luminosity inhibition tests with Vibrio fischeri . Experiments on soil slurry revealed that SPC/Fe(III)/CA system was feasible for the removal of complex PAHs, directing the SPC-induced AOPs process for the remediation of PAHs contaminated soils and groundwater.
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Food Analytical Methods
·
2026
·Vol. 19
·期 1
·61
·
IF 3
Huang Lei,Zhang Qiaoling,Zhao Yiwei,Ye Xilei,Chen Huaixia,Dang Xueping
In this study, the Cu 7 Mn 2 bimetallic cluster was synthesized via a solvothermal method using copper (II) chloride dihydrate (CuCl 2 ·2H 2 O) and manganese (II) chloride tetrahydrate (MnCl 2 ·4H 2 O) as the metal centers, and 1,2-cyclohexanediamine-N,N′-bis-(3-carboxylsalicylide) as the ligand. Subsequently, the Cu 7 Mn 2 bimetallic cluster fiber coating was prepared using a physical coating method and applied for the solid phase microextraction (SPME) of 7 polycyclic aromatic hydrocarbons (PAHs). The coating was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, thermogravimetric analysis, and contact angle measurement. Based on adsorption isotherms and density functional theory (DFT) calculation, the adsorption mechanism was speculated to be hydrophobic interaction, π-π stacking, and N − H···π interaction. The coating exhibited higher extraction efficiency for 7 PAHs than the Cu cluster, Mn cluster, commercial PDMS, and PDMS/CAR fiber coatings. Under the optimized extraction conditions, an SPME-HPLC method was developed for the determination of 7 PAHs in corn oil, sesame oil, blended oil, and rapeseed oil. The linear ranges of the method were 1.0 − 1000 µg·kg –1 for naphthalene, 0.1 − 1000 µg·kg –1 for anthracene, phenanthrene, and pyrene, 3.0 − 1000 µg·kg –1 for fluorene, 0.3 − 1000 µg·kg –1 for fluoranthene, and 1.5 − 1000 µg·kg –1 for 1-methylnaphthalene ( R 2 > 0.99), respectively. The limits of detection (LODs, S/N = 3) and the limits of quantitation (LOQs, S/N = 10) were in the ranges of 0.030 − 1.0 µg·kg –1 and 0.10 − 3.0 µg·kg –1 , respectively. The precisions (RSDs) were less than 10.0% and the recoveries were in the range of 82.9 − 115.2%. These results demonstrate that the Cu 7 Mn 2 bimetallic cluster coating is an effective SPME adsorbent for separation and sensitive determination of PAHs in edible oils. Graphical
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MOLECULES
·
2023
·Vol. 28
·期 8
·3542
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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 Environmental Chemical Engineering
·
2023
·
IF 7.7
Shiyu Bao,Likun Zhao,Yuanwen Liu,Lewei Yang,Peng Liu,Chaoqi Chen,Xuhui Mao
Polycyclic aromatic hydrocarbons (PAHs) are a group of contaminants with low bioavailability and biodegradability . As a result, removing PAHs from contaminated soils is often inefficient. In this study, soils spiked with fluoranthene and pyrene were inoculated with Aeromonas sp. BCP-3, a newly isolated strain from coke-plant sludge , and treated in slurry bioreactors . The removal of PAHs was significantly affected by aeration rate, slurry water-soil mass ratio, stirring rate, temperature, and the concentration of Tween-80. Such effects were attributed to changes in BCP-3 growth, PAHs solid-liquid mass transfer, and slurry particle size. Notably, under optimal conditions (i.e., aeration rate of 1.5 L/min, temperature of 30 °C, stirring rate of 200 rpm, water-soil mass ratio of 1.5:1, and Tween-80 concentration of 1.3 %), 96.3 % and 97.2 % of initially spiked fluoranthene and pyrene were removed within 12 days, respectively. A PAH-contaminated soil was collected from a local coking plant and treated under the same conditions, except for the Tween-80 concentration. For the real soil, the Tween-80 concentration was 4 % to ensure a significant proportion of PAHs released into the liquid phase. Twenty-one days after inoculation of BCP-3, the removal efficiencies of low molecular weight PAHs and high molecular weight PAHs were 82.2 % and 51.8 %, respectively. The removal efficiencies of PAHs were significantly higher than the slurry without BCP-3 or HgCl 2 -sterilized slurry. BCP-3 improved the bioavailability and biodegradability of PAHs, resulting in effective PAH removal in slurry bioreactors . Overall, successful bioaugmentation was achieved with the addition of Tween-80 and the optimization of operating conditions.
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SCIENCE OF THE TOTAL ENVIRONMENT
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2023
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IF 9.8
Zan Wang,Haiyang Hu,Zhan Zhang,Yongming Xu,Ping Xu,Hongzhi Tang
Polycyclic aromatic hydrocarbons (PAHs) and heterocyclic derivatives are organic pollutants which threaten ecosystems and human beings. In this study, a new strain, Shinella sp. FLN 14, was isolated and characterized. It can utilize fluorene as its sole carbon source and effectively co-metabolize multiple PAHs and heterocyclic derivatives, including phenanthrene , acenaphthene, and fluoranthene . Two possible metabolic pathways are proposed (i.e., salicylic acid pathway and phthalic acid pathway). Whole-genome sequencing revealed that strain FLN14 possesses a chromosome and four plasmids. However, when combined with ensemble genetic information, novel fluorene-degrading functional gene clusters were not located within the genome of FLN 14, except for some new dioxygenases and electron transport chains, which typically initiate the oxidation of aromatic compounds. In wastewater bioremediation, strain FLN14 removed nearly 95 % of PAHs within 5 days and maintained high degrading activity during the 18-day reaction compared to the control. Overall, our study provides a promising candidate to achieve bioremediation of PAHs-contaminated environments.
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2022
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IF 4.52
Qiaoling Zhang,Xiaofang Yu,Huaixia Chen,Xueping Dang,Xiaolan Liu
In this study, bimetallic coordination cluster Cu 7 Mn 2 was synthesized by solvent thermal method and based on the features of large specific surface area, rich adsorption sites, the material was applied for the dispersive solid-phase extraction of pyrene, fluoranthene , phenanthrene and fluorene in lettuce followed by high performance liquid chromatography analysis. The sythesized Cu 7 Mn 2 cluster was characterized by Fourier transform infrared spectroscopy , scanning electron microscopy, thermogravimetric analysis , hydrophobicity and nitrogen adsorption-desorption experiments. The adsorption kinetics and adsorption isotherms were carrued out. Then, the adsorption mechanism was speculated to be the coexistence of π − π stacking, hydrophobic interaction and N−H···π interaction. The adsorption experimental results indicated that Cu 7 Mn 2 cluster had better adsorption properties for pyrene, fluoranthene, phenanthrene, fluorene than Cu cluster and Mn cluster. The extraction conditions such as the kind and volume of desorption solvent, the adsorption and desorption time, the sample volume and salinity were investigated. Under the optimal conditions, a DSPE-HPLC method was developed for the determination of pyrene, fluoranthene, phenanthrene and fluorene in lettuce. The linearities were 0.5 − 1000 μg/kg for phenanthrene, fluorene and 3−1000 μg/kg for pyrene, fluoranthene (R 2 >0.99), respectively. The limits of detection (LODs, S/N = 3) and the limits of quantification (LOQs, S/N = 10) were in the ranges of 0.12−0.81 μg/kg and 0.40 − 2.7 μg/kg, respectively. The intra- and inter-day precisions (RSDs) were less than 2.9% and 4.0%, respectively, and the recoveries were in the range of 94.9% − 101.1%. The established DSPE-HPLC method has been proven to be accurate for the analysis of four polycyclic aromatic hydrocarbons in lettuce samples.
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MICROCHEMICAL JOURNAL
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2022
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IF 5.304
Yahuan Li,Yang Li,Qingyun Chang,Xiaohuan Zang,Shuaihua Zhang,Chun Wang,Zhi Wang
MXene-polyvinylpyrrolidone (MXene-PVP) was first prepared by physically doping combined with spray drying, which can overcome the aggregation of the MXene. Then, the MXene-PVP was carbonized to result in a carbonized MXene-PVP (MXene-PVP-C), which was then immobilized on stainless steel wire by sol–gel approach to prepare a new solid-phase microextraction (SPME) fiber. The prepared MXene-PVP-C coated fiber was studied for the extraction of 10 polycyclic aromatic hydrocarbons (PAHs) from tea beverages by using SPME method prior to gas chromatographic detection. The main SPME parameters, including extraction temperature, extraction time, salt concentration, sample solution pH and stirring rate, were investigated by central composite design methodology. Under the optimized conditions, the developed method gave the limits of detection of 0.03–0.15 µg/L, and the limits of quantification of 0.10–0.50 µg/L for the PAHs. The method recoveries for the PAHs in spiked tea beverages ranged from 78.6 % to 122 %. The single-fiber and fiber-to-fiber relative standard deviations were lower than 8.2 % and 9.6 %, respectively.
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Xinze Wu,Qiqi Chu,Qiong Ma,Huaixia Chen,Xueping Dang,Xiaolan Liu
The contamination of polycyclic aromatic hydrocarbons (PAHs) in edible oil is a health threat. Thus, trace analysis of PAHs is of high necessity. Based on the efficient adsorption of PAHs on Zn 5 metal cluster, a Zn 5 functionalized copolymer monolithic column was rationally designed for pipette tip micro-solid phase extraction (μ-SPE). The modified Zn 5 improved the adsorption selectivity and capacity of the monolith for naphthalene, phenanthrene, fluoranthene and pyrene. Chemical doping and copolymerization stabilized the monolith with a long life. Under optimal extraction conditions, a μ-SPE-high performance liquid chromatography with ultraviolet detector method was established for the detection of 4 PAHs in edible oils. The method yielded detection ranges of 0.15–250 μg L −1 ( R 2 > 0.997), detection limits of 0.050–1.5 μg L −1 , satisfactory recoveries (86.3–101.5 %), and high precisions (RSDs < 7.9 %). The results indicated that the Zn 5 functionalized copolymer monolithic column was an ideal separation medium for the detection of PAHs residues in edible oils.
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MICROCHIMICA ACTA
·
2022
·Vol. 189
·期 12
·1-10
·
IF 6.408
Sun Min,Wang Xiuqin,Ding Yali,Feng Juanjuan
In order to improve the selectivity and stability of melamine–formaldehyde (MF) aerogel, it was composited with TiO 2 aerogel. A TiO 2 -MF hybrid aerogel was in situ prepared on the surface of carbon fibers for in-tube solid-phase microextraction (SPME). The extraction performance of TiO 2 -MF aerogel was regulated by changing the ratio of TiO 2 sol and MF sol during the material preparation. Coupled with high-performance liquid chromatography-diode array detection (HPLC–DAD), the extraction tube filled by TiO 2 -MF aerogel-coated carbon fibers was evaluated with several types of environmental pollutants including polycyclic aromatic hydrocarbons (PAHs), estrogens, and ultraviolet filters. Because of favourable extraction performance of PAHs they were selected as model analytes, and some important influence factors were optimized for satisfactory sensitivity. The detection limits were in the range 0.05–0.10 μg L −1 , owing to high enrichment factors (653–1007). The online in-tube SPME-HPLC–DAD method was verified for the determination of trace PAHs in environmental water samples, and acceptable recovery (70–118%) was achieved. The analytical methods also displayed some advantages in comparison with other reports. Moreover, the extraction tube exhibited satisfactory chemical stability. Graphical abstract
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Xiumin Yang,Junmin Wang,Guifen Chang,Cuihong Sun,Qiuhua Wu,Zhi Wang
Analysis of organochlorine pesticides (OCPs) residues in milk faces a significant challenge. Herein, a sea urchin structured covalent organic framework bearing boric acid groups named COF-B(OH) 2 was synthesized and applied as a coating material for solid-phase microextraction (SPME) of the OCPs in cattle’s milk. Its performance was superior to that of three commonly used commercial SPME fibers, which could be due to the coexistence of hydrogen bonding , halogen bonding, π-stacking and electrostatic interactions. Besides, the fiber coating displayed good stability and reusability. After optimization, a COF-B(OH) 2 based SPME coupled with gas chromatography-electron capture detection was established for the sensitive detection of the OCPs from milk samples. The limits of detection (S/N = 3) were between 0.04 and 1.00 μg kg −1 . Satisfactory accuracy was achieved with the method recoveries in the range of 87.5 % to 112.5 %. These results manifest the feasibility of the COF-B(OH) 2 coated fiber for the enrichment of the trace OCPs from milk samples.
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