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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SEPARATION AND PURIFICATION TECHNOLOGY
·
2024
·
IF 8.1
Dongni Liu,Peng Cui,Fangfang Zhang,Hao Ren,Lilin Fang,Xiaosi Sun,Haiyan Ji,Wenshuai Zhu,Zhichang Liu
Ionic liquid is an ideal candidate in the extraction of aromatic compounds. The design and construction of ionic liquids with high extraction efficiency and selectivity towards to the specific aromatics remain crucial question. In this paper, with the aid of orthogonal array experiment, the imidazolium-based ionic liquids with long alkyl chain on the cations were determined to possess high aromatics extraction efficiency. Furthermore, the Lewis acid anion was introduced into the ionic liquid to form 1-dodecyl-3-methylimidazolium ferric chloride ([C 12 mim][FeCl 4 ]) and performed 62 % and 100 % extractant efficiency of naphthalene (NAP) and anthracene (ANT), respectively. Then the porous carbon materials (P1-1000) derived from hyper-crosslinked porous polymers (HCP) which possessed high BET surface area (1186 m 2 /g) was dispersed in [C 12 mim][FeCl 4 ] to form porous ionic liquid. The single extraction efficiency of NAP improved from 62 % to 77 %. The great single extraction efficiency was attributed to the high porosity, additional adsorption sites provided by the Lewis acid anions and the hydrophobic long alkyl chain on the cations. After three times extraction, the concentration of NAP dropped down to 0. The porous ionic liquids also showed good recycle performance. The construction of porous ionic liquids provided an efficient approach for extraction of polycyclic aromatic hydrocarbons from aliphatic hydrocarbon.
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CHEMICAL ENGINEERING JOURNAL
·
2024
·
IF 13.3
Xiao Wang,Bingcheng Lin,Jian Wang,Yunfeng Ma,Rong Jin,Guorui Liu,Minghui Zheng
Four inhibitors (CaO, CaS, CH 4 N 2 S, and (NH 4 ) 2 SO 4 ) were employed to inhibit the formation of multiple unintentional persistent organic pollutants (POPs) and environmentally persistent free radicals (EPFRs) using anthracene as a precursor, with CuCl 2 serving as both a transition metal catalyst and chlorine source. The inhibition mechanisms were elucidated in terms of chlorine immobilization, catalyst deactivation, and free radical regulation. The inhibition efficiency of the four inhibitors on polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), polychlorinated biphenyls (PCBs), and polychlorinated naphthalenes (PCNs) ranged from 64.7 % to 98.4 %, with the corresponding inhibition rates on toxic equivalency quantity ranging from 86.3 % to 99.7 %. The distribution of homologs shifted towards less chlorinated species, indicating effective suppression of chlorination. Calcium- and nitrogen-containing compounds consumed chlorine sources by forming CaCl 2 , CaClOH, and NH 4 Cl, while sulfur-containing compounds deactivated catalysts by forming CuSO 4 . EPFRs derived from anthracene were identified as carbon-centered anthracene-type and anthraquinone-type radicals. Positive correlations were observed between POPs and EPFRs concentrations, suggesting the pivotal role of organic free radicals as intermediates in POPs formation. Anthraquinones derived from anthracene underwent decomposition, recombination and chlorination, leading to the formation of PCDD/Fs and PCBs. The addition of inhibitors reduced EPFRs concentrations by 74.2–95.1 %. Sulfur- and nitrogen-containing inhibitors generated radicals that attacked POPs precursors and intermediates, forming heteroatomic compounds and inhibiting POPs formation. These findings enhanced the understanding of the source control mechanisms of POPs and provided theoretical and technical support for the synergistic inhibition of POPs and EPFRs in industrial thermal processes.
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Zhihao Li,Dihong Zhong,Haipeng Lin,Peiyin Li,Yongyi Li,Qingmei Huang,Lingzhi Yang,Xueji Zhang
Solid-phase microextraction (SPME) is essential for analyzing ultra-low concentration samples, such as trace drugs and environmental pollutants. Among various formats, pipette tip-based SPME (PT-SPME) stands out for its advantages in efficiency, automation, and flexibility. However, PT-SPME faces challenges such as material loss, high synthesis costs, and environmental impact. To address these issues, we developed a novel PT-SPME device by synthesizing Schiff-base covalent organic frameworks (COFs) in situ on diatomaceous earth (DE), which served as both a matrix and support. This approach significantly improved stability and reduced COFs consumption by 93.7 %. The DE@COFs were packed into pipette tips with a sandwich-like structure and used to extract polycyclic aromatic hydrocarbons (PAHs), with detection achieved through high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD). The method exhibited excellent sensitivity, with limits of detection (LODs) ranging from 2.05 to 52.5 pg/mL and limits of quantification (LOQs) from 15.0 to 159 pg/mL. It also demonstrated high accuracy, with recoveries between 87.05 % and 115.86 %, and strong repeatability, making it suitable for trace pollutant analysis in complex matrices This cost-effective and environmentally friendly PT-SPME system enhances extraction efficiency while reducing material usage, providing a practical and innovative solution for trace pollutant analysis in pharmaceutical and environmental applications.
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2024
·
IF 8.1
Lilin Fang,Peng Cui,Dongni Liu,Xiaosi Sun,Hao Ren,Hanyu Zhang,Yan Huang,Wenshuai Zhu,Zhichang Liu
The polycyclic aromatic hydrocarbons (PAHs) are serious organic contaminants that are produced naturally and anthropogenically. The separation of PAHs by adsorption approach provides an efficient method to avoid the negative effects of PAHs pollution. In this study, cyclodextrin (CD) was grafted to chitosan (CS) by using glutaraldehyde as crosslinking agent to construct shaped CD-CS polymers and carbonization was executed subsequently. The carbonized β-CD-CS-1000 exhibited a significant increasement of BET surface area (CD-CS polymer: 1 m 2 ·g −1 ; β-CD-CS-1000: 1083 m 2 ·g −1 ) and great PAHs adsorption performance (anthracene: 106.34 mg/g; acenaphthylene: 41.02 mg/g). The adsorption kinetic behavior and the equilibrium adsorption process were further explored. β-CD-CS-1000 showed good cyclic adsorption capacity and anti-interference stability with the xylenes as interferon. Furthermore, the adsorbents based CD-CS can be synthesized at the gram-level in the lab and exhibited great adsorption capacity in real diesel. The large-scale preparation of shaped CD-CS adsorbents made it possible to be applied to the petrochemical industry.
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GREEN CHEMISTRY
·
2024
·Vol. 26
·期 6
·3211-3220
·
IF 9.3
Pengfei Li,Yehong Han,Dandan Han,Hongyuan Yan
An innovative solid-phase microextraction (SPME) fiber coating, melamine–formaldehyde resin (MFR), was synthesized with a green cross-linker (paraformaldehyde), and it exhibited high heat resistance (up to 350 °C). Seven polycyclic aromatic hydrocarbons (PAHs) were chosen as analytes, and the results demonstrated the MFR-based SPME fiber's exceptional enrichment capabilities and efficient extraction, with high enrichment factors and significantly improved efficiency compared to the conventional polydimethylsiloxane (PDMS) fibers. The unique superiority of the MFR was attributed to its strong π–π interactions and amino-associated enhancement, as well as its porous structure and rough surface, which provided abundant adsorption sites and facilitated rapid mass transport of analytes. Furthermore, the preparation conditions of the MFR-coated SPME fiber were compared with those of commercially available and reported fibers, emphasizing the advantages of the MFR-coated fiber, such as its simplicity, cost-effectiveness, reproducibility, and eco-friendliness. The MFR-based SPME fiber exhibited significant advantages, including high enrichment factors (ranging from 1906- to 7153-fold) for PAHs and good fiber-to-fiber reproducibility (8.7–14.6%), outperforming commercially available PDMS fibers by a factor of 4.9–82.8-fold. This study also considered important factors affecting the extraction process, such as ionic strength, temperature, and time, and optimized these parameters for the best extraction efficiency. The greenness of the developed method was assessed using the Analytical Eco-Scale, and the results showed that it was green in terms of reagent dosage, energy consumption, and waste. The developed headspace solid phase microextraction–gas chromatography–tandem mass spectrometry (HS-SPME-GC-MS/MS) method based on the MFR coating exhibited excellent precision, accuracy, and repeatability, making it a reliable method for the determination of trace PAHs in environmental water samples.
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ANALYTICA CHIMICA ACTA
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2024
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IF 5.7
Min Sun,Jiaqing Feng,Yang Feng,Xubo Xin,Yali Ding,Juanjuan Feng
Background Because of the advantages of good selectivity , high sensitivity, and fast analysis, high performance liquid chromatography (HPLC) has become one of the modern analytical techniques in wide application range, such as biological analysis, environmental detection, pharmaceutical and food inspection, agriculture and other fields. The stationary phase greatly decides the chromatographic separation performance, so the development of novel stationary phase is most important for HPLC. Results Pyridyl conjugated microporous polymers (P-CMP) with one to four layers were modified on the surface of amino silica to obtain a novel core-shell material (SiO2@P-CMP) by the layer-by-layer assembly strategy and Chichibabin reaction . The relationship between the structure of SiO2@P-CMP and chromatographic performance was carefully investigated, and the retention mechanism was revealed. The interactions including π-π stacking, hydrophobic effect and hydrogen bond gradually enhanced with the increase of P-CMP layers on the silica surface. Compared with C18 column, SiO2@P-CMP columns displayed better separation selectivity for polycyclic aromatic hydrocarbons (PAHs). According to the relative retention values ( α ), the separation performance of SiO2@P-CMP columns ( α = 1.144–1.884) for PAH isomers and other analytes was obviously better than that of C18 column ( α = 0.998–1.487). Furthermore, the SiO2@P-CMP column with four layers was selected to separate different types of analytes (eight PAHs, four bisphenols , four estrogens and nine phthalates), and the peak order of analytes was different from that on the C18 column due to the influence of hydrogen-bonding and π-π interactions. The relative standard deviations (n = 10) of retention time and peak area on SiO2@P-CMP column were between 0.28 % and 1.98 %. Significance and novelty Pyridyl conjugated microporous polymer was introduced as the stationary phase for the first time in HPLC. The proposed column displayed better separation characteristics compared to Zorbax SB-C 18 column. It provided a new idea for the separation of small molecules and the development of chromatographic packing or extraction material.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Yali Yang,Jia Chen,Xiaojing Liang,Bei Liu,Kaijun Quan,Xiuhui Liu,Hongdeng Qiu
In this paper, three imidazole- and C18- bifunctional silica stationary phases (Sil-Im-C18) were prepared by adjusting introduction interval of octadecyltrichlorosilane (ODS) and 3-imidazol-1-ylpropyl(trimethoxy)silane (TMPImS), which can be used for reversed-phase liquid chromatography (RPLC) and ion exchange chromatography (IEC) with adjustable performance. The successful preparation of Sil-Im-C18 were confirmed by the characterizations of elemental analysis, infrared spectroscopy (FTIR) and contact angle (CA). Chromatographic performance of Sil-Im-C18 were evaluated by the separation of Tanaka test mixture, alkylbenzenes, linear PAHs and a set of analytes with different properties (uracil, phenol, 1,2-dinitrobenzene and naphthalene), and compared with commonly used C18 column. It was found that the chromatographic performance of Sil-Im-C18 changed significantly with the difference in bonding amount of imidazole and C18. Sil-Im-C18 demonstrated the excellent separation performance towards polycyclic aromatic hydrocarbons (PAHs), phenylesters, phenylamines , phenols and inorganic anions, and notably, nucleobases and nucleosides can be separated using pure water as mobile phases . The van Deemter plot showed that the column efficiency of Sil-Im-C18-3 was 64,933 plate· m − 1 for naphthalene, indicated that Sil-Im-C18 was reasonably chromatographic columns. The RSD values of retention time were 0.22 %-0.61 % for 10 needles alkylbenzenes injected continuously at 50 °C to investigate thermal stability and repeatability, all the fluctuations of k of naphthalene were less than 2.3 % for Sil-Im-C18-1 during flushing 24 h with the mobile phase at different pH values (pH = 3 and 8), the retention time of alkylbenzenes were almost same for Sil-Im-C18-1 at different time, the RSD values of retention time of alkylbenzenes were 0.45 %-2.28 % for two batches Sil-Im-C18-1, revealing the excellent repeatability, thermal stability, durability and reproducibility of Sil-Im-C18, and implying a commercial prospect.
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CHEMICAL ENGINEERING JOURNAL
·
2024
·
IF 13.3
Shuhui Huo,Xiaohui Deng,Nan Yang,Mengya Qin,Xiaonan Zhang,Xiaoqiang Yao,Cuixiang An,Pengxin Zhou,Xiaoquan Lu
In this study, a durable hydrophobicity hydrazone covalent organic framework (BTCH-PTA-COF) has been developed as fiber coating, which was applied to solid-phase microextraction (SPME) of polycyclic aromatic hydrocarbons (PAHs). The hydrophobic and π-π packing interactions between BTCH-PTA-COF and PAHs were confirmed by contact angle experiments and Van der Waals surface electrostatic potential analysis. Further, large specific surface area, good chemical and thermal stability have positive promoting effect on extraction. The method of wide linearity (0.25–300 µ g·L −1 ), low detection limits (0.03–0.05 µ g·L −1 ) and high enrichment factors (767–1411) for the detection of PAHs is explored, coupling BTCH-PTA-COF based SPME with gas chromatography with hydrogen flame detector (GC-FID). The relative standard deviations (RSDs) for inter-day and intra-day extractions of PAHs are ranging from 4.1 % to 9.6 % and 2.9 % to 6.4 %, respectively. The method successfully detected and quantified trace PAHs in tea beverages and river water samples with recoveries from 88.5 % to 104.8 %. The BTCH-PTA-COF coated fiber is ultra-stable in recycled extraction and reused at least 120 times, which could surpass published and commercial SPME fiber.
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JOURNAL OF HAZARDOUS MATERIALS
·
2025
·
IF 11.3
Yuqian Li,Haomin Chen,Wei Li,Beidou Xi,Caihong Huang
The remediation of sites co-contaminated with polycyclic aromatic hydrocarbons (PAHs) and heavy metals (HMs) poses challenges for efficient and ecofriendly restoration methods. In this study, three strains ( Pseudomonas sp. PDC-1, Rhodococcus sp. RDC-1, and Enterobacter sp. EDC-1) were isolated from sites contaminated with PAHs and HMs. The constructed bacteria consortium was then immobilized using biochar, bentonite, and peat. The immobilized bacteria consortium (IBC) demonstrated efficient removal ability of phenanthrene (58.1 %-73.4 %) and benzo[ a ]pyrene (69.6 %-83.5 %) during 60 days. Additionally, the IBC decreased soil bacterial richness and diversity, but increased the relative abundance of Proteobacteria phylum and Ochrobactrum genus, which were capable of degrading PAHs. Soil microbial co-occurrence network with IBC was classified into three main modules, and 14 genera were identified as keystone taxa linked to PAHs degradation and HMs resistance. The IBC enhanced the dioxygenase metabolic pathways for PAHs degradation, including phthalic acid and salicylic acid pathways, which became the main driving factor affecting PAHs removal efficiency based on the structural equation modeling analysis. This study confirmed the potential application of the constructed IBC in the bioremediation of soil co-contaminated with PAHs-HMs, and provides insights into key removal mechanism and main driving factor of the enhanced elimination of PAHs.
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TALANTA
·
2014
·
IF 3.511
Man Wang,Shihai Cui,Xiaodi Yang,Wentao Bi
An easy preparation of g-C 3 N 4 /Fe 3 O 4 nanocomposites by chemical co-precipitation has been demonstrated. The as-prepared materials were characterized by X-ray diffraction, transmission electron microscopy , Fourier transform infrared spectroscopy and thermogravimetric analysis . The high affinity of g-C 3 N 4 toward polycyclic aromatic hydrocarbons and the magnetic behavior of Fe 3 O 4 were combined to provide an efficient and simple magnetic solid phase extraction (MSPE). The adsorption and desorption of polycyclic aromatic hydrocarbons on g-C 3 N 4 /Fe 3 O 4 were examined. Different factors affecting the magnetic solid phase extraction of polycyclic aromatic hydrocarbons were assessed in terms of adsorption, desorption, and recovery. Under the optimized conditions, the proposed method showed good limits of detection (LOD, S/N=3) in the range of 0.05–0.1 ng mL −1 and precision in the range of 1.8–5.3% (RSDs, n =3). This method was also successfully applied to the analysis of real water samples; good spiked recoveries over the range of 80.0–99.8% were obtained.
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JOURNAL OF HAZARDOUS MATERIALS
·
2024
·
IF 12.2
Ziyue Li,Xiaolei Wang,Fei Peng,Ning Chen,Guodong Fang
The use of peracetic acid (PAA) in advanced oxidation processes has gained significant attention recently, but the knowledge of activating PAA to degrade polycyclic aromatic hydrocarbons (PAHs) is limited due to the variety and selectivity of reactive substances in PAA oxidation system. This paper presented the first systemically study on the degradation of PAHs by PAA activation in soil. It was found that heat-activated peracetic acid (heat/PAA) was capable of degrading phenanthrene (PHE) efficiently with degradation efficiency > 90 % within 30 min. Experimental results demonstrated that a series of reactive oxygen species (ROS) including organic radicals (RO • ), hydroxyl radicals (HO • ) and singlet oxygen ( 1 O 2 ) were generated, while acetylperoxyl (CH 3 C(O)OO • ) and acetyloxyl (CH 3 C(O)O • ) radicals were primarily responsible for PHE degradation in soil. Further analysis shows that polymerization products such as diphenic acid , 2′-formyl-2-biphenylcarboxylic acid and other macromolecules were dominant products of PHE degradation, suggesting polymerization driving PHE degradation instead of the conventional mineralization process. Toxicity analysis shows that most of the polymerization products had less toxicity than that of PHE. These results indicate that PAA activation was a highly effective remediation method for PAHs contaminated soil, which also provided a novel mechanism for pollutant degradation with the PAA activation process for environmental remediation.
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