JOURNAL OF CHROMATOGRAPHY A
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2013
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IF 4.612
Xingmei Guan,Chuande Zhao,Xiaoyan Liu,Haixia Zhang
A polymer monolith column was prepared using click chemistry for on-line solid phase microextraction of polycyclic aromatic hydrocarbons (PAHs), using 2,2′,7,7′-tetraethynyl-9,9′-spirobifluorene(TES) and 1,4-bis(6-azidoalkoxy)benzene (BAB) as monomers, and Cu(PPh 3 ) 3 Br as the catalyst. The polymer with spirocyclic cross-links was porous and presented an appropriate interspace of PAHs. Enrichment of PAHs, in the range of 100 to more than 1000 times, was due to the π – π stacking interaction and the effect of small size. The factors affecting the on-line microextraction efficiency were optimized, and the analytical conditions were evaluated to ensure reliability.
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TALANTA
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2014
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IF 3.511
Guijiang Zhang,Xiaohuan Zang,Zhi Li,Chun Wang,Zhi Wang
In this study, polydimethylsiloxane/metal-organic frameworks (PDMS/MOFs), including PDMS/MIL-101 and PDMS/MOF-199, were immobilized onto a stainless steel wire through sol–gel technique as solid-phase microextraction (SPME) fiber coating. The prepared fibers were used for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatography–mass spectrometry (GC–MS) analysis. Under the optimized experiment conditions, the PDMS/MIL-101 coated fiber exhibited higher extraction efficiency towards PAHs than that of PDMS/MOF-199. Several parameters affecting the extraction of PAHs by SPME with PDMS/MIL-101 fiber, including the extraction temperature, extraction time, sample volume, salt addition and desorption conditions, were investigated. The limits of detection (LODs) were less than 4.0 ng L −1 and the linearity was observed in the range from 0.01 to 2.0 µg L −1 with the correlation coefficients ( r ) ranging from 0.9940 to 0.9986. The recoveries of the method for the PAHs from water samples at spiking levels of 0.05 and 0.2 µg L −1 ranged from 78.2% to 110.3%. Single fiber repeatability and fiber-to-fiber reproducibility were less than 9.3% and 13.8%, respectively.
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JOURNAL OF CHROMATOGRAPHY A
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2015
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IF 4.169
Chengjiang Zhang,Gongke Li,Zhuomin Zhang
Covalent organic polymers (COPs) connected by covalent bonds are a new class of porous network materials with large surface area and potential superiority in sample pretreatment. In this study, a new hydrazone linked covalent organic polymer (HL-COP) adsorbent was well-designed and synthesized based on a simple Schiff-base reaction. The condensation of 1,4-phthalaldehyde and 1,3,5-benzenetricarbohydrazide as organic building blocks led to the synthesis of HL-COP with uniform particle size and good adsorption performance. This HL-COP adsorbent with high hydrophobic property and rich stacking π electrons contained abundant phenyl rings and imine ( C N) groups throughout the entire molecular framework. The adsorption mechanism was explored and discussed based on π–π affinity, hydrophobic effect, hydrogen bonding and electron–donor–acceptor (EDA) interaction, which contributed to its strong recognition affinity to target compounds. Enrichment factors were 305–757 for six Sudan dyes by HL-COP micro-solid phase extraction (μ-SPE), indicating its remarkable preconcentration ability. Furthermore, the adsorption amounts by HL-COP μ-SPE were 1.0–11.0 folds as those by three commonly used commercial adsorbents. Then, HL-COP was applied as adsorbent of online μ-SPE coupled with high performance liquid chromatography (HPLC) for enrichment and analysis of trace Sudan dyes in food samples with detection limit of 0.03–0.15 μg/L. The method was successfully applied for online analysis of chilli powder and sausage samples. Sudan II and Sudan III in one positive chilli powder sample were actually found and determined with concentrations of 8.3 and 6.8 μg/kg, respectively. The recoveries of chilli powder and sausage samples were in range of 75.8–108.2% and 73.8–112.6% with relative standard deviations of 1.2–8.5% and 1.9–9.4% ( n = 5), respectively. The proposed method was accurate, reliable and convenient for the online simultaneous analysis of trace Sudan dyes in food samples.
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JOURNAL OF CHROMATOGRAPHY A
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2017
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IF 3.981
Shengju Liu,Jiaxi Peng,Hongyan Zhang,Xin Li,Zheyi Liu,Xiaohui Kang,Minghuo Wu,Ren’an Wu
An organic-silica hybrid monolithic capillary column was fabricated by crosslinking (3-aminopropyl)trimethoxysilane (APTMS) modified mesoporous carbon nanoparticles (AP-MCNs) with tetramethoxysilane (TMOS) and n-butyltrimethoxysilane (C4-TriMOS). Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy, mercury intrusion porosimetry and inverse size-exclusion chromatography characterization proved the successful immobilization of mesoporous carbon nanoparticles (MCNs). The crosslinking of AP-MCNs into the hybrid monolithic matrix has significantly increased the reversed-phase retention of alkylbenzenes and chromatographic performance for small molecules separations in comparison with the neat one without MCNs. The resulting column efficiency of the mesoporous carbon nanoparticle-based butyl-silica hybrid monolithic column (MCN-C4-monolith) was up to ca. 116,600 N/m for the capillary liquid chromatography (cLC) separation of butylbenzene. Enhanced performance of proteins separation was achieved on the MCN-C4-monolith in comparison with the butyl-silica hybrid monolithic column without MCN (C4-monolith). The separation of peptides from bovine serum albumin (BSA) digest was carried out on the MCN-C4-monolith by capillary liquid chromatography–tandem mass spectrometry (cLC–MS/MS) with protein sequence coverage of 81.9%, suggesting its potential application in proteomics.
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JOURNAL OF CHROMATOGRAPHY A
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2017
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IF 3.981
Yunzhong Zheng,Qing Han,Meiling Qi,Liangti Qu
Seaweed-like graphitic carbon nitride (g-C 3 N 4 ) has a unique porous architecture composed of interlocking g-C 3 N 4 nanofibers (NF-C 3 N 4 ) with much higher surface area than bulk g-C 3 N 4 and shows good potential in separation science. This work investigated the separation performance of NF-C 3 N 4 as stationary phase for capillary gas chromatographic (GC) separations. The NF-C 3 N 4 column exhibits weak polarity and high column efficiency of 4728 plates/m for n -dodecane. Importantly, it displays good separation performance for a wide range of analytes and shows different retention behaviors from the bulk g-C 3 N 4 column and commercial HP-5MS column with 5% phenylpolysiloxane. Particularly, it shows high resolving capability for both aliphatic and aromatic isomers. In addition, NF-C 3 N 4 column has high thermal stability up to 280 °C and good separation repeatability with relative standard deviation (RSD) values in the range of 0.29–0.61% for intra-day, 0.56–1.1% for inter-day and 2.0–4.9% for between-column, respectively. Moreover, it was applied for the determination of isomer impurities in real samples, showing good potential in GC applications.
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SCIENCE OF THE TOTAL ENVIRONMENT
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2024
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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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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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SEPARATION AND PURIFICATION TECHNOLOGY
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2024
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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
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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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CHEMICAL ENGINEERING JOURNAL
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2024
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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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Reaction Chemistry & Engineering
·
2024
·
IF 3.4
Hui Jin,Mengyu Cui,Peiwen Liu,Zhuo Wang,Tongxia Jin,Yonghui Yang,Weiping Zhu,Xuhong Qian
Heterogeneous palladium catalysts are widely used in catalytic hydrogenation, oxidation, reduction, and coupling reactions due to their good stability, recyclability, and reusability. Based on the palladium ion fluorescent probe, a novel magnetically recyclable heterogeneous palladium catalyst Fe3O4@FSM@Pd was constructed and characterized, which is highly efficient and reusable for the Suzuki–Miyaura cross-coupling reaction. The subsequent series of Maitlis' filtration test, catalyst concentration–yield kinetic experiments, and phase trajectory experiments further demonstrated that Fe3O4@FSM@Pd catalyzed through a heterogeneous mechanism under selected reaction conditions. In addition, Fe3O4@FSM@Pd was applied to catalyze the synthesis of five intermediates of active pharmaceutical ingredients (APIs): valsartan, sonidegib, erdafitinib, tubulin inhibitor, and lumacaftor. Importantly, the palladium residue in the API intermediates synthesized with Fe3O4@FSM@Pd as catalyst was less than 1 ppm. Furthermore, Fe3O4@FSM@Pd is stable and can be reused at least 5 times without losing activity.
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