ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2023
·
IF 4.3
Hu Xingru,Pang Long,Wu Mingkai,Wang Chaohai,Li Jiansheng
Metal–organic framework-derived carbon materials have shown extensive application in the sensitive extraction of polycyclic aromatic hydrocarbons (PAHs), but more active sites for its adsorption were still a tireless pursuit. In this study, ZIF-nanoleaf-derived carbon (NLCs) was synthesized and developed as a solid-phase microextraction (SPME) fiber (NLCs-F). The extraction performance was compared with ZIF-dodecahedron-derived carbon (DHCs) coated fiber (DHCs-F), which was prepared by only changing the ratio of the reactants. The unique morphology of NLCs provided abundant adsorption active sites for the selected PAHs, while the large average aperture facilitated selective extraction of high molecular weight analytes. Additionally, the high carbon content enhanced the strong enrichment capability for hydrophobic PAHs. Hence, the prepared NLCs-F coupled with GC–MS showed a good correlation coefficient (0.9975) in a wide linear range, low limits of detection (0.3–1.8 ng L −1 ), satisfactory repeatability, and reproducibility, which made it apply in the enrichment of PAHs in actual tea and coffee samples. Graphical abstract
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MICROCHIMICA ACTA
·
2023
·Vol. 190
·期 9
·1-10
·
IF 5.7
Xu Li,Hu Wei,Luo Xiaogang,Zhang Juan
A novel MIL-88-NH 2 @COF composite was produced by in situ growth of covalent organic framework (COF) on the metal–organic framework (MOF) surface. To obtain a coating fiber for solid-phase microextraction (SPME), the MIL-88-NH 2 @COF composite physically adhered to the stainless steel wire. Combined with gas chromatography-flame ionization detection (GC-FID), various analytes such as chlorophenols (CPs), phthalates (PAEs), and polycyclic aromatic hydrocarbons (PAHs) were extracted and determined to evaluate the extraction performance of MIL-88-NH 2 @COF coated fibers and explore their extraction mechanism. This composite exhibit excellent extraction performance and adsorption capacity for various analytes, especially for PAHs with enrichment factor up to 9858. The SPME-GC-FID method based on MIL-88-NH 2 @COF fiber was established for the determination of five PAHs after the main extraction conditions were optimized. Under optimal conditions, the proposed technique showed a wide linear range (1–150 ng mL −1 ) with a low limit of detection (0.019 ng mL −1 ) and a high coefficient of determination ( R 2 > 0.99). The developed SPME-GC-FID method was used to determine PAHs in green tea and black tea samples, with good recoveries of 51.70–103.64% and 68.56–103.64%, respectively. It is worth mentioning that this is the first time MIL-88-NH 2 @COF composites have been prepared and applied to SPME. The preparation method of the composite provides a new idea in adsorbent preparation, which will contribute to the field of SPME. Graphical abstract
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ANALYTICAL CHEMISTRY
·
2023
·
IF 7.4
Yuanji Gao,Hongru Feng,Bing Xia,Lei He,Congling Yang,Lijuan Zhao,Yuanjiang Pan
Ultratrace organic pollutants in the environment pose severe threats to human health; hence, their accurate detection is essential. In this study, we develop a secondary solvent-free enrichment strategy based on bubbling extraction (BE). Especially, we used BE solid-phase microextraction and BE carbon nanotube paper absorption to capture aerosols from a liquid water surface, desorb analytes, and analyze the analytes using mass spectrometry. The application of a solvent-free enrichment strategy helps overcome technical challenges in implementing BE technology, including reproducibility, quantification, and sensitivity. This approach objectively demonstrates the enrichment efficiency of BE, resulting in improved mass spectrometry response and quantification. It effectively tackles the difficulties in detecting and quantifying ultratrace environmental pollutants in mass spectrometric analysis. The present study successfully conducted a quantitative analysis of 16 polycyclic aromatic hydrocarbons and 7 antibiotics in 48 environmental water samples. This strategy proved effective in detecting the presence and distribution of polar and nonpolar environmental pollutants in rivers and lakes. Moreover, this strategy has several advantages, such as ultrahigh sensitivity at the femtograms per liter level, good greenness, multiplexed quantitation, low sample consumption, and ease of operation. Overall, the utilization of the ultrasensitive and environmentally friendly BE approach presents a reliable and adaptable method for the identification of ultratrace environmental pollutants in water specimens, thereby enabling early monitoring of pollutant levels.
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WATER AIR AND SOIL POLLUTION
·
2023
·Vol. 234
·期 7
·1-13
·
IF 2.9
Zhou Danli,Zhang Dong,Zhang Ming,Lü Ting,Huang Jingang,Zhao Hongting,Lin Jun
To clarify the sorption mechanism and removal efficiency of PAHs by waste biomass-based magnetic sorbents, the sorption performance of magnetic Myriophyllum aquaticum biomass (MMaB) for PAHs was studied. The structural characteristics and magnetic properties of MMaB were measured by FTIR, SEM–EDS, XRD and VSM. Batch experiments were carried out to evaluate the effects of contact time, initial concentration and properties of PAHs, pH, ionic strength and temperature on PAH sorption. The results showed that the sorption of seven PAHs achieved equilibrium at approximately 4–6 h, which fit well to the pseudo-second-order kinetic model. The isotherms followed the Freundlich model and linear model well, indicating that the sorption process was controlled by chemisorption. The distribution parameter ( K d ) values were 91.3, 563.7, 1010.5, 2917.8, 2706.6, 9046.8 and 15969.0 L·kg −1 for naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, pyrene, and fluoranthene on MMaB, respectively, following the order of their hydrophobicity (e.g., K ow ). A positive correlation was obtained: log K d = 0.8091log K ow + 1.7034. Water chemical properties such as pH and ionic strength had no obvious effect on PAH removal. The spontaneity, feasibility and exothermic properties of PAH removal by MMaB were explained from thermodynamic point of view. The as-prepared MMaB sorbent underwent four consecutive sorption cycles and had good cycling performance. These studies indicate that MMaB has great potential as an easily-prepared, easy-to-operate and efficient biosorbent to remove PAHs from wastewater.
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JOURNAL OF CHEMICAL EDUCATION
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2023
·
IF 3
Xiang Wan,Dian Wang,Yuqing He,Jiafei Wang,Qin Xu,Donglin Zhao,Fazhi Xie,Qishu Qu
High-performance liquid chromatography (HPLC) experiments are an important part of the undergraduate analytical instrumentation laboratory courses and usually use commercial C18 silica-packed reversed-phase columns. In this experiment, a simple method of preparing SiO2 core–shell packed columns was developed to enable students to master the whole process of HPLC experiment from stationary phase preparation and column packing to separation experiments, just as they do for gas chromatography. Nonporous SiO2 particles with a particle size of approximately 2.2 μm were prepared by a three-step dilution reaction using the sol–gel method. The product yield was 92.1%. Monodisperse and spherical SiO2 core–shell particles (SiO2@dSiO2) with a particle size of about 2.4 μm were prepared by a one-step hydrothermal method using the prepared SiO2 spheres as the core. The product yield was 83.3%. The prepared SiO2@dSiO2 particles were derivatized with n-octadecyldimethylchlorosilane and then packed into a stainless steel chromatography column. A high column efficiency of 83,188 theoretical plates per meter was obtained for fluorene in reversed-phase mode for the separation of a mixture of polycyclic aromatic hydrocarbons. The column efficiency obtained with this method is the same as that of a commercial column packed with fully porous particles of the same particle size. The SiO2 core–shell stationary phase preparation method developed in this experiment has the advantages of simple process, high yield, and good repeatability. The experiment can be designed to be completed over a period of 1–3 weeks. Inorganic material synthesis is another important aspect of this experiment.
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CHEMICAL ENGINEERING JOURNAL
·
2023
·
IF 15.1
Yaling Wang,Maolin Wang,Qing Xie,Xiyun Cai
We report new activated persulfate systems with cyclodextrin (CD)-coated Fe 3 O 4 @Fe 0 nanoparticles (Fe 3 O 4 @Fe 0 -CD) that are characterized by both highly activating persulfates and rapidly accessing hydrophobic PAHs. Fe 3 O 4 @Fe 0 -β-CD displays chain-like structure of core–shell Fe 3 O 4 @Fe 0 nanoparticles coated with a CD layer (about 5.9 nm). CD coating stabilizes the polycrystalline structure of Fe 3 O 4 @Fe 0 nanoparticles and accelerates mass transfer of PAHs in water, thereby making Fe 3 O 4 @Fe 0 -β-CD intrinsically stable and reactive. Fe 3 O 4 @Fe 0 -β-CD/PS, featured by high yields of highly reactive Fe(IV), had about 30-fold rate constants of naphthalene (Nap) in water as much as Fe 3 O 4 @Fe 0 /PS. Fe 3 O 4 @Fe 0 -β-CD/PS completely removed Nap in water during 13 of total 18 supplementations of Nap and/or PS, whereas Fe 3 O 4 @Fe 0 /PS completely removed Nap only at the first supplementation of Nap. Likewise, Fe 3 O 4 @Fe 0 -β-CD/PS completely removed Nap in simulated groundwater, and degraded four PAHs in soils by >63%. This study may provide a technical basis for the developments of new PS activators to remove recalcitrant hydrophobic contaminants in water and soils.
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Food Analytical Methods
·
2023
·Vol. 16
·期 6
·1131-1144
·
IF 2.9
Yu Chen,Luo Xiaogang,Wu Fengshou,Zhang Juan
A covalent organic framework/reduced graphene oxide composite (COF/rGO) was fabricated by facile ultrasonic self-assembly strategy and further coated onto stainless-steel wire by physically adhesion for headspace solid-phase microextraction (HS-SPME) of polycyclic aromatic hydrocarbons (PAHs) prior to their determination by gas chromatography-flame ionization detection (GC-FID). Compared with the individual porphyrin-based COF and GO, the as-prepared COF/rGO composite effectively prevented the stacking of GO nanosheets and exhibited enhanced extraction efficiency due to the synergistic effect, with the enrichment factor up to 8816 for phenanthrene. The morphology, structure, and stability of COF/rGO composite was characterized by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, and N 2 adsorption–desorption. Effective adsorption and desorption parameters including extraction temperature, extraction time, desorption temperature, desorption time, agitation speed, and ionic strength were optimized. The established HS-SPME/GC-FID method based on COF/rGO composite fiber was evaluated in terms of linear ranges from 0.5 to 250.0 ng mL −1 with R 2 ≥ 0.9985, limits of detection in the range of 0.09–0.59 ng mL −1 , and limits of quantitation in the range of 0.31–1.97 ng mL −1 . The intra-day, inter-day, and fiber-to-fiber relative standard deviations (RSDs) were in the range of 1.86–4.37%, 2.48–5.40%, and 3.51–7.81%, respectively. The established method was employed to determine trace level of PAHs in honey with good recoveries (62.99–128.8%) and reliable reproducibility (0.51–7.63%).
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TALANTA
·
2023
·
IF 6.1
Li Xu,Wei Hu,Fengshou Wu,Juan Zhang
In this work, a novel spherical metal organic framework (MOF) was first in situ grown on the surface of iron wire (IW), in which IW served as the substrate and metal source for MOF (type NH 2 -MIL88) growth without adding additional metal salts in the process, while spherical NH 2 -MIL88 provided more active sites for further construction of multifunctional composites. Subsequently, a covalent organic framework (COF) was covalently bonded to the surface of the NH 2 -MIL88 to obtain the IW@NH 2 -MIL88@COF fibers, which were used for headspace solid-phase microextraction (HS-SPME) of polycyclic aromatic hydrocarbons (PAHs) in milk samples prior to determination by gas chromatography-flame ionization detection (GC-FID). Compared with the fiber prepared by physical coating, the IW@NH 2 -MIL88@COF fiber prepared by in situ growth and covalent bonding exhibits better stability and possesses more uniform layer. The extraction mechanism of the IW@NH 2 -MIL88@COF fiber for PAHs was discussed, which mainly owed to π-π interactions and hydrophobic interactions. After optimization of the primary extraction conditions, the SPME-GC-FID method was established for five PAHs with a wide linear range (1–200 ng mL −1 ), good linearity coefficient (0.9935–0.9987) and low detection limits (0.017–0.028 ng mL −1 ). The relative recoveries for PAHs detection in milk samples ranged from 64.69 to 113.97%. This work not only provides new ideas for the in situ growth of other types of MOF, but also provides new methods for the construction of multifunctional composites.
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JOURNAL OF MOLECULAR STRUCTURE
·
2023
·
IF 3.8
Yuxiu Fu,Xiaoli Song,Yaming Pang,Yinan Zheng,Liguo Gao
In this paper, a green solvent [BMIM] [PF 6 ] ionic liquid was selected for the extraction and separation of quinoline from simulated wash oil. The effects of extraction temperature, extraction time, and solvent oil ratio on the extraction of quinoline from wash oil were studied. The optimal process parameters were obtained by changing single factor conditions and optimizing the experiment using response surface methodology. When the temperature is 71 ℃, the time is 60 min, and the solvent oil ratio is 3:5, the extraction efficiency can reach 67%. The ionic liquids were recovered and their properties were investigated by infrared spectroscopy. The mechanism of quinoline extraction by ionic liquids was analyzed using infrared spectroscopy and GROMACS kinetic simulation calculations.
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MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Rui Shi,Yipeng Huang,Yanqun Yang,Zhuqiang Wu,Zhengyi Chen,Guihua Ruan
In this work, spherical amine-functionalized mesoporous silica (Sp- Amino-Si ) molecular sieve was fabricated by an acid hydrothermal method using 3-aminopropyltriethoxysilane as a modifier and toluene as the solvent. The results of scanning electron microscopy, Barrett-Joyner-Halenda pore size distribution, Fourier transform-infrared spectroscopy, and low-angle X-ray diffraction patterns revealed that the Sp- Amino-Si was monodispersed microspheres with uniform and controllable pore sizes sharing two-dimensional hexagonal P6mm symmetry and a large number of amino groups. The Sp- Amino-Si molecular sieve was verified to be suitable for the selective separation of aromatic hydrocarbons (AMHs) containing two fused benzene rings among other compounds from environmental water matrix. Under the optimized conditions, the Sp- Amino-Si exhibited much higher adsorption efficiency for AMHs (above 88.19%), comparing to the original SBA-15 (below 44.52%). The maximum adsorption capacities for naphthalene, methyl naphthalene, 2-methyl naphthalene, and acenaphthene were 477.1, 1006.5, 893.3, and 1253.2 µg·g −1 , respectively. The high selectivity of Sp- Amino-Si for the four AMHs attributed to the size sieving and p-π interactions between the lone pair electrons of amine groups and the π-electrons in AMHs molecules. The Sp- Amino-Si based solid-phase extraction coupled with high performance liquid chromatography detection method was constructed for the analysis of the four AMHs, and the recoveries of spiked AMHs ranged from 89.67% to 112.74% with a relative standard deviation lower than 5.75%. This study provides some inspiration and a reliable method for AMHs separation, removal, and analysis.
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Journal of Cleaner Production
·
2023
·
IF 11.1
Chun Wang,Qianqian Wang,Jintao Yu,Xinmeng Wang,Lijuan Wang,Bin Zhao,Lin Hao,Weihua Liu,Zhi Wang,Hao Chen,Qiuhua Wu
White pollution caused by the massive discharges of waste expanded polystyrene (WEPS) has become a critical global issue, so the effective conversion of WEPS is of great significance to reduce white pollution. Herein, adopting WEPS as raw material, three high-value-added hyper-crosslinked polymers (WEPS-HCPs) with high surface areas and abundant micro/mesoporous structures were synthesized via Friedel-Crafts alkylation reaction using dimethoxymethane, dichloroxylene and 4,4′-bis(chloromethyl)-1,1′-biphenyl (BCB) as cross-linker, respectively. The WEPS-HCPs were used as sorbent to extract aflatoxins (AFs) and all the HCPs exhibited high adsorption capacity . For the fast separation and recovery of the sorbent, WEPS-BCB was chosen as a model HCP to be magnetically functionalized to obtain a magnetic HCP (mWEPS-BCB) for the first time. Based on magnetic solid phase extraction with the mWEPS-BCB as sorbent, a fast and sensitive method was developed to determine trace level of AFs in grain food . Under the optimal conditions, the proposed method presented wide linear range (0.008–10.0 ng g −1 ), low detection limit (0.002–0.015 ng g −1 ) and satisfactory precision (relative standard deviation < 7%). Converting WEPS into a high-value-added sorbent not only provided a facile strategy for effective recycling of WEPS, but also developed a sensitive method for accurate determination of AFs in grain food, achieving significant economic and environmental benefits.
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CHEMICAL ENGINEERING JOURNAL
·
2023
·
IF 15.1
Maolin Wang,Yaling Wang,Xudong Jing,Jiahui Xu,Min Li,Qing Xie,Xiyun Cai
Iron-activated persulfate (PS) systems commonly suffer from the poor Fe(III)/Fe(II) redox cycle in groundwater and soils, due to the rapid oxidation of Fe(II) by both PS-related and naturally occurring oxidative substances. Maintaining the Fe(III)/Fe(II) redox cycle is necessary to achieve the high efficiency and stability of iron-activated persulfate systems toward aromatic contaminants (e.g., PAHs) in groundwater and soils. Herein, we discover the mixtures of dithionite (DTN) and zerovalent iron (ZVI) to synergistically activate PS, and develop highly efficient, stable DTN-ZVI/PS systems for PAHs removal in groundwater and soils. DTN and intermediates sulfite/thiosulfate initiated reduction of ZVI-derived Fe(III) species in DTN-ZVI/PS systems. This reaction accelerated the Fe(III)/Fe(II) redox cycle and coated ZVI with FeS x , both favoring the generation of HO and SO 4 − . DTN-ZVI/PS exhibited Nap removal of >90% in water during 11 of 15 supplementations of Nap and/or PS, 1.4–2.4 times ZVI/PS. Similarly, 0.47–4.3 fold increments of Nap removal k obs were obtained in five chemical types of groundwater, and 1.3–2.4 fold increments of PAHs removal in soils. This study may provide a technical basis to develop new Fe-activated oxidation systems for groundwater and soil remediation .
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