MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Qiao Li,Guanyong Wu,Xinze Wu,Huaixia Chen,Xueping Dang,Xiaolan Liu
An acidity-sensitive poly(N-isopropylacrylamide-methyl acrylic acid-co-divinyl- benzene) monolith was prepared in situ in a pipette tip for solid phase extraction of phenol, m-cresol, o-nitrophenol, 2,4-dichlorophenol and p- tert -butylphenol. The monolith was characterized by FT-IR, BET (surface area = 266.56 m 2 /g) and thermogravimetric analysis (thermally stable up to 350 °C). The introduction of methyl acrylic acid enhanced the stability in the strong alkaline condition. The adsorption experiments and density function theory calculations indicated NIPAM was the main adsorption sites and the adsorption mechanism of phenol on the monolith was hydrophobic interaction, H-bond interaction, C − H···π interaction of isopropyl group of NIPAM with the phenyl group of phenols. Based on these features and under the optimal extraction conditions, a pipette tip solid phase extraction coupled to high-performance liquid chromatography with ultraviolet detection method was developed for the determination of 5 phenols in the diffusion of polycarbonate cups. Due to the usage of 0.1 M NaOH as the eluent, the method presented selectivity for phenols based on the acidity-sensitive of the monolith. Wide linear range (0.6–200 µg/L), low detection limits (0.2–0.3 µg/L), good reproducibility (%RSD less than 9.8%) and satisfactory recoveries (86.3–114.1%) were obtained. The proposed method was suitable for quantitative analysis of phenollic in water samples.
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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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MICROCHEMICAL JOURNAL
·
2022
·
IF 5.304
Yuan Peng,Si-Yuan He,Fang-Huan Wang,Hao-Bo Zheng,Zhe Meng
In this work, a magnetic mesoporous molybdenum disulfide/graphite nanosheets (mm-MoS 2 /GN) was successfully synthesized and applied to magnetic solid phase extraction (MSPE) of 13 polycyclic aromatic hydrocarbons (PAHs) from edible oil samples. The prepared mm-MoS 2 /GN was characterized by FT-IR, XRD, VSM, BET, SEM and TEM. The influence of various parameters such as the adsorbent mass, adsorption/desorption time, and elution solvent through response surface methodology in MSPE was investigated. The porous and fluffy structure with rich active sites (π interactions, electrostatics, hydrogen bonds) and amphiphilicity properties of mm-MoS 2 /GN make it an ideal material for the separation and enrichment of trace PAHs in edible oils. Under optimal MSPE and GC-MS conditions, the linearity ranges of the proposed method were 1.0–100.0 μg·kg −1 with a satisfactory correlation coefficient above 0.9907. The limits of detection and quantification for 13 PAHs were 0.10–2.50 μg·kg −1 and 0.85–5.00 μg·kg −1 , respectively. The intra- and inter-day precisions were less than 3.0 % and 3.6 %, respectively. The recoveries for spiked edible oil samples ranged from 70.2 % to 112.6 % with RSDs of less than 5.8 %. In this work, a novel, rapid, economic and effective method was proposed, and successfully applied to detect polycyclic aromatic hydrocarbons in several oil samples from local market.
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Nanomaterials
·
2022
·Vol. 12
·期 17
·2921
·
IF 5.719
Yu Tian,Zhigang Xu,Zhimin Liu,Xiaoxi Si,Fengmei Zhang,Wei Jiang
In the present study, silica-coated magnetic nanoparticles functionalized with vancomycin (Fe3O4@SiO2@VAN) were synthesized. The Fe3O4@SiO2@VAN nanocomposite was used as a sorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) from environmental water, followed by GC-MS. The nanocomposite was characterized by Fourier-transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometry, and nitrogen sorption. Various experimental parameters were optimized, including extraction condition and desorption condition. Results show that Fe3O4@SiO2@VAN combined the advantages of nanomaterials and magnetic separation technology, showing excellent dispersibility and high selectivity for PAHs in environmental water sample. Under the optimal extraction conditions, an analytical method was established with the sensitive limit of detection (LOD) of 0.03–0.16 μg L−1. The method was successfully applied for the analysis of environmental water samples. The relative standard deviations (%) were in the range of 0.50–12.82%, and the extraction recovery (%) was in the range of 82.48% and 116.32%. MSPE-coupled gas chromatography–mass spectrometry quantification of PAHs is an accurate and repeatable method for the monitoring of PAH accumulation in environmental water samples. It also provides an effective strategy for the tracing and quantification of other environmental pollutants in complex samples.Keywords:magnetic solid-phase extraction;polycyclic aromatic hydrocarbons;vancomycin;GC-MS
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TALANTA
·
2022
·
IF 6.556
Hao-Fei Sun,Yuan-Yuan Cui,Chang-Qing Zhen,Cheng-Xiong Yang
Microporous organic networks (MONs) are promising in high performance liquid chromatography (HPLC) with large specific surface area, good hydrophobicity and stability. However, their superhydrophobic structures restrict MONs-based HPLC only in reversed-phase mode. To decrease the hydrophobicity of pristine MONs and to expand their broad application in HPLC, here we described the monomer-mediated fabrication of core-shell MON-2COOH@SiO 2 microspheres for reversed-phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode chromatography for the first time. The –COOH groups were introduced into MONs’ skeleton to improve their hydrophilicity and to provide hydrophilic interaction sites. The MON-2COOH was grafted onto silica via a monomer mediated method to produce monodispersed core-shell microspheres. By adjusting the concentration of reactants, the thickness of MON-2COOH shell was easily manipulated. The packed MON-2COOH@SiO 2 column showed high resolution and selectivity for separating both hydrophobic (alkylbenzenes, polycyclic aromatic hydrocarbons , anilines and phenols) and hydrophilic (nucleoside and nucleic bases) probes, highlighting the promise of MONs in mixed-mode HPLC. The MON-2COOH@SiO 2 column also achieved good separation to sulfonamides, nonsteroidal anti-inflammatory drugs, flavonoids and phenylurea herbicides , and offered better resolution than commercial C18 and pristine SiO 2 column. Multiple retention mechanisms were also found on MON-2COOH@SiO 2 packed column, underlining the great potential of MONs in mixed-mode HPLC.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Chengcheng Zhai,Mingwei Wang,Yanke Lu,Hongyuan Yan
Polycyclic aromatic hydrocarbons (PAHs) posed a serious threat to food safety and human health due to long-term emission. In this work, a new method was established using phloroglucinol-urotropine porous polymer (PU-PP) in a pipette tip for solid phase extraction (PT-SPE) for the first time and used prior to determination of four PAHs (phenanthrene, anthracene, fluoranthene, and pyrene) in lotus roots. Synthesis of the PU-PP adsorbent was green compared with alternatives; urotropine was used as a cross-linker and ethanol–water as the solvent. PU-PP-based PT-SPE had the advantages of low solvent consumption, good purification, practicability, stability, and low-cost. The proposed pre-purification method offered low limits of detection (0.09–0.28 ng/g) and good recoveries (84.6–114.3 %, RSDs ≤ 5.6 %) for determination of the four PAHs, which were detected at trace concentrations in samples. This new method provides an alternative for monitoring trace pollutants in aquatic plant ingredients.
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yanyan Wang,Lili Lian,Xiyue Wang,Boying Yue,Lan Ding,Dawei Lou
In this study, velvet-like carbon nitride (V-g-C 3 N 4 ) was prepared from urea aqueous solutions by one-step thermal polycondensation. The V-g-C 3 N 4 material was then characterized using a scanning electron microscope (SEM), X-ray diffractometer (XRD), Fourier transform infrared spectrophotometer (FT-IR), and nitrogen adsorption-desorption isotherms. The specific surface area of V-g-C 3 N 4 (60.66 m 2 /g) was 1.8 times that of the carbon nitride (g-C 3 N 4 ) prepared by the traditional method. V-g-C 3 N 4 was modified on the surface of stainless-steel wire by a sol-gel technique to obtain a solid-phase microextraction (SPME) coating for the extraction of five polycyclic aromatic hydrocarbons (PAHs) from water samples. The chromatography signal of the PAHs extracted using the V-g-C 3 N 4 coating was 1.5 times that when using a g-C 3 N 4 coating, and 5–10 times that when using commercial PDMS. Under the optimized extraction conditions, the linear range of the method developed for the determination of five PAHs was 0.05–100 µg/L, the limits of detection were 0.005–0.012 µg/L, and the recoveries from actual water samples were 85.94–103.47%. Furthermore, the developed SPME device is remarkably durable and can be reused up to 160 times.
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yang Feng,Min Sun,Mingxia Sun,Jiaqing Feng,Haili Sun,Juanjuan Feng
Polyamidoamine dendrimers with different generations (G1-G5) were synthesized in situ on silica progressively via Michael addition and amidation reactions. A sequence of materials was characterized by elemental analysis and Brunauer-Emmett-Teller test, the content of each element (C, H and N) was increased but the surface area was reduced gradually from G1 to G5. These materials were separately packed in a stainless steel column (10 × 4.0 mm, i.d.) for SPE . These SPE columns were combined with high performance liquid chromatography (HPLC) to establish an online SPE-HPLC analysis. According to the chemical structures of materials, polycyclic aromatic hydrocarbons (PAHs) and bisphenols as model analytes were selected to investigate the extraction performance and the extraction mechanism, so as to reveal the extraction performance-structure relationship of G1-G5. The extraction performance was improved with the increase of functional groups from G1 to G4 or G5, the hydrophobic effect played main role accompanied with possible weak hydrophilic, hydrogen-bonding and electrostatic interactions in extraction mechanism. The adsorption capacity, enrichment factor, partition coefficient and extraction efficiency for PAHs and bisphenols reached to 17.52 µg g −1 and 2.70 µg g −1 , 5353 and 3002, 5066 and 1197, and 90.09% and 60.05% respectively. Compared with commercial SPE materials, these dendrimer-grafted silica materials were inferior to C18, but better than silica. Furthermore, the G4 and G5 were separately selected to develop two online SPE-HPLC analytical methods for determining trace PAHs and bisphenols in real water samples, and satisfactory results were obtained.
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Nanomaterials
·
2022
·Vol. 12
·期 10
·1766
·
IF 5.719
Qiong Jiang,Shuwu Zhang,Juanjuan Feng,Min Sun
To improve the extraction performance of the silica aerogel, a melamine-terephthalaldehyde polymer was used to hybridize silica aerogel, and the hybridized aerogel was coated on the surface of stainless steel wire to prepare a fiber-filled extraction tube through placing four wires into a polyetheretherketone tube. The tube was combined with high-performance liquid chromatography, then the online extraction and detection were established. Several polycyclic aromatic hydrocarbons (PAHs) were selected as the target analytes. Under the optimum extraction and desorption conditions, the limit of detection was as low as 3.0 ng L−1, and the linear range was 0.01–20.0 μg L−1. The enrichment factors of PAHs were in the range of 1724–2393. Three environmental water samples of mineral water, tap water and river water were analyzed by this method, and the recoveries that spiked at 1.0–10.0 μg L−1were between 80.5–126%. It showed many advantages compared with other methods, such as better sensitivity, faster detection and online analysis.Keywords:solid-phase microextraction;silica aerogel;melamine-terephthalaldehyde polymer;polycyclic aromatic hydrocarbons;online analysis
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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
Haoyu Long,Yanhao Jiang,Yanjuan Liu,Yuefei Zhang,Wei Chen,Sheng Tang
In this work, 2,4,6-tris(4-aminophenyl)-1,3,5-triazine (TAPT) and 1,3,5-tris(4-formylphenyl)benzene (TFPB) were used as monomers to construct a triazine-containing imine-linked covalent organic framework (COF), which was then bonded onto the surface of aldehydized silica (SiO 2 –CHO), and finally a COF@silica composite material (TAPT-TFPB COF@SiO 2 ) was successfully prepared. The chromatographic separation performance of SiO 2 –CHO, TAPT-TFPB COF@SiO 2 and TAPT-TFPB COF@SiO 2 /SiO 2 –CHO (80/20, mass ratio) was evaluated and compared. It was found that separation efficiency was obviously enhanced by adding an appropriate amount of SiO 2 –CHO into TAPT-TFPB COF@SiO 2 . The obtained TAPT-TFPB COF@SiO 2 /SiO 2 –CHO showed more favorable separation ability than SiO 2 –CHO and TAPT-TFPB COF@SiO 2 . Various aromatic compounds including alkylbenzenes , polycyclic aromatic hydrocarbons , environmental endocrine disruptors , foodborne stimulants and phenyl ketones were effectively separated on the TAPT-TFPB COF@SiO 2 /SiO 2 –CHO column in reversed phase chromatography mode. The silica microspheres surface-modified with triazine-containing imine-linked COFs proved to be a new type of promising chromatographic packing materials.
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LUMINESCENCE
·
2023
·Vol. 38
·期 11
·1938-1945
·
IF 2.9
Jiayan Shen,Long Li,Kehan Xu,Kaijun Wang,Yiping Du,Ting Wu,Huipeng Deng
A rapid and sensitive strategy was proposed for the detection of fluoranthene (FL), which is a polycyclic aromatic hydrocarbon (PAH), in water samples. In this work, syringe solid-phase extraction (SPE) combined with solid-phase fluorescence spectrometry was used to determine FL in PAHs polluted environmental samples. The fluorescence signals were directly monitored on the membrane surface after FL was enriched by syringe SPE. Under the optimal conditions, the proposed method showed a linear relationship in the concentration range 2–50 μg/L with a correlation coefficient ( R 2 ) of 0.998, and the limit of detection was 0.143 μg/L. The recoveries varied from 93.47% to 109.81% in the actual samples, with the relative standard deviations ( n = 3) ranging from 2.06% to 6.32%. According to the results, the established method can be applied in the field of rapid detection as it is fast, simple, portable, and highly sensitive, and has strong anti-interference.
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