SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY
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2023
·
IF 4.4
Kun Huang,Hai-Long Wu,Tong Wang,Ming-Yue Dong,Xiao-Qin Yan,Ru-Qin Yu
Polycyclic aromatic hydrocarbons (PAHs), as a class of organic pollutants that have attracted much attention, are likely to be formed with the production and processing of plastic products, and they may migrate from contaminated plastic products to food, causing the risk of poisoning or cancer. In this study, migration tests were carried out on disposable plastic products for food contact, and a novel strategy that combines excitation-emission matrix (EEM) fluorescence spectroscopy with the advanced second-order calibration method based on the three-direction resection alternating trilinear decomposition (TDR-ATLD) algorithm was used to monitor the migration of three PAHs anthracene (ANT), pyrene (PYR), and phenanthrene (PHE) from the plastic products to food simulants in real-time. With the “second-order advantage”, even if the fluorescence spectra of the target analytes overlapped seriously, and other unknown substances migrated from the plastic products to food simulants, accurate qualitative and quantitative results were still obtained by the proposed method. In the static system, the coefficient of determination ( R 2 ) of the three PAHs within the calibration range were all greater than 0.99, and the average spiked recoveries were 99.5-107.1%, with the standard deviation lower than 8.9%. The figures of merit (FOMs) and intra- or inter-day precision also showed good feasibility and reliability of the method. In the simulation study of the migration kinetic process, three PAHs can be quantified in real-time in complex matrix, then the related migration equations were established. The results indicate that the proposed method can be used for real-time migration quantitative monitoring of PAHs, providing a potential and available method for the study of the migration kinetics of hazardous substances from food contact materials to food or food simulants.
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MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Xiaomei Chen,Liulin Wei,Qian Liu,Xueyun Gao,Jingchan Zhao
In the present study, a novel temperature-sensitive hyperbranched polysiloxane dispersive liquid–liquid microextraction combined with high-performance liquid chromatography method (TS-HBPSi-DLLME-HPLC-UV) has been developed for the determination of five polycyclic aromatic hydrocarbons (PAHs) in instant noodles, in which temperature-sensitive hyperbranched polysiloxane (p(Ph-HBPSi-co-NIPAM)) was used as the extraction solvent. The method adsorbs the target analytes based on π-π and hydrophobic interaction between p(Ph-HBPSi-co-NIPAM) and PAHs, and then separates the polymer with the adsorbed target analytes from the solution by a phase transition. Microextraction parameters of the method including polymer ratio, type and concentration of salt, pH, extraction time and volume of acetonitrile were examined in detail and optimized. At the optimum conditions, the established method showed good linearity (R 2 ≥ 0.9971) with satisfactory limits of detection (0.089–0.16 ng mL −1 ) and limits of quantitation (0.27–0.48 ng mL −1 ). The values for intra-day and inter-day precisions were lower than 3.2% and 4.4%, respectively. Enrichment factors (EFs) and extraction recoveries (ERs) ranged from 62 to 70 and 75 to 85%, respectively. Finally, the proposed microextraction technique was validated by analyte addition and recovery studies, and applied to the determination of five PAHs in instant noodles, demonstrating that temperature-sensitive hyperbranched polymers have great potential for application in sample pretreatment techniques.
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CHINESE JOURNAL OF CHEMICAL ENGINEERING
·
2023
·
IF 3.8
Xudong Zhang,Yanhua Liu,Jun Shen,Yugao Wang,Gang Liu,Yanxia Niu,Qingtao Sheng
Carbazole is an irreplaceable basic organic chemical raw material and intermediate in industry. The separation of carbazole from anthracene oil by environmental benign solvents is important but still a challenge in chemical engineering. Deep eutectic solvents (DESs) as a sustainable green separation solvent have been proposed for the separation of carbazole from model anthracene oil. In this research, three quaternary ammonium-based DESs were prepared using ethylene glycol (EG) as hydrogen bond donor and tetrabutylammonium chloride (TBAC), tetrabutylammonium bromide or choline chloride as hydrogen bond acceptors. To explore their extraction performance of carbazole, the conductor-like screening model for real solvents (COSMO-RS) model was used to predict the activity coefficient at infinite dilution ( γ ∞ ) of carbazole in DESs, and the result indicated TBAC:EG (1:2) had the stronger extraction ability for carbazole due to the higher capacity at infinite dilution ( C ∞ ) value. Then, the separation performance of these three DESs was evaluated by experiments, and the experimental results were in good agreement with the COSMO-RS prediction results. The TBAC:EG (1:2) was determined as the most promising solvent. Additionally, the extraction conditions of TBAC:EG (1:2) were optimized, and the extraction efficiency, distribution coefficient and selectivity of carbazole could reach up to 85.74%, 30.18 and 66.10%, respectively. Moreover, the TBAC:EG (1:2) could be recycled by using environmentally friendly water as antisolvent. In addition, the separation performance of TBAC:EG (1:2) was also evaluated by real crude anthracene, the carbazole was obtained with purity and yield of 85.32%, 60.27%, respectively. Lastly, the extraction mechanism was elucidated by σ -profiles and interaction energy analysis. Theoretical calculation results showed that the main driving force for the extraction process was the hydrogen bonding ((N–H … Cl) and van der Waals interactions (C–H … O and C–H … π), which corresponding to the blue and green isosurfaces in IGMH analysis. This work presented a novel method for separating carbazole from crude anthracene oil, and will provide an important reference for the separation of other high value-added products from coal tar.
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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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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
·
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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CHEMOSPHERE
·
2023
·
IF 8.8
Wei Zhang,Wenjie Wu,Jianfei Wu,Xiaobin Liu,Jian Tian,Heng Li,Qingbiao Li,Yanmei Zheng
Although advanced oxidation processes (AOPs) based on persulfate (PS) is an attractive approach for repairing polycyclic aromatic hydrocarbons (PAHs) contaminated soils, limited oxidizability of PAHs and efficient in-situ activation of PS hinder its practical applications. In this study, we comprehensively examined the contributions of five representative surfactants on the oxidative remediation of PAHs-contaminated soil in terms of degradation kinetics of the pollutants, and further proposed an innovative coupling strategy of surfactant-enhanced thermally activated PS remediating PAHs-contaminated soil. The results showed that the degradation process of PAHs in soil was significantly facilitated only via adding sodium dodecyl benzenesulfonate (SDBS) and fitted the pseudo-first-order kinetic pattern. The removal of phenanthrene (PHE) reached 98.56% at 50 mM PS, 50 °C, 5 g L −1 SDBS and 48 h reaction time, accompanying an increase of 25% in reaction rate constant from 0.0572 h −1 (without SDBS) to 0.0715 h −1 . More importantly, SDBS-enhanced thermally activated PS degrading PAHs with higher benzene rings were more effective as the reaction rate constants of pyrene (PYR) and benzo(a)anthracene (BaA) were significantly increased by 49.40% and 56.86%. Additionally, only appropriate dosages (5–10 g L −1 ) of SDBS facilitated the oxidative degradation of PHE, as well as the aging time of contaminant-soil contact slowed down the enhancement of oxidative degradation of PHE by SDBS. Scavenger experiments demonstrated that SO 4 ·- and 1 O 2 were the dominant reactive oxygen species . Finally, a possible oxidative degradation pathway of PHE was proposed, and the toxicity of derived intermediates got alleviation by the assessment using the Toxicity Estimation Software Tool . This investigation was promising for in situ scale-up remediation of PAHs-contaminated soil.
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Journal of Materials Chemistry C
·
2023
·Vol. 11
·期 25
·8446-8453
·
IF 6.4
Minghui Zhang,Shikun Zhao,Zhen Qin,Yuhuan Lv,Han Zhu,Biao Zhao,Kai Pan
Flexible porous Janus-structured fluorescent nanofibers with white-light emission are obtained by a side-by-side electrospinning technique. Experimental results show that the combination of porous structure and Janus structure on one single nanofiber is conducive to controlling the fluorescence properties for achieving white-light emission. The porous structure can effectively increase the fluorescence area of fluorescent molecules and weaken the blocking effect of the polymer carrier, thus improving the utilization efficiency of fluorescent molecules inside the nanofiber. Besides, the Janus structure effectively realizes the spatial isolation of the donor and acceptor to inhibit the energy transfer between each other. Moreover, the prepared porous Janus nanofibers have the characteristics of excellent hydrophobicity, strong flexibility and designable shape. This paper provides a practical idea for the preparation of new fluorescent nanomaterials, which has great application potential in the field of flexible displays.
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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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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Chengjiang Zhang,Yuhuang Li,Hongmei Yuan,Zeyi Lu,Qi Zhang,Lirong Zhao
Covalent organic frameworks (COFs) are a burgeoning class of crystalline porous materials with unique properties and have been considered as a promising functional extraction medium in sample pretreatment. In this study, a new methacrylate-bonded COF (TpTh-MA) was well designed and synthesized via the aldehyde-amine condensation reaction, and the TpTh-MA was incorporated into poly (ethylene dimethacrylate) porous monolith by a facile polymerization reaction inside capillary to prepare a novel TpTh-MA monolithic column. The fabricated TpTh-MA monolithic column was characterized with scanning electron microscope, Fourier transform infrared spectrometer, X-ray diffraction, and N 2 adsorption–desorption experiments. Then, the homogeneous porous structure, good permeability and high mechanical stability of TpTh-MA monolithic column was used as separation and enrichment media of capillary microextraction, which was coupled with high-performance liquid chromatography fluorescence detection for online enrichment and analysis of trace estrogens. The main experimental parameters influencing the extraction efficiency were systematically investigated. The adsorption mechanism for three estrogens was also explored and discussed based on hydrophobic effect, π-π affinity and hydrogen bonding interaction, which contributed to its strong recognition affinity to target compounds. The enrichment factors of the TpTh-MA monolithic column micro extraction method for the three estrogens were 107–114, indicating a significant preconcentration ability. Under optimal conditions, a new online analysis method was developed and exhibited good sensitivity and wide linearity range of 0.25–100.0 µg·L -1 with a coefficient of determination ( R 2 ) higher than 0.9990 and a low limit of detection with 0.05–0.07 µg·L -1 . The method was successfully applied for online analysis of three estrogens of milk and shrimp samples and the recoveries obtained from spiking experiments were in range of 81.4–113% and 77.9–111%, with the relative standard deviations of 2.6–7.9% and 2.1–8.3% ( n = 5), respectively. The results revealed the great potential for the application of the COFs-bonded monolithic column in the field of sample pretreatment.
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MOLECULES
·
2023
·Vol. 28
·期 8
·3542
·
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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