JOURNAL OF CHROMATOGRAPHY A
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2020
·
IF 4.049
Luping Sun,Shuyun Zhu,Zhenjia Zheng,Jing Sun,Xian-En Zhao,Huwei Liu
Hydroxyl-polycyclic aromatic hydrocarbons (OH-PAHs) are biomarkers for assessing the exposure levels of polycyclic aromatic hydrocarbons (PAHs). A series of stable isotope mass tags (SIMT-332/338/346/349/351/354/360/363/374/377) were firstly designed and synthesized to perform multiplexed stable isotope labeling derivatization (MSILD) of OH-PAHs in human plasma and urine. Their derivatives were enriched and purified by magnetic dispersive solid phase extraction (MDSPE) using prepared Fe 3 O 4 /GO and then determined by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) in multiple reaction monitoring mode. 9-Plexed MSILD reagents were prepared using pipemidic acid as core structure with different isotope mass tags, in which carbonyl chloride group was used to label OH-PAHs. The SIMT-346 labeled OH-PAHs standards were used as internal standards, which can greatly increase the quantitative accuracy. 9-Plex labeled nine different real samples can be quantified by UHPLC-MS/MS in a single run. Under optimized MSILD-MDSPE conditions, good linearities of seven OH-PAHs were obtained with satisfactory coefficient of determination R 2 > 0.991. Limits of detection (LODs) of seven OH-PAHs were from 0.1 to 0.5 pg/mL, and limits of quantitation (LOQs) ranged from 0.5 to 2.0 pg/mL. The intra- and inter-day precisions ranged in 2.3–12.4% with accuracies in the range of 91.7–108.4%. Acceptable results of matrix effect (89.7–105.7%) and derivatization efficiency (> 96.4%) were obtained. In short, the developed method has been proved to be high-throughput, sensitive, accurate and easy-handling. This method was applied for the measurement of seven free OH-PAHs in human urine and plasma, and expected to provide technical support for the evaluation of PAHs exposure levels in humans.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2020
·
IF 4.192
Yong-Qiang Li,Li-Sha Bai,Cai-Xia Zhao,Jing-Jing Xu,Zhong-Juan Sun,Yan-Ling Dong,De-Xian Li,Xi-Li Liu,Zhi-Qing Ma
Insect carboxylesterases are major enzymes involved in metabolism of xenobiotics including insecticides. Two carboxylesterase genes, CarE001A and CarE001H, were cloned from the destructive agricultural pest Helicoverpa armigera. Quantitative real-time polymerase chain reaction showed that CarE001A and CarE001H were predominantly expressed in fat body and midgut, respectively; developmental expression analyses found that the expression levels of both CarEs were significantly higher in fifth-instar larvae than in other life stages. Recombinant CarE001A and CarE001H expressed in the Escherichia coli exhibited high enzymatic activity toward α-naphthyl acetate. Inhibition assays showed that organophosphates had strong inhibition on CarEs activity compared to pyrethroids. Metabolism assays indicated that CarE001A and CarE001H were able to metabolize β-cypermethrin and λ-cyhalothrin. Homology modeling and molecular docking analyses demonstrated that β-cypermethrin could fit nicely into the active pocket of both carboxylesterases. These results suggested that CarE001A and CarE001H could play important roles in the detoxification of pyrehtroids in H. armigera.
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ANALYTICA CHIMICA ACTA
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2021
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IF 6.558
Jiayang Zhang,Xueping Dang,Jiahuan Dai,Yuling Hu,Huaixia Chen
An electrochemical assistance solid-phase microextraction (EA-SPME) was developed based on amino functionalized multi-walled carbon nanotube/polypyrrole (MWCNTs-NH 2 /PPy) composite coating. It was applied for the extraction of eight phenols in food contact material, including 2-chlorophenol, o-cresol, m-cresol, 2,4-dichlorophenol, 4- tert -butylphenol, 4-chlorophenol, 4-tertoctylphenol and alpha-naphthol. MWCNTs-NH 2 /PPy coating was characterized by scanning electron microscopy, transmission electron microscope , X-ray energy spectrometer, X-ray diffraction, Fourier transform infrared and thermogravimetric analysis . The adsorption mechanism of phenols on the composite coatings was investigated. The coating modified steel-wire as an extraction fiber has good electroconductibility, reproducibility and long service life. A determination method for the eight phenols was established by EA-SPME coupled with gas chromatography-flame ionization detection. Under the optimal experimental conditions (extraction temperature: 40 °C; extraction time: 30 min; stirring rate: 600 rpm; NaCl concentration: 0.15 g mL −1 ; desorption temperature: 250 °C and desorption time: 4 min), the detection linear range was 0.005–50 μg L −1 ( R 2 >0.99), and the detection limit was 0.001–0.1 μg L −1 (S/N = 3). For the quintuple analysis of 50 μg L −1 phenols, the single fiber RSDs were 2.2–12.4%, and the fiber-to-fiber RSDs were 1.9–10.5%. The method was used to detect the migration quantity of the eight phenols from five canned packaging materials, which showed satisfactory recovery 87.3–118.9%.
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ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY
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2021
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IF 6.291
Zhijian Ke,Qian Zhu,Wankui Jiang,Yidong Zhou,Mingliang Zhang,Mingli Jiang,Qing Hong
Carbaryl is the representative of carbamate insecticide. As an acetylcholinesterase inhibitor, it poses potential threat to humans and other non-target organisms. Agrobacterium sp. XWY-2, which could grow with carbaryl as the sole carbon source, was isolated and characterized. The carH gene, encoding a carbaryl hydrolase, was cloned from strain XWY-2 and expressed in Escherichia coli BL21 (DE3). CarH was able to hydrolyze carbamate pesticides including carbaryl, carbofuran, isoprocarb, propoxur and fenobucarb efficiently, while it hydrolyzed oxamyl and aldicarb poorly. The optimal pH of CarH was 8.0 and the optimal temperature was 30 ℃. The apparent K m and k cat values of CarH for carbaryl were 38.01 ± 2.81 μM and 0.33 ± 0.01 s −1 , respectively. The point mutation experiment demonstrated that His341, His343, His346, His416 and D437 are the key sites for CarH to hydrolyze carbaryl.
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Analytical Methods
·
2019
·Vol. 11
·期 42
·5413-5420
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IF 2.378
Jiawei Li,Ping Yang,Rui Huang,Danqun Huo,Changjun Hou
An accurate, effective, and convenient method for identification of Baijiu (a distilled liquor popular in China) components could be important for its commercial management. Herein, we report, for the first time, a fluorescence-amplifying sensor array chip based on photonic crystals (PCs) employed to identify Baijiu components. Transmission electron microscopy and scanning electron microscopy were employed to characterize polystyrene microspheres and PCs, which exhibited characteristic uniform and compact arrangements. A spotting machine and fluorescence scanner were used for dye loading and data collection. Array performance was evaluated by pattern recognition and neural-network simulation. Our array chip was manufactured successfully and revealed outstanding discriminative ability for Baijiu. Compared with other liquid sensor arrays used only for configuration, our array chip possessed >90% leave-one-out accuracy after 10 days of dry storage under a N2 atmosphere. This simple and accurate method shows potential for quality control and detection in factories/markets.
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SCIENCE OF THE TOTAL ENVIRONMENT
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2019
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IF 5.589
Shanshan Sun,Haizhen Wang,Binxin Fu,Hao Zhang,Jun Lou,Laosheng Wu,Jianming Xu
Rhodococcus sp. WB9, a strain isolated from polycyclic aromatic hydrocarbons contaminated soil, degraded phenanthrene (PHE, 100 mg L −1 ) completely within 4 days. 18 metabolites were identified during PHE degradation, including 5 different hydroxyphenanthrene compounds resulted from multiple routes of initial monooxygenase attack. Initial dioxygenation dominantly occurred on 3,4-C positions, followed by meta -cleavage to form 1-hydroxy-2-naphthoic acid (1H2N). More than 95.2% of 1H2N was transported to and kept in extracellular solution without further degradation. However, intracellular 1H2N was converted to 1,2-naphthalenediol that was branched to produce salicylate and phthalate. Furthermore, 131 genes in strain WB9 genome were related to aromatic hydrocarbons catabolism, including the gene coding for salicylate 1-monooxygenase that catalyzed the oxidation of 1H2N to 1,2-naphthalenediol, and complete gene sets for the transformation of salicylate and phthalate toward tricarboxylic acid (TCA) cycle. Metabolic and genomic analyses reveal that strain WB9 has the ability to metabolize intracellular 1H2N to TCA cycle intermediates, but the extracellular 1H2N can’t enter the cells, restricting 1H2N bioavailability and PHE mineralization.
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Canadian Journal of Chemistry
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2019
·Vol. 97
·期 4
·
IF 1.252
Jun Wang,Junyi Xie,Libo Wang,Yan Jiang,Na Zhang
A salen nickel complex has been prepared in good yield with ethylenediamine, salicylaldehyde, and NiCl2·6H2O as raw materials. The structure of the complex was characterized by FTIR, 1H NMR, UV, and ESI-MS. Upon activation with methylaluminoxane (MAO), the precatalyst showed high activity for ethylene oligomerization. To reduce the simultaneous production of insoluble polymers during the nickel-catalyzed ethylene oligomerization, a series of phenolic compounds were introduced as modifiers for the production of linear α-olefins. The researched result showed that the phenolic compounds have a significant impact on the selectivity of oligomers and the concentration of polymers. With the increase of phenolic compounds, the content of polymers decreased and the distribution of oligomers gradually shifted toward lighter olefins. The sterically hindered 4-tert-butyphenol proved to be an especially efficient polymer-retarding modifier among the studied phenolic compounds in this work. Furthermore, the retarding effect of phenolic compounds toward insoluble polymers may be mainly related to their interaction with MAO, giving rise to larger MAO aggregates.
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JOURNAL OF MOLECULAR STRUCTURE
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2019
·
IF 2.12
Maocai Yan,Zhen Zhang,Jinhui Zhou,Wei Li,Chunyan Zhang,Jingchang Zhang,Huannan Wang,Xuelu Yang,Shuai Fan,Zhaoyong Yang
Maleimide skeleton distributes widely in a great many substances, and maleimides are very useful building blocks in organic synthesis and many related disciplines, like bioconjugation . As an excellent leaving group, tosyloxy (-OTs) group are very popular in organic synthesis; however, reports on use of -OTs group on maleimide scaffold are very rare. In this study, 3-tosyloxymaleimide was prepared from l -tartaric acid and used to react with various phenols or naphthols under PTC condition to give 3-aryloxymaleimides through nucleophilic substitutions. Yields of the reaction were not high due to a competitive transesterification reaction; however, this reaction would be practical if the side-reaction could be suppressed by appropriate reaction conditions. The reaction mechanism was investigated by theoretical computation. The intermediates and transition states of the reaction, as well as the potential barrier and reaction free energy , were calculated using density functional theory (DFT), and influencing factors of the reaction were discussed. Theoretical computations showed that this nucleophilic substitution is favorable both kinetically and thermodynamically, while electron-withdrawing groups on phenols are harmful to such reactions. This study will provide new knowledge and insights on the chemical properties of maleimide and tosyloxy group, as well as the related chemical reactions.
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Separation Science Plus
·
2019
·Vol. 2
·期 4
·120-128
·
IF 0
Xiao-Ling Huang,Hai-Hang Lan,Yi-Lun Yan,Gui Chen,Zi-Hao He,Kai Zhang,Song-Liang Cai,Sheng-Run Zheng,Jun Fan,Wei-Guang Zhang
Covalent organic frameworks are a new class of crystalline porous materials that have various potential applications. However, utilization of covalent organic frameworks as new stationary phases for gas chromatography separation has been less explored. In this work, a hydrazone-linked chiral covalent organic framework has been covalently bonded onto the inner surface of fused silica capillary. The fabricated hydrazone-linked covalent organic framework-bound capillary column displays a moderate polarity nature and exhibits relatively high resolution performances for separation of linear alkanes and alcohols, as well as aromatic positional isomers including xylene, nitrotoluene, chloronitrobenzene, benzenediol, and naphthol isomers. The present study reveals that the hydrazone-linked covalent organic framework-bound capillary column is quite promising for the gas chromatography separation of aromatic positional isomers.
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ACS Sustainable Chemistry & Engineering
·
2019
·
IF 6.97
Hongjing Wang,Dandan Yang,Songliang Liu,Shuli Yin,You Xu,Xiaonian Li,Ziqiang Wang,Liang Wang
The Au catalyst is attractive for electrochemical ammonia synthesis. The design of Au catalyst with favorable morphology and composition is significant for enhancing its performance. Herein, an effective and universal synthetic method is proposed to fabricate unique metal–nonmetal AuPdP nanowires (AuPdP NWs), which is simply performed by the solvothermal reaction of Au nanowires with Pd(PPh3)4. The facile hydrogen adsorption at Pd sites and weak binding to Au sites favor the selective hydrogenation of N2 to NH3. Moreover, phosphorus doping provides more sites for the nitrogen reduction reaction due to its rich valence electrons. Therefore, the AuPdP NWs exhibit superior electrocatalytic performance for electrochemical ammonia synthesis with high NH3 yield, faradic efficiency, and stability. The presented synthetic method provides an attractive strategy for the simultaneous incorporation of Pd and P into metallic catalysts with controlled morphology for various electrocatalytic applications.
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ACS Sustainable Chemistry & Engineering
·
2019
·
IF 6.97
Hongjing Wang,Dandan Yang,Songliang Liu,Shuli Yin,Hongjie Yu,You Xu,Xiaonian Li,Ziqiang Wang,Liang Wang
The electrocatalytic nitrogen to ammonia has attracted intensive attention but suffers from severe bottlenecks of low Faradaic efficiency and NH3 yield. Herein, we report a two-step process to prepare amorphous sulfur multilayer decorated gold nanowires (S/Au NWs) as superior catalysts for electrochemical NH3 production. The chemisorbed sulfur multilayers are favorable for selective hydrogenation of nitrogen to ammonia and provide sufficient exposed active sites for nitrogen reduction reaction (NRR). The S/Au NWs show a high NH3 yield of 21.04 μg h–1 mg–1cat. and Faradaic efficiency of 15.34%, as well as excellent durability. The superior NRR performance of Au catalysts with S chemisorption would stimulate interest toward NRR catalyst design of sulfur bonding to metal surfaces.
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JOURNAL OF CHROMATOGRAPHY A
·
2018
·
IF 3.716
Yanlong Chen,Wenfen Zhang,Yanhao Zhang,Zhifen Deng,Wenjie Zhao,Huifang Du,Xue Ma,Dan Yin,Fuwei Xie,Yu Chen,Shusheng Zhang
This study reports a novel strategy for the preparation of porous aromatic framework (PAF-6) coated magnetic nanoparticles (PAF-6 MNPs) using cyanuric chloride as a planar trigonal basis upon which to build a linear piperazine linker unit. The PAF-6 MNPs were examined as an efficient solid-phase extraction (SPE) sorbent for enrichment of trace organic pollutants including phenol, 2,4,6-trinitrophenol, naphthalene, naphthol, bisphenol A, 2,4-dichlorophenol and 3-nitrochlorobenzene in water. The high-performance liquid chromatography detection limits of such analytes were in the range of 0.08–5.02 ng/mL and recoveries were found to be 84.0–94.0% in well water, tap water, river water and wastewater. The main toxic components of cigarette smoke, including phenolic compounds and benzo[a]pyrene, are efficiently adsorbed by PAF-6 MNPs, and over 50% of such toxins are removed. Theoretical computations were performed to understand the molecular interaction mechanism between PAF-6 and such analytes. The results demonstrate that the PAF-6 MNPs sorbents show excellent adsorption of phenols, polycyclic aromatic hydrocarbons and nitroaromatics based on multiple π-π stacking and hydrogen-bond interactions. These results suggest that the PAF-6 MNPs can be applied to extraction, removal and determination of diverse trace multi-target analytes from complex media.
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