CHINESE JOURNAL OF CHEMICAL ENGINEERING
·
2020
·
IF 2.627
Cui-Ping Ye,Ya-Fei Qiao,Rui-Nan Wang,Wen-Ying Li
To identify the effect of solvents and anthracene on the purification of carbazole, the solvent crystallization of carbazole was investigated with xylene, chlorobenzene and tetrachloroethylene (TCE) as solvents under two forced circulation cooling (FCC) modes. The co-crystalline experimental data were obtained from runs carried out at different anthracene levels between 1% (mass) and 10% (mass). The results showed that a uniform flake carbazole crystal obtained when using xylene and chlorobenzene under the FCC-1 mode with gradual cooling rate. Nevertheless, fine flake crystals grown under shock cooling of FCC-2 mode. It is beneficial to improving the purity of carbazole with chlorobenzene as solvent under cooling mode of FCC-1. Anthracene could promote the growth of carbazole in solution, and it has a significant influence on the purification of carbazole.
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MICROCHEMICAL JOURNAL
·
2020
·
IF 3.594
Zhengdong Shen,Haiying Wang,Qian Yu,Qiang Li,Xiaomin Lu,Xianming Kong
The accumulated polycyclic aromatic hydrocarbons (PAHs) in edible oil can bring serious health concerns because of their carcinogenic features. PAHs could accumulate in edible oil from contaminated environment or food stuff. In this study, the combination uses of on-site thin layer chromatography and surface enhanced Raman scattering (SERS) spectroscopy has been successfully displayed to identify PAHs from edible oil samples. Diatomite which is a kind of porous biosilica was used to construct stationary phase on TLC plate, the photonic crystal feature of diatomite is beneficial for SERS enhancement. The highly-porous stationary phase composed of porous diatomite with void shell structure could promote mobile phase interaction with the stationary phase, which leading to improved mass transfer, uniformity and analyte resolution compare with the conventional silica gel plate. The edible oil (1 µL) was directly applied to the diatomite plate without pretreatment, and subjected to TLC separation. The polarity of target analytes was calculated for eluent optimization, on which four compounds of PAHs(benzo[a]pyrene, pyrene, anthracene and indeno[1,2,3-cd] pyrene) were successfully separated by using hexane/chloroform (15/1, v/v) as eluent, including compounds with similar polarity(benzo[a]pyrene 0.0477, indeno[1,2,3-cd] pyrene 0.6545, pyrene and anthracene are 0). 2 µL of Au colloid at 2.4 × 10 −7 M were transferred onto the diatomite plate for the SERS measurement. The limit of detection was found to be nearly at 1 ppm. The obtained results can easily identify the four compounds of PAHs in edible oil by their own characteristic Raman peaks. This proposed method provides a simple, instant and effective strategy for on-site identification PAHs from food samples.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 413
·期 7
·1983-1997
·
IF 4.157
Jing Qi,Chen Liyuan,Zhao Qiaowei,Zhou Peipei,Li Yanyan,Wang Huili,Wang Xuedong
Herein, we developed a novel effervescence-assisted dual microextraction method, abbreviated as EM-LPSH, using lighter-than-water phosphonium-based ionic liquids (LPILs) and switchable hydrophilic/hydrophobic fatty acids (SHFAs). The EM-LPSH method was utilized for quick enrichment/extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oils. Owing to lower density than water, LPILs used as the first extractant were floated on the upper layer of the aqueous phase, leading to a convenient separation/collection compared with traditional heavier-than-water imidazolium-based ionic liquids. Interestingly, SHFAs play triple functions: a dispersive solvent in the microextraction process, an acidic source in effervescent reaction, and the second extractant in dual microextraction, due to switchability from hydrophilicity to hydrophobicity. Consequently, the integration of LPILs with SHFAs greatly enhanced the extraction efficiency for PAHs owing to the quick dual microextraction process. Some important variables were rigorously optimized using a one-factor-at-a-time approach. Under optimized conditions, the EM-LPSH/HPLC-FLD method provided a wide linear range (0.07~0.63–200 μg kg −1 ), satisfactory recovery (80.12–103.27%), and low limit of detection (0.02–0.19 μg kg −1 ), as well as high intra-day and inter-day precision (0.03–6.55) for six PAHs in edible oils. By using certified reference material in olive oil samples (GBW10162), the recoveries ranged from 97.40 to 98.39%, demonstrating high accuracy and precision. According to the detected levels of PAHs in six unheated and heated oils, their edible safety was evaluated in detail. In short, the newly developed method is simple, convenient, and highly efficient, thereby showing great prospects for application in conventional monitoring of trace-level PAHs in edible oils.
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Catalysts
·
2020
·Vol. 10
·期 12
·1379
·
IF 3.52
He Liu,Shiguang Fan,Xu Gong,Jian Wang,Aijun Guo,Kun Chen,Zongxian Wang
Partial hydrogenation of anthracene under CO-H2O, N2-H2O, and H2-H2O over Fe-based catalysts was studied at 400 °C and 10 MPa. Results show that the Fe-based catalysts display obvious catalytic activity for anthracene hydrogenation under CO-H2O instead of hydrogenation under N2-H2O and H2-H2O. The activity follows in the order of Fe(NO3)3·9H2O > Fe naphthenate > FeSO4·7H2O. Even though the amount of molecular hydrogen remains higher than that of in situ hydrogen, the anthracene conversion with in situ hydrogen is remarkably higher. It demonstrates that the in situ hydrogen is more active than molecular hydrogen for PAH hydrogenation. To further reveal the exact fate of these Fe-based catalysts, the decomposed products under CO-H2O, N2-H2O and H2-H2O were characterized by TG, XRD, and TEM. Results indicate that the Fe3O4species play a key role in hydrogenation of anthracene under CO and H2O. Higher catalytic activity for Fe(NO3)3·9H2O is due to its complete decomposition at 350 °C to acquire higher concentration of active Fe3O4species. The possible form of in situ hydrogen during this process is also discussed. Given that heavy oil contains abundant polyaromatics, these results are meaningful for enhancing hydrogen shuttling to heavy oil by producing natural hydrogen donors and, thus, benefiting the high-efficient upgrading.Keywords:PAH hydrogenation;in situ hydrogen;water gas shift reaction;natural hydrogen donors
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MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 4
·1-8
·
IF 6.232
Li Lin,Han Dandan,Wang Mingwei,Han Yehong,Yan Hongyuan
A composite was synthesized from two-dimensional molybdenum disulfide (MoS 2 ) nanosheets and hypercrosslinked polymers (HCP), and the composite was characterized by infrared spectroscopy, scanning electron microscopy, and specific surface area. The fluffy and porous structure and multiple adsorption sites (π-interaction, static electricity, hydrogen bonding) make it ideal for use as an adsorbent. A pipette tip solid-phase extraction with the composite as the adsorbent combined with HPLC–FLD was developed to determine trace amounts of polycyclic aromatic hydrocarbons (phenanthrene, anthracene, fluoranthene, pyrene, benzo(α)anthracene) in environmental water. Under optimal extraction conditions, the method has a wide linear range (0.5–100 ng mL −1 ) and low limit of detection (0.024–0.099 ng mL −1 ), and the recoveries of PAHs from spiked environmental water were 73.8% to 123.6% (relative standard deviation ≤ 6.7%, n = 3).
Schematic representation of a three-dimensional molybdenum disulfide–ethylenediamine–hypercrosslinked polymer composite (MoS 2 –EDA–HCP) using pipette tip solid-phase extraction adsorbent for extracting trace levels of polycyclic aromatic hydrocarbons (PAHs) prior to HPLC–FLD. HCP, hypercrosslinked polymer; MoS 2 , molybdenum disulfide; EDA, ethylenediamine
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JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Xiaohuan Zang,Yachao Pang,Hongda Li,Qingyun Chang,Shuaihua Zhang,Chun Wang,Zhi Wang
A covalent organic framework modified graphitic carbon nitride (g-C 3 N 4 @TpBD) was synthesized by modifying the graphitic carbon nitride (g-C 3 N 4 ) with a covalent organic framework (COF-TpBD). The synthesis conditions including the mass ratio between g-C 3 N 4 and benzidine (BD), solvent type, reaction temperature and reaction time were optimized. Under the optimal synthetic conditions, a novel spiny dendritic g-C 3 N 4 @TpBD adsorbent was obtained. The g-C 3 N 4 @TpBD was then coated on stainless-steel wire by sol-gel technique and the coated fiber was used for the solid phase microextraction of polycyclic aromatic hydrocarbons prior to gas chromatography-mass spectrometric detection. The established method was successfully applied to determine eight PAHs in six environmental water samples. Under the optimal extraction conditions, a wide linear quantification range for the analytes was obtained from 0.07 to 60.0 ng mL −1 with the coefficients of determination varying from 0.9979 to 0.9998, and the limits of detection (S/N = 3) ranged from 0.02 to 0.05 ng mL −1 . The relative recoveries of the analytes for the six environmental water samples at the spiked concentrations of 0.2, 0.5, 3.0 and 30.0 ng mL −1 were between 83.6% and 118% with the relative standard deviations ranging from 2.4% to 11.3%.
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Wenjin Wang,Shuaihua Zhang,Zhi Li,Jinqiu Li,Xiumin Yang,Chun Wang,Zhi Wang
Honey, a highly nutritious functional food, might be contaminated by polycyclic aromatic hydrocarbons (PAHs) during its production and/or harvest. The preconcentration and analysis of trace levels of PAHs from the complex sample matrices like honey still poses challenges for analytical researchers. In this study, three different covalent triazine-based frameworks (CTFs) were synthesized and explored as the solid-phase microextraction (SPME) coating for the extraction of some PAHs from various honey samples. Among the CTFs, cyanuric chloride- p -quaterphenyl (CC-QP) exhibited the highest extraction capability toward PAHs due to its largest specific surface area and π-electrons system. Under the optimum experimental conditions, the CC-QP based SPME method exhibited wide linearity (0.10–100 ng g −1 ), low limits of detection (0.03–0.19 ng g −1 ) and good reproducibility (relative standard deviations < 9.9%). The new SPME method coupled with chromatography-mass spectrometry detection was successfully applied for the determination of PAHs in honey samples with satisfactory recoveries (82.0–116.8%).
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MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 6
·1-9
·
IF 6.232
Chen Yang,Huang Ailan,Zhang Lu,Bie Zijun
A highly oriented crystalline metal-organic framework (MOF) nanofilm array was prepared and used for surface-assisted laser desorption ionization mass spectrometry (SALDI-MS) for determination of small molecules. The MOF nanofilm was characterized using scanning/transmission electron microscopy, X-ray diffraction, and ultraviolet-visible spectroscopy. Different small molecules (anthracene, n-eicosanoic acid, Rhodamine B) were successfully determined by this MOF nanofilm array with limits of detection (LOD) between 0.1–5 ng·mL −1 and limits of quantification (LOQ) between 1 and 10 ng·mL −1 . Compared to previously reported MOF-based SALDI-MS, this array exhibits better reproducibility (3.3–5.2%) and recovery (89–105%). The intensity of the MS peak remains the same after 25 repeated cycles. This indicates good repeatability. This MOF nanofilm-based SALDI-MS array can be used for determination of fatty acid and Rhodamine B in real samples with good recovery (83–106%).
Schematic representation of the principle of crystalline MOFs nanofilm-based SALDI-MS array
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JOURNAL OF SEPARATION SCIENCE
·
2020
·Vol. 43
·期 18
·3655-3664
·
IF 2.878
Herman Maloko Loussala,Sen Han,Juanjuan Feng,Min Sun,Jiaqing Feng,Jing Fan,Meishan Pei
To enhance the extraction performance, a mesoporous silica was modified with ordered mesoporous carbon for solid-phase microextraction. Three stainless-steel wires coated with the mesoporous material were placed in a polyetheretherketone tube for getting an extraction tube. The tube was coupled to high-performance liquid chromatography with diode array detector, and the online analysis system was constructed. Then its extraction performance was evaluated using hydrophobic polycyclic aromatic hydrocarbons, phthalates, and hydrophilic neonicotinoids. The best selectivity was presented for polycyclic aromatic hydrocarbons. Several main conditions were optimized such as sampling volume, sampling rate, methanol concentration in the sample, and desorption time, a rapid and sensitive analytical method was established toward polycyclic aromatic hydrocarbons. The analytical method exhibited wide linear range from 0.017 to 15 µg/L with acceptable correlation coefficients more than 0.9990, limits of detection in 0.005-0.020 µg/L, limits of quantification ranging from 0.017 to 0.066 µg/L as well as large enrichment factors of 377-2314. It was successfully applied to detect trace polycyclic aromatic hydrocarbons in some real water samples including tap water, snow water, and domestic sewage.
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2020
·Vol. 27
·期 33
·41458-41474
·
IF 3.056
Sun Kailun,Song Yan,Zong Wansong,Tang Jingchun,Liu Rutao
At present, research progress of anthracene’s toxicity lags far behind the pollution caused on its application fields such as petroleum and minerals. In this paper, anthracene-induced oxidative stress effects and genetic toxicity were investigated at both the molecular and cellular levels. The intracellular oxidative stress effect of anthracene on earthworm primary coelomocyte was confirmed by the detection of reactive oxygen species, antioxidant enzymes activity, and malondialdehyde content. Moreover, after anthracene exposure, the decrease in the mitochondrial membrane potential and cell viability also indicated the adverse effects of anthracene on earthworm coelomocyte. The comet assay proved the break in DNA strand, revealing the anthracene-induced DNA damage. On the molecular level, we revealed that anthracene caused the shrinkage of the catalase skeleton and altered the microenvironment of chromophores of catalase by multi-spectral methods. Molecular simulation results indicated that anthracene interacted with His74 by “arene-arene” force and the dominant binding site between anthracene and catalase was close to the active site of catalase. In addition, anthracene was shown to bind to the DNA molecule by groove binding mode. This study proposed a new combined analysis method for the toxicity evaluation of anthracene at the cellular and molecular levels.
This study creatively proposed a new combined analysis for the toxicity evaluation of ANT at the cellular and molecular levels.
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JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 43
·期 3
·622-630
·
IF 2.516
Chunying Li,Min Sun,Xiangping Ji,Sen Han,Jiaqing Feng,Wenjuan Guo,Juanjuan Feng
Triazine-based organic polymers@SiO 2 nanospheres were prepared and applied as an extraction coating onto stainless steel wires and the wires were filled into polyetheretherketone tube for in-tube solid-phase microextraction. Taking polycyclic aromatic hydrocarbons as targets, main factors affecting extraction performance of the tube were investigated through coupling to high performance liquid chromatography. Under the optimum conditions, an online analytical method for polycyclic aromatic hydrocarbons was established with large linear ranges (0.010-20 µg/L), low limits of detection (0.003-0.010 µg/L), high enrichment factors (533-2954), and good repeatability (relative standard deviations <1.7% for intraday test, <5.0% for interday test). The analysis method was successfully applied to the detection of trace targets in real water samples and the relative recoveries ranged from 82.9 to 119.9%, which demonstrated the applicability of extraction tube in sample preparation.
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ADVANCED FUNCTIONAL MATERIALS
·
2019
·Vol. 29
·期 49
·1905576
·
IF 15.621
Dan Han,Dongya Ni,Qing Zhou,Jingjing Ji,Yanqin Lv,Yanfei Shen,Songqin Liu,Yuanjian Zhang
Rapid screening of polycyclic aromatic hydrocarbons (PAHs), a large class of toxic and carcinogenic compounds, is highly desirable for environmental and food safety. In principle, a photoluminescent (PL) assay is a potential route, but demands highly efficient and stable, low cost, and environment-friendly photoactive materials. 2D carbon nitride nanosheets (CNNS) that have triggered increasing interest may meet all these requirements. However, conventional applications of CNNS are restricted in aqueous solution, in which the long-term dispersibility is difficult to be addressed. Here, the harnessing of unique PL properties of CNNS is reported by dispersing them in a hierarchical polymeric matrix, driven by electrostatic interactions. Such a configuration not only enables a solid-state host to perpetually maintain homogeneous dispersibility of CNNS but also processes free channels for sufficient mass transfer. Moreover, the nanohybrid inherits the unique PL properties of CNNS. Further using β-CD as the molecular recognition unit, an economic, highly selective and sensitive paper-based PL sensor for PAHs is constructed via an inner-filter effect. This work opens a new avenue in harnessing unique PL properties of CNNS in solid state with superior stability for a variety of potential sensing applications, especially for point-of-care testing and/or in developing countries.
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