RSC Advances
·
2023
·Vol. 13
·期 39
·27535-27548
·
IF 3.9
Fang-chao Yang,Yang Yang,Long Yan,Feng-yun Wang,Lei Wu,Ming-zhu Xia,Xiao-Sen Li
Methyl-diethanolamine (CAS: 105-59-9), ethyl-diethanolamine (CAS: 139-87-7), and triethanolamine (CAS: 102-71-6) were identified as the degradation products and bio-markers of nitrogen mustard exposure. Sensitive and convenient detection methods for amino alcohol are of great importance to identify nitrogen mustard exposure in forensic analysis. Herein, analytical methods including gas chromatography-tandem mass spectrometry combined with heptafluorobutyryl derivatization and solid phase extraction were established for retrospective detection of the biomarkers in human plasma and urine samples. The efficiency of the method was improved by optimizing the conditions for sample preparation and the GC-MS/MS method. The optimization included the derivatization temperature, reaction time, reagent dosage and solid phase extraction cartridges, eluent and pH of the loading sample. The results indicated that the SCX cartridge resulted in better enrichment and purification effects, and the best recovery could be obtained with pH = 3–4 for the loading samples and an eluent of 2 mL 10% NH4OH/MeOH. The GC-MS/MS parameters were also optimized for better specificity and sensitivity. The established method was fully validated for each analyte both in plasma and urine matrixes. The linear range of analytes in plasma was 1.0–1000 ng mL−1 with a correlation parameter (R2) of ≥0.994, intra-day/inter-day accuracy of 93.7–117%, and relative standard deviation (RSD) of ≤6.5%. Meanwhile the results in urine were 1.0–1000 ng mL−1 with R2 of ≥0.996, intra-day/inter-day accuracy of 94.3–122%, and RSD of ≤6.6%. The detection limit of the analytes was 1.0 ng mL−1. The method was applied for the detection and identification of trace amino alcohols present in urine samples dispatched by the Organization for the Prohibition of Chemical Weapons (OPCW) and the results were confirmed to be correct.
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JOURNAL OF CHROMATOGRAPHY A
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2023
·
IF 4.1
Yangkun Sun,Shengli Ruan,Yuanyuan Zhou,Linhao Zhao,Wenjing Xiong,Chuhui Lin,Jingjing Kuang,Fanghong Ning,Min Zhang,Hongyang Zhang,Ping Hu
In this paper, we designed and manufactured a reliable magnetic solid phase extraction (MSPE) microfluidic chip for determination of polycyclic aromatic hydrocarbons (PAHs) in water combined with gas chromatography-mass spectrometry. Sample loading, washing and elution are implemented with microinjection pump and integrated on a single chip, which reduced manual operation. Magnets were used to fix octadecyl/phenyl bifunctional Fe 3 O 4 @SiO 2 extractant to avoid the design of weir structure in extraction chamber. The whole microfluidic chip was simple and low cost. Based on the microfluidic chip extraction platform, the on-chip MSPE method for the determination of PAHs was optimized and established. The results showed that this method required only 2 mL of sample, 2 mg of extractant, and 50 μL of elution organic solvent for whole on-chip MSPE process, which was environmentally friendly and consistent with green chemistry. Method verification results were displayed which the linear range of five PAHs was between 1-100 ng/mL with good linearity (R 2 ≥ 0.9985), and the detection limits (S/N = 3) were 0.08–0.26 ng/mL. The RSDs of intra-day precision (n=6) and inter-day precision (n=9) for PAHs were less than 6.1 % and 7.2 %, respectively. Enrichment factors were determined to be 31.3–37.7. The recoveries of river water, tap water, bottle water, waste water and urine at three spiked levels were in the range of 89.9% to 113.7% and the matrix effect values were between 83.8% to 109.6%. The extraction platform has the advantages of accurate analysis, simple design and cost-effective, which is conducive to the widespread use of microfluidic chips
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Catalysts
·
2023
·Vol. 14
·期 1
·24
·
IF 3.9
Chunlian Luo,Luwei Chen,Abdullah N. Alodhayb,Jianhua Wu,Mingwu Tan,Yanling Yang
The development of catalysts for low-temperature methane combustion is crucial in addressing the greenhouse effect. An effective industrial catalyst strategy involves optimizing noble metal utilization and boosting metal–metal interaction. Here, the PdNi-H catalyst was synthesized using the self-assembly method, achieving the high dispersion and close proximity of Pd and Ni atoms compared to the counterparts prepared by the impregnation method, as confirmed by EDS mapping. The XRD and TEM results revealed Pd2+and Ni2+doping within the CeO2lattice, causing distortions and forming Pd-O-Ce or Ni-O-Ce structures. These structures promoted oxygen vacancy formation in CeO2, and this was further confirmed by the Raman and XPS results. Consequently, the PdNi-H catalyst demonstrated an excellent redox ability and catalytic activity, achieving lower ignition and complete methane burning temperatures at 282 and 387 °C, respectively. The highly dispersed PdNi species played a pivotal role in activating methane for enhanced redox ability. Additionally, the narrow size distribution range contributed to more vacancies on the surface of CeO2, as confirmed by the XPS results, thereby facilitating the activation of gas phase oxygen to form oxygen species (O2−). This collaborative catalytic approach presents a promising strategy for developing efficient and stable methane combustion catalysts at low temperatures.
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2023
·
IF 8.6
Qi Zhao,Haicheng Jiang,Changchun Wang,Shuai Zhao,Lina Wang,Guodong Kang,Xingming Jie,Yiming Cao
In this study, as an efficient technology membrane absorption was applied with newly developed polyetheretherketone (PEEK) hollow fiber membrane (HFM) to remove CO 2 from flue gas. To alleviate membrane wetting issue, 1H,1H,2H,2H-perfluorodecyltrimethoxysilane (FAS) was integrated into polydimethylsiloxane (PDMS) and then crosslinked FAS-PDMS was coated on porous PEEK membranes to prepare composite membranes. Surface characterization verified that PDMS layer containing fluoroalkylsilane had been successfully formed on membrane surface. As mass ratio of FAS to PDMS in coating solution raised, an interesting honeycomb-like structure was observed dispersing on composite membrane surface. Meanwhile, water contact angle was improved from 90.0° to 133.5° indicating enhanced membrane hydrophobicity. The effects of gas and liquid flow velocities on CO 2 absorption performance of FAS-PDMS/PEEK HFM were systematically studied. The highest CO 2 removal efficiency of 99.6% was achieved when gas and liquid velocity were 0.027 and 0.019 m s −1 . When gas velocity raised to 0.110 m s −1 , the maximum absorption flux of 1.22 × 10 -4 mol m −2 s −1 and overall mass-transfer coefficient of 2.69 × 10 −5 m s −1 could be obtained. Compared with the original membrane, the CO 2 absorption flux of FAS-PDMS-0.6 HFM was increased by 50.9%, and the performance had no degradation in 36 h test. This study provides a novel strategy to alleviate the membrane wetting problem during CO 2 membrane absorption process.
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FOOD CONTROL
·
2023
·
IF 6
Qianqian Li,Bei Li,Chaoyang Zhang,Xiaoqian Zhou,Wei Liu,Yu Mi,Zuorong Xie,Yi Li,Jianxun Li
It is an urgent requirement to explore the key aroma of vine tea to provide the guidance for tea quality evaluation. In this study, three levels of vine tea of bud tip, tender leaf, and aged leaf were characterized by headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME/GC-MS). The relative odor activity value (rOAV) calculation coupled with gas chromatography-olfactometry (GC-O) technology were implemented to seek the aroma-active compounds. Afterwards, the chemometrics methods were employed to explore the critical volatile compounds on the basis of S-line, variable importance for projection (VIP), jack-knifing confidence interval, p values (<0.05), and fold change (FC). As a result, five aroma compounds of ethyl acetate, (E,E)-2,4-heptadienal, geraniol, hexanal, and geranyl acetone were considered as key markers by taking an overall consideration of rOAV, GC-O and chemometrics methods. Finally, the mathematical equation of the vine tea grade with respect to the key aroma was established. The ethyl acetate and geraniol were positively related with the vine tea level evaluation, whereas the hexanal, geranyl acetone, and (E,E)-2,4-heptadienal were negatively correlated with the tea grade, among which the hexanal played a significant role on tea level assessment. This study provides compelling evidence for the vine tea quality evaluation in the perspective of key aroma compounds.
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LANGMUIR
·
2023
·
IF 3.9
Zhimin Yang,Zefeng Wei,Yunpeng Xing,Liang Zhao,Yaqing Zhang,Congcong Xin,Teng Fei,Sen Liu,Tong Zhang
The development of room-temperature chemiresistive gas sensors with low limit of detection, high sensitivity, and selectivity for dimethyl methylphosphonate (DMMP) detection remains a challenge. Herein, a synergy of the two intermolecular hydrogen bond-promoted approach was proposed to fabricate a room-temperature DMMP sensor with enhanced performances. As a proof of concept, ternary p-hexafluoroisopropanol phenyl (HFIP) functionalized polypyrrole-reduced graphene oxide hybrids (HFIP-PPy-rGO) were rationally designed. During the sensing process, rGO serves as a conductive carrier, ensuring that the sensors operate at room temperature, and both HFIP and PPy act as adsorption sites for DMMP through hydrogen bonding interactions. As expected, the HFIP-PPy-rGO sensor exhibits high selectivity and sensitivity to DMMP. Besides, the HFIP-PPy-rGO sensor also possesses excellent linear response to DMMP and long-term stability. Experimental results and quartz crystal microbalance measurements prove that the specific recognition of DMMP is realized by forming two intermolecular hydrogen bonds between HFIP and DMMP, as well as PPy and DMMP. Additionally, the introduction of HFIP groups also contributes to adjusting device conductivity, enhancing signal conversion function. To put the DMMP sensor into potential practical application, the obvious sensing response to different DMMP concentrations in soil was confirmed, and a wireless detection system was built to realize real-time monitoring of DMMP concentrations in the surroundings. Overall, this study provides a facile and practical solution for improving the sensing performance of room-temperature sensors based on the hydrogen bond theory.
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CHEMICAL ENGINEERING JOURNAL
·
2023
·
IF 15.1
Xiang Li,Xueqian Wang,Li Yuan,Langlang Wang,Yixing Ma,You Wu,Yibing Xie,Rui Cao,Yiran Xiong,Ping Ning
The lengthy processes and cumbersome operations for the separate removal of COS and H 2 S have severely limited the development of blast furnace gas recycling process. CuO exhibits excellent H 2 S oxidation performance, but weak COS hydrolysis performance; in contrast, ZrO 2 shows the opposite trend. However, the functional combination of CuO and ZrO 2 has never been used for simultaneous removal of COS and H 2 S. In this study, a Cu/Zr co-doped K@TiO 2 bifunctional catalyst was tailored to simultaneously remove COS and H 2 S. The combined COS and H 2 S capacity of this catalyst reaches 340.5 mg/g at a low temperature of 60 °C, which is much higher than those of other reported bifunctional catalysts. The microcrystal structure formed by Cu/Zr co-doping increases the specific surface area of the catalyst and promotes the adsorption of COS/H 2 S. Specifically, Zr doping increases the content of moderate basic sites and significantly improves the hydrolysis efficiency of COS. Moreover, Cu doping induces lattice distortion of TiO 2 , while CuO captures 4 s valence electrons of K to form Cu 2 O. These two processes lead to the release of lattice oxygen from TiO 2 and CuO, generating oxygen vacancies and ·O 2 − , which promotes H 2 S oxidation. By proposing a simple route for the bifunctionalization of a desulfurization catalyst, this study drives innovation in both the theory and application of simultaneous removal of COS and H 2 S.
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SENSORS AND ACTUATORS B-CHEMICAL
·
2023
·
IF 8.4
Zi-ang Zhang,Li-fan Nie,Quan Zhou,Zhi-Dan Song,Ge-bo Pan
The structure and morphology of gas-sensitive materials were extremely important to performances of gas sensor. In this work, ZnO nano-crystalline (ZnO NCs) was synthesized on foam-like GaN (F-GaN) by sol-gel method as gas-sensitive materials of H 2 S gas sensor. When ZnO NCs/F-GaN composite structure was used as gas- sensitive materials for detection of H 2 S with the concentration of 50 ppm at 220 °C. Importantly, rapid response and recovery time was 78 and 31 s, respectively. Enhancement of the sensing response was mainly attributed to the combination between ZnO NCs and F-GaN. In addition, a multiphase catalytic mechanism was proposed to description the catalytic role of F-GaN in the gas sensing procedure. These results further broadened the application of as-prepared metal oxide semiconductor based GaN in the gas sensing field.
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POLYMER TESTING
·
2022
·
IF 4.931
Shanshan Jia,Songlin Deng,Yiqiang Wu,Yan Qing
Inspired by the biomaterial nacre, we report a versatile and facile strategy to rugged, flame retardant superhydrophobic materials by embedding a nacre-like montmorillonite (MMT) based gas barrier layer into hierarchical epoxy-resins. The well-aligned MMT layer imparted excellent oxygen and water barrier properties that rendered the coating surface water repellent yet protected the substrate materials from fire by suppressing heat and oxygen transfer. The hierarchical epoxy not only provided the robust superhydrophobic structure but offered strong adhesion to MMT layer. After application of this coating to a flammable sponge, it demonstrated superhydrophobicity with a contact angle of ∼153°. Furthermore, the material was rugged, resisting 1200 compression cycles and induced marked flame retardancy. The coated sponge delayed ignition (689% delay in ignition time) and promoted significant flame extinguishing property, compared with the uncoated material (demonstrated by LOI, CONE combustion, and fire scenario tests). Owing to its robustness and multifunctionality, the coated sponge was able to efficiently separate oil from multi-environments including strong corrosive, icy, boiling or vibrating mixtures. Additionally, the versatile application to wood, cotton, textile and other lignocellulosic substrates has been verified. This research opens up a new direction for durable waterproof and fireproof materials.
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2018
·
IF 0.827
Jianlin Zhuang,Jinmao You,Shijuan Zhang,Zhiwei Sun,Zhongyin Ji,Jiamin Liu,Yanxin Yu
A new fluorescence labeling reagent 1-(4-(1 H-phenanthro[9,10-d]imidazol-2-yl)phenyl)-1 H-pyrrole-5-dione (PIPD) used for the sensitive determination of thiols in food samples has been successfully prepared. Thiols were extracted by a gas purge microsyringe extraction (GP-MSE) device. The derivatization of PIPD with thiols could be finished within 10 minutes at 35 °C in weak alkaline condition, and the corresponding derivatives showed excellent fluorescence properties with excitation and emission wavelengths of 264 nm and 396 nm, respectively. The eight thiol derivatives could be easily separated on normal reversed phase column because of the introduction of highly hydrophobic PIPD unit into the target analytes. It is the first time that GP-MSE has been applied to the extraction of a wide range of thiols in food samples with only a small amount of methanol (0.5 mL) needed. The limits of detection (LODs) were in the range of 0.19–0.98 µg/kg, while the recoveries were in the range of 85.6%–97.1% with relative standard deviations (RSDs) < 4.98%. Good linearities were observed for all analytes with correlation coefficients of higher than >0.9995.GRAPHICAL
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CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 4
·657-667
·
IF 1.401
Yu Guo-Wei,Cheng Qiang,Nie Jing,Wang Xia-Jun,Wang Peng,Li Zu-Guang,Lee Maw-Rong
Abstract Deep eutectic solvent has been gaining much attention in recent years due to its various novel properties. The present study develops a novel microwave-assisted hydrodistillation method based on pretreatment using deep eutectic solvent, for the extraction of essential oil (EO) from dry fruits of Amomum kravanh , Amomum tsaoko, and Amomum villosum , respectively. The process is optimized by single-factor experiments taking the improvement in the essential oil yield of A. kravanh as the target. The results indicate that using the reaction product of choline chloride and ethylene glycol as the deep eutectic solvent with 7:1 of mass ratio to fruit powder, the optimal conditions are (1) pretreatment stage: 500 W of microwave power, 50 °C of temperature, and 7 min of duration; (2) fast heating stage: 600 W of microwave power, 110 °C of temperature, and 5 min of duration; (3) hydrodistillation stage: 300 W of microwave power, 110 °C of temperature, and 30 min of duration. Under these conditions, the EO yields of A. kravanh , A. tsaoko, and A. villosum are 3.64, 2.16, and 1.62%, respectively. The EOs are analyzed by gas chromatography–mass spectrometry, with totally 63 compounds identified. In most cases, the new method brings about more identified compounds than the traditional methods. Moreover, the relative contents of hydrocarbons in most essential oils are improved by applying the new method. Thus, the approach based on deep eutectic solvent has been proved superior in the enhancement of essential oil production. Graphical abstract
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CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 5
·799-807
·
IF 1.401
Wang F. Q.,Li J.,Wu J.-F.,Zhao G.-C.
Abstract In this study, magnesium/aluminum-layered double hydroxide (Mg/Al-LDH) was prepared with the hydrothermal method and the morphological features of Mg/Al-LDH were characterized. The as-prepared Mg/Al-LDH was employed as a coating material and coated on the stainless steel wire to construct a solid-phase microextraction fiber. To evaluate the extraction performance of the fiber, four phthalate esters including benzyl butyl phthalate, di- n -butyl phthalate, di- n -octyl phthalate and bis (2-ethylhexyl) phthalate were selected as model compounds. Several experimental parameters affecting the extraction efficiency, such as extraction temperature, extraction time and ionic strength, were optimized. Under the optimum conditions, linear ranges of 1–400 μg L −1 for di- n -butyl phthalate, 10–500 μg L −1 for di- n -octyl phthalate and 10–400 μg L −1 for two other compounds were observed. The limits of detection and limits of quantification ranged from 0.24 to 2.31 μg L −1 and 0.81 to 7.69 μg L −1 , respectively. The intra-day and inter-day precision are less than 15.3 and 8.7%. The relative standard deviation of fiber to fiber reproducibility ranged from 8.3 to 16.7%. Finally, the established method was satisfactorily applied to the determination of phthalate esters in the Yangtze River water samples and the recoveries were 76.1–110.6%. Graphical Abstract
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