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International Journal of Analytical Chemistry · 2021 ·Vol. 2021 ·期 1 ·9980212 · IF 1.885

An Effective and Efficient Sample Preparation Method for 2-Methyl-Isoborneol and Geosmin in Fish and Their Analysis by Gas Chromatography-Mass Spectrometry

Liang-liang Tian,Feng Han,Essy Kouadio Fodjo,Wenlei Zhai,Xuan-Yun Huang,Cong Kong,Yong-Fu Shi,You-Qiong Cai

The intensive aquaculture strategy and recirculating aquaculture system often lead to the production of off-flavor compounds such as 2-methyl-isoborneol (2-MIB) and Geosmin (GSM). The regular purge and trap extraction followed by analysis with gas chromatography-mass spectrometry (GC-MS) usually involve a complicated assembly of facilities, more working space, long sample preparation time, and headspace solid-phase microextraction (SPME). In this work, a method with easier sample preparation, fewer and simplified facilities, and without SPME on GC-MS analysis is developed for the determination of 2-MIB and GSM in fish samples. Unlike previous methods, solvent extract from samples, QuEChERS-based cleanup, and solid-phase extraction for concentration are applied. The LOD (S/N > 3) and LOQ (S/N > 10) of this method were validated at 0.6 μ g/kg and 1.0 μ g/kg for both 2-MIB and GSM, which are under the sensory limit (1 μ g/kg). Application of this method for incurred fish samples demonstrated acceptable analytical performance. This method is suitable for large-scale determination of 2-MIB and GSM in fish samples, owing to the use of simple facility and easy-to-operate procedure, rapid sample preparation, and shorter time for GC-MS analysis without SPME.

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Analytical Methods · 2015 ·Vol. 7 ·期 20 ·8793-8800 · IF 1.821

Graphene grafted magnetic microspheres for solid phase extraction of bisphenol A and triclosan from water samples followed by gas chromatography-mass spectrometric analysis

Xiaohuan Zang,Qingyun Chang,Mengying Hou,Chun Wang,Zhi Wang

Graphene grafted magnetic microspheres were prepared and used as the adsorbent for magnetic solid phase extraction (MSPE) of bisphenol A and triclosan from water samples prior to their determination by gas chromatography-mass spectrometric (GC-MS) detection. A new customized ground-glass stoppered conical flask with a side tube was used for MSPE operations to simplify the separation of the magnetic adsorbent from the sample solution. The main experimental factors affecting the extraction recoveries of the analytes including the amount of adsorbent, pH of the sample solution, extraction time, salt concentration, desorption conditions, and derivatization conditions were investigated. Under the optimal conditions, a linear response was observed in the concentration range of 0.05–2.50 μg L−1 for bisphenol A and 0.10–5.00 μg L−1 for triclosan. The limits of detection (S/N = 3) were 10.0 ng L−1 for bisphenol A and 20.0 ng L−1 for triclosan. The established method was applied to the determination of bisphenol A and triclosan residues in environmental water samples with satisfactory results. The recoveries of the analytes using this method from lake, river, bottled and tap water samples were in the range from 93.9% to 104.3% (intra-day), and from 93.5% to 99.5% (inter-day) with the relative standard deviations varying from 2.1% to 5.8% (intra-day), and from 3.1% to 5.7% (inter-day).

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Food Quality and Safety · 2025 · IF 4.4

Detection of citronellol in sweetpotato black spot disease using a quartz crystal microbalance (QCM) gas sensor based on Co/Zn-ZIF@MIP composite

Lu Xinghua,Liu Suqi,Zhang Lu,Wang Chenglong,Wang Zhenhe,Pang Linjiang,Lu Guoquan,Cheng Jiyu,Chen Wei,Guan Yuge

Citronellol is a kind of terpene produced by plants in response to external stress, thus can be used as a gas biomarker to detect black spot Ceratocystis fimbriata infection in sweetpotato. However, many contemporary analytical methods, exemplified by gas chromatography-mass spectrometry (GC-MS), are technically demanding, time-consuming, and require complex sample preparation procedures. In this study, a quartz crystal microbalance (QCM)-based gas sensor fabricated via a surface molecular imprinting technique was modified with a Co/Zn-ZIF@MIP composite, in which cobalt-zinc bimetallic ZIF (Co/Zn-ZIF) served as the support material. A linear relationship was observed between the frequency shift and citronellol concentrations ranging from 0.88 to 22 mg/L, with a sensitivity of –6.08 Hz/(mg·L) and a limit of detection (LOD) of 1.35 mg/L. This result indicated that this sensor has excellent selectivity for citronellol and demonstrates high repeatability, as evidenced by R² value of 0.97. In evaluations with real samples, the sensor reliably identified citronellol among the complex volatile organic compounds (VOCs) emitted from black spot-infected sweetpotato, indicating a high level of selectivity. Our research achieved the rapid characterization of sweetpotato black spot disease within 4 min and provided new insights into the development of QCM-based gas sensors for the rapid assessment of agricultural product quality and safety.

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SENSORS AND ACTUATORS B-CHEMICAL · 2025 · IF 7.7

Research on the coil-shaped element made of α-Fe2O3 doped MWCNTs for the simultaneous measurement of gas and gap at room temperature

Luheng Wang,Maoyuan Nan,Xisi Long

The coil-shaped element based on α-Fe 2 O 3 doped multi-walled carbon nanotubes (MWCNTs) is fabricated by sputtering and spraying technology for simultaneously measuring the gap and ethanol vapor at room temperature. The experimental results show that with the increase of spraying time, the gas response properties of MWCNTs-based coil-shaped elements change from p-type to n-type, while the gas response properties of the coil-shaped elements based on α-Fe 2 O 3 doped MWCNTs change from n-type to p-type with the increase of mass ratio of α-Fe 2 O 3 to MWCNTs. Particularly, the coil-shaped element with a mass ratio of 100 exhibits the highest gas response value and gap sensitivity in the gap range of 0–0.5 mm, the gas response value of impedance amplitude, impedance angle, and resistance is 0.659 %, 0.265 %, and 6.768 % at the ethanol vapor concentration of 5000 ppm, respectively. The absolute/relative gap sensitivity of impedance amplitude and impedance angle is 54,101.8 Ω·mm −1 /4.589 %·mm −1 and 2.069°·mm −1 / 5.287 %·mm −1 in the gap range of 0–0.1 mm, respectively. Finally, a signal processing method is proposed for the simultaneous measurement of ethanol vapor concentration and gap. These results lay a foundation for the development of MWCNTs-based sensors and the sensors applied between narrow gaps.

CAS / MDL: 1309-37-1
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GREEN CHEMISTRY · 2025 · IF 9.2

Highly efficient ruthenium catalytic system for the direct synthesis of butanol from propylene and CO2: a low temperature reverse water-gas shift route

Chenfei Yao,Boyu Zhu,Peng Zheng,Xingbang Hu

A catalytic system containing (Ru(CO)3Cl2)2, LiCl, ionic liquid and organic base was reported, which could effectively promote the following processes: low-temperature reverse water gas shift (RWGS) (at 100 oC), hydroformylation and hydrogenation of butyraldehyde to butanol, enabling the direct synthesis of butanol from propylene and CO2. The possible catalytic mechanism and the role of each additive were proposed based on the detection of reactive intermediates, control experiments and theoretic calculations. The critical step in this transformation is achieving RWGS at low temperatures without external reductants or dehydrating agents. Up to 99% conversion of propylene with 97% selectivity of butanol (n:i=1.4) was achieved, which represents the highest yield to date. Meanwhile, the catalytic system could maintain a certain degree of stability during recovery process. The results reported here may create a chance for the industrial application of the direct synthesis of butanol from propylene and CO2.

CAS / MDL: 121-44-8
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MICROCHEMICAL JOURNAL · 2025 · IF 5.1

Comprehensive characterization of chemical components in Wenjing decoction by offline two dimensional liquid chromatography-high resolution mass spectrometry and gas chromatography–mass spectrometry

Yan Sun,Jing Zhou,Yuxin Hu,Qingqing He,Yang Zhou,Xiaoyue Min,Zijia Zhang,Jinjun Hou,Huali Long,Wanying Wu,Dean Guo

Wenjing Decoction, a traditional Chinese medicine known for its blood-regulating effects, is primarily used to treat gynecological disorders in women. Despite its widespread clinical use, there remain gaps in the quality control of Wenjing Decoction, particularly in the comprehensive characterization of its volatile components, which are crucial to its therapeutic efficacy but often overlooked in conventional analyses. To address this issue and provide a more thorough chemical profile of Wenjing Decoction, we applied two complementary analytical methods: offline two-dimensional liquid chromatography coupled with high-resolution mass spectrometry (LC-HRMS) and gas chromatography–mass spectrometry (GC–MS). Using LC-HRMS, we successfully characterized 401 non-volatile compounds, which were classified into terpenoids, flavonoids, organic acids, phenylpropanoids, and lactones. GC–MS analysis identified 129 volatile components, including sesquiterpenoids, monoterpenoids, alcohols, and esters. These findings fill a critical gap in the systematic characterization of volatile components in Wenjing Decoction and provide a comprehensive chemical profiling approach for complex traditional Chinese medicine formulations. The results not only support the identification of potential quality control markers but also contribute to the standardization and quality assurance of Wenjing Decoction in clinical practice.

CAS / MDL: 631-61-8
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ENERGY & FUELS · 2025 · IF 5.3

Effect of the Oxygen Vacancy-Tunable Ce1–xGdxO2−δ Support on the Ni-Catalyzed CO2 Utilization via the Reverse Water–Gas Shift Reaction

Shuomei Wang,Nuo Cheng,Zhilin Jiang,Sicong Tian,Lujia Han

The reverse water–gas shift (RWGS) reaction offers a critical option for CO2 utilization, yet challenged by the endothermic nature of the reaction and high activation energy required for cleavage of the inert C═O bond. Oxygen vacancy engineering has been increasingly attractive as an effective strategy to activate CO2 via the electrostatic interaction. Herein, we develop a novel RWGS catalyst by dispersing metallic nickel on the gadolinia-doped ceria (GDC) support, where the oxygen vacancy concentration is tuned by varying the Gd/Ce molar ratio. The electron paramagnetic resonance (EPR), Raman, and X-ray photoelectron spectrometry (XPS) characterization of the Ni-GDC catalysts revealed that the oxygen vacancy concentration of the catalysts was increased with the increasing doping percent of Gd until 50%, and the interaction between metallic Ni and the GDC support kept strengthening as the Gd percent was increased. The developed Ni-GDC catalysts exhibited excellent activity and stability in driving the RWGS reaction, achieving a maximum CO yield of 19.4 mmol g–1 min–1 at 700 °C and retaining stable catalytic performance with no loss of activity throughout 20 h of the continuous test. It was found in this study that the CO2 conversion rate of the catalyst was positively correlated with its oxygen vacancy concentration, despite the observation that the oxygen vacancy concentration was less influential to CO2 conversion compared to temperature and the H2/CO2 feeding ratio.

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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2017 · IF 2.536

Vibrational spectroscopy of the mass-selected tetrahydrofurfuryl alcohol monomers and its dimers in gas phase using IR depletion and VUV single photon ionization

Pengchao Wang,Yongjun Hu,Huaqi Zhan,Jiaxin Chen,Shan Jin,Wentao Song,Yujian Li

Tetrahydrofurfuryl alcohol (THFA, C 5 H 10 O 2 ) is a close chemical analog of the sugar rings present in the phosphate-deoxyribose backbone structure of the nucleic acids . In present report, the infrared (IR) spectra of the size-selected THFA monomer and its dimer have been investigated in a pulsed supersonic jet using infrared-vacuum ultraviolet (VUV) ionization. Herein, the laser light at 118   nm wavelength served as the source of “soft” ionization in a time-of-flight mass spectrometer. The IR features for the monomers located at 3622   cm −   1 can be assigned to the intramolecular hydrogen bonding stretch vibrations mainly referring to A and C conformers . Compared with the monomer, however, characteristic peaks for the dimer centered at 3415 and 3453   cm −   1 , red shifted 207 and 169   cm −   1 , respectively, were associated with the intermolecular hydrogen bonding stretch vibrations. Combined with the quantum-chemical calculations, the dimer in the gas phase preferred cyclic AC conformer stabled by forming two strong intermolecular hydrogen bonds, which shown the high hydrogen bond selectivity in the cluster. The conclusions drawn from the role played in the conformational flexibility by the hydroxyl and ether groups may be extended to other biomolecules.

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JOURNAL OF COLLOID AND INTERFACE SCIENCE · 2024 · IF 9.4

Gas-specific adsorption capability of titanium dioxide and MXene nanocomposite thin films prepared by ultrasonic spray printing using inks oxidized at room temperature

Jinhong Liu,Chen Chen,Shenghui Xia,Hui Zhang,Ajit Khosla

The development of two-dimensional (2D) layered MXene materials has opened new possibilities for gas adsorption applications due to their high specific surface area, tunable surface chemistry, and excellent selectivity towards specific gases. These materials exhibit tremendous potential in adsorption-based gas separation and detection, particularly due to their strong interactions with target gas molecules, making them highly effective in gas removal and detection applications. However, currently available methods for synthesizing these oxidized nanocomposite inks are limited by the typically high temperatures involved. The present work addresses this issue by developing titanium dioxide and MXene (TiO 2 /Ti 3 C 2 MXene) nanocomposite inks, where TiO 2 nanoparticles are formed between the layers of the Ti 3 C 2 MXene via oxidation in solution state under extended exposure in an oxygen rich atmosphere at room temperature. As a proof of concept , gas adsorption studies are conducted by applying the TiO 2 /Ti 3 C 2 MXene nanocomposite inks onto gold-coated silicon wafers via an ultrasonic spray printing method. The gas adsorption results demonstrate that the TiO 2 /Ti 3 C 2 MXene nanocomposites possess excellent adsorption selectivity toward methane and butane among alkane gases, and can achieve maximum adsorption capacities of 8.62 and 18.8 cm 3 /g, respectively. The results of ultrasonic spray printing quality tests conducted for different numbers of printed layers using the proposed TiO 2 /Ti 3 C 2 MXene nanocomposite ink demonstrate that the film thickness can be regulated by controlling the number of printed layers, and the average thin film thickness remains only 0.313 μm for 10 printed layers. Meanwhile, the average roughness of the films resides between 0.130 μm (3 layers) and 0.220 μm (8 layers), which is uniformly and less than the average roughness of 0.225 μm measured for the original gold-plated silicon wafer. Hence, by employing facile ink-based printing techniques, such as ultrasonic spray printing, thin films with controlled thickness can be fabricated, thereby laying the foundation for their practical applications in environmental monitoring and industrial gas separation.

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ORGANIC PROCESS RESEARCH & DEVELOPMENT · 2025 · IF 3.5

Supramolecular Interaction-Mediated Diffusion Enhancement for Facilitated Synthesis of the Pharmaceutically Active Ingredient Dantrolene and Its Analogues via Spiral Gas–Solid Two-Phase Flow

Yong Song,Jinsong Li,Shikang Liu,Bo Jin,Rufang Peng

Although mechanochemical synthesis has gained widespread application, our understanding and enhancement of the control of the reaction need to be improved. In this work, we confirm that the mechanochemical reaction of the active pharmaceutical ingredient dantrolene is controlled by diffusion-controlled kinetics. On this basis, we demonstrate a novel approach to modulate mechanochemical reactivity through a diffusion enhancement strategy mediated by supramolecular interactions. The method employs a highly efficient spiral gas–solid two-phase flow technique, in which urea, an additive that can establish supramolecular interactions with 1-aminohydantoin hydrochloride, is introduced into the reaction system to substantially enhance diffusion, thus facilitating the efficient synthesis of dantrolene. Notably, in this diffusion enhancement process, the weakening of mechanical forces triggers the nucleation and growth of the active substrate to form structurally well-defined eutectic crystals that inhibit the reaction. This strategy reduces the mechanochemical reaction time of dantrolene and its analogs to less than 30 s. In addition, thiourea and acetamide, which are structurally similar to urea, promote the reaction, and their effects correlate with the number of supramolecular sites of action.

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DESALINATION · 2025 · IF 9.8

A novel blended adsorbent granule of crown ether polymer mixed with Mn-based lithium-ion sieves for efficient lithium recycling from shale gas wastewater

Xifan Li,Xin Li,Mingmei Zheng,Jialin Shi,Lu Yang,Yushun Yang,Guijing Chen,Shengchi Bai,Xiao Lin,Wen Liu,Baicang Liu

The transition in the global energy structure has significantly increased the demand for new energy resources, particularly lithium. To efficiently recover lithium from shale gas wastewater, this study developed an innovative blended adsorbent granule combining crown ether (CE) polymer backbones integrated with Mn-based lithium-ion sieve to maximize lithium adsorption sites. The CE-based adsorbent featured a porous, honeycomb-like interior structure and a high specific surface area of 15.20 m 2 /g, with Mn-based adsorbent uniformly dispersed within the CE polymer matrix. Lithium adsorption performance was systematically evaluated through adsorption isotherms, kinetics, selectivity and reusability tests. The CE-based adsorbent exhibited a lithium adsorption capacity of 17.04 mg/g, recovering over 82.7 % of lithium, with a partition coefficient reaching 1686.75 mL/g, outperforming the PVC-based counterpart. Moreover, the adsorbent showed excellent selectivity for lithium, with a Li/Na separation factor of 421.80. In fixed-bed adsorption-desorption experiments, the CE-based adsorbent processed shale gas wastewater volume up to 100 times its own bed volume, concentrating lithium ions by a factor of 5. To better understand the extraction mechanisms and selectivity, density functional theory calculations were conducted, including optimized structures, molecular orbitals, charge transfer and stabilization energy. Compared to Na + , the CE polymer preferential adsorbed Li + ion, which occupied the crown ether ring core, exhibited shorter O Li bond lengths, greater charge transfer and stabilization energy. This study provides a novel strategy for advancing lithium adsorption materials and presents promising potential for efficient lithium recovery from complex wastewater sources.

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Materials Today Nano · 2026 · IF 7.6

“Moisture-gas dual-effect”: Three-layer leaf-vein-inspired nanofiber filter membrane based on multi-gradient structure for personal protection in high-dust environments

Shuangying Li,Yueyuan Zhu,Jia Xu,Wenpeng Cui,Ren Li,Dong Wang,Meiyu Chen,Xinyuan Shi,Shaoxiang Li

Designed MC-loaded leaf-vein-inspired 3-layer gradient P224 membrane with multi-functions for high-dust protection. • Combined electrospinning with pore/wettability gradient to make filter with dust removal & moisture transport. • Achieved dual mechanism of efficient dust filtration and unidirectional moisture transport. • Enabled P224 use in high-dust environments, promoting next-gen personal respiratory protective equipment. Herein, we designed a facial nanofiber filter capable of efficiently adsorbing dust and achieving unidirectional water transport for moisture wicking (named P224). Multifunctional filtering fiber membrane loaded with Cu-MOF@MXene (MC) was successfully prepared via electrospinning, based on a three-layer leaf-vein-inspired multi-gradient structure. From inner to outer layers, P224 consists of PVDF@MC, PVDF/PVA, and PVA@MC. The decreasing fiber pore size gradient and the increasing wettability gradient enable it to have both mechanical filtration and single-stream water transport functions. The P224 fiber membrane prepared under the optimal ratio and spinning conditions has a filtration performance of up to 99.2% for PM0.3 (NaCl aerosol), an increased self-cleaning ability of approximately 150%, an antibacterial rate of 90% against Staphylococcus aureus . The test results of the unidirectional water transmission experiment and the water vapor transmission meter show that the water vapor transmission rate of this fiber membrane is 1542 g/(m 2 ·24h), and it has very good unidirectional water transmission capacity. This “moisture-gas dual-effect” nanofiber protective dust-filtering membrane paved the way for the design of personal protective equipment. We designed a three-layer leaf-vein-inspired nanofiber filter membrane (P224) via electrospinning, composed of inner PVDF@MC, middle PVDF/PVA, and outer PVA@MC. It has pore size and wettability gradients, enabling “moisture-gas dual-effect”. Optimized P224 shows 99.2% PM2.5 filtration efficiency, ∼150% enhanced self-cleaning, 90% antibacterial rate against Staphylococcus aureus , 1542 g/(m 2 ·24h) water vapor transmission rate, and good unidirectional water transport, laying a foundation for personal protective equipment. Download: Download high-res image (350KB) Download: Download full-size image

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