ANALYTICAL LETTERS
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2025
·
IF 1.8
Lin Yang,Guoqing Zou,Fengfeng Xiu,Dandan Zhao,Jianliang Fei,Jun Xie
Polycyclic aromatic hydrocarbons (PAHs) in soil pose significant analytical challenges due to matrix complexity, low concentrations, and co-extracted interferents. Conventional gas chromatography-mass spectrometry (GC-MS) methods suffer from limited sensitivity and selectivity, particularly for high-molecular-weight PAHs with stable molecular ions that resist fragmentation. Here, we present a novel gas chromatography-tandem mass spectrometry (GC-MS/MS) method using pseudo-multiple reaction monitoring (PMRM) coupled with an optimized extraction protocol for precise quantification of 16 USEPA priority PAHs in soil. By exploiting the inherent stability of PAH molecular ions ([M]+), PMRM achieved 3.1–4.8 times lower detection limits than traditional selected ion monitoring (SIM) while resolving critical isomer pairs (e.g., phenanthrene/anthracene, R > 1.5) through time-segmented collision energy (CE) optimization (5–25 eV). A streamlined extraction using acetonitrile modified with anhydrous Na2SO4 eliminated labor-intensive cleanup, achieving >85% recovery across a wide logKow range (3.37–6.50). The PMRM strategy enhanced signal-to-noise ratios by collisional focusing and differential interference fragmentation, enabling direct injection of crude extracts without compromising sensitivity. This approach addresses long-standing limitations in PAH analysis, offering a robust, high-throughput solution for environmental monitoring and regulatory compliance, with potential applications to other structurally stable pollutants.
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Materials Today Communications
·
2025
·
IF 4.5
Xiaochi Xu,Xinya Wang,Weiqiu Huang,Xufei Li,Xiaotong Li,Ping Xia,Jing Zhong
The persistent rise in global carbon emissions has driven a concurrent increase of CO₂ concentrations, escalating climate change impacts and exacerbating environmental crises. Among emerging decarbonization technologies, non-thermal membrane-based gas separation has emerged as a promising approach, where mixed matrix membranes (MMMs) demonstrate particular advantages through their structure-tunable frameworks and exceptional operational stability. Zirconium-based Metal-Organic Frameworks (Zr-MOFs) demonstrate exceptional potential as nanofillers in mixed matrix membranes (MMMs) due to their precise and tunable pore architectures and molecular screening properties. However, the presence of intercrystalline defects and inadequate interfacial adhesion between the selective layer and polymer matrix compromises membrane integrity and separation efficiency. So, we developed an innovative internal-external coupling strategy combined with multi-lock self-assembly, resulting in the successful fabrication of TA@PVDF-UIO membranes. In this work, the hydroxyl groups on the TA (Tannic Acid) surface can form a stable TA-Zr-MOF composite with Zr 4 + ions through coordination bonds, constituting the first "lock". Secondly, the oxidized functional groups of PDA can interact with zirconium-based MOF (Zr-MOF) through hydrogen bonds and π-π interactions, while Zr atoms may also coordinate with PDA, forming the second "lock". Finally, by utilizing the self-assembly of ZrCl 4 and NH 2 -BDC ligands at room temperature, the secondary growth of Zr-MOF is achieved on the membrane surface, creating the third "lock", which effectively compensates for the defects in the Zr-MOF-PDA layer. This approach demonstrates remarkable enhancement in both separation selectivity and operational stability. The TA@PVDF-UIO-4 membrane achieves exceptional CO 2 permeance of 12,394 GPU with optimal selectivities of 19.8 (CO 2 /N 2 ) and 17.6 (CO 2 /CH 4 ), exceeding the so-called "2019 upper bound for polymeric membranes". Remarkably, the membrane maintains stable performance under continuous operation, owing to the multi-lock interfacial engineering strategy that creates covalent-anchored and defect-free MOF-polymer interfaces. This innovative strategy provides a new idea for designing high-performance composite membranes and offers a new method for the design of next-generation gas separation technologies and advanced membrane materials.
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MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Jinyi Li,Zhixiong Kang,Zhongbo Li,Guangqing Cui
The global demand for Panax notoginseng powder has surged greatly because of its pharmacological efficacy. However, an escalation in adulteration practices has raised substantial concerns. We aimed to establish a headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS) method for detecting adulteration in P. notoginseng . Pure P. notoginseng powder was mixed with wheat flour, corn starch, and yellow dextrin at 10 %, 20 %, 40 %, 60 %, and 80 % ( w/w ). HS-GC-IMS showed minimal visual divergence between P. notoginseng powders adulterated with low levels of wheat flour (10 %, 20 %, and 40 %) and those with different ratios of cornstarch or yellow dextrin. Ninety-five volatile compounds were detected in the 19 samples, including aldehydes, alcohols, ketones, esters, acids, terpenes, heterocycles, nitrides, and sulfides. Principal component analysis based on the signal intensity of the volatile compounds effectively discriminated pure P. notoginseng from adulterated samples ( R 2 > 0.94, Q 2 > 0.91). Propanoic acid, acetic acid, methyl acetate, butyl acetate, ethyl acetate, 1-heptanol, 3-methyl-1-butanol, octanal, (E)-2-heptenal, pentanal, benzaldehyde, furfural, citronellal, 2-propenal, 2-decanone, acetone, 3-hydroxy-2-butanone, and pinene were identified as volatile markers for P. notoginseng authentication. Partial least squares discriminant analysis confirmed the reliability of the results ( R 2 of X-axis > 0.65, R 2 of Y-axis > 0.994, and Q 2 > 0.984). In conclusion, HS-GC-IMS is a valuable tool for the rapid, accurate, and simple determination of P. notoginseng adulteration.
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Bing Wang,Fuwei Xie,Mantang Chen,Pingping Shang,Lining Pan,Huapeng Cui,Yaqiong Qin,Li Zhang,Jizhao Guo,Xiaobing Zhang,Cong Nie,Xiaoyu Wang,Shaofeng Liu
Glycidol, 3-chloropropane-1,2-diol (3-MCPD), and 2-chloropropane-1,3-diol (2-MCPD), known as thermal processing contaminants, have been identified in heated tobacco product (HTP) aerosol, raising significant health concerns. Therefore, it is necessary to establish a quantitative analytical method for the release of them. In this study, ethyl acetate was used to extract the aerosol of HTP collected by Cambridge filter pad (CFP), the extract was derivatized with heptafluorobutyrylimidazole (HFBI), washed and dried before being analyzed by gas chromatography-mass spectrometry (GC-MS). The retention index and mass spectral characteristics of glycidol-HFBI derivative were characterized for the first time. The limits of quantification (LOQs) for glycidol, 3-MCPD and 2-MCPD were 58.32, 37.51 and 55.88 ng/cigarette respectively;the intra- and inter-day precision were less than 10% with recoveries ranging from 89% to 111%. The analysis results of eight domestic and foreign HTPs showed that: (1) The three target compounds were detected in all eight samples, indicating their widespread presence in HTP aerosol. (2) Significant variations in per-puff emission among samples suggested formulation and heating mode significantly impact glycidol and MCPDs release. (3) Glycidol and 3-MCPD were the major released substances, accounting for about 80% of the total three compounds emission. This study establishes a sensitive, reliable method for determining glycidol, 3-MCPD and 2-MCPD in HTP aerosol, providing critical technical support for health risk assessments.
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APPLIED CATALYSIS A-GENERAL
·
2025
·
IF 4.8
Kaihao Li,Yongwang Li,Yang Qin,Zheng Wang,Bingxin Zhu,Yancong Yin,Fumin Wang,Xubin Zhang
The production of high-purity hydrogen chloride from petrochemical by-product hydrogen chloride gas represents the primary industrial approach for manufacturing electronic-grade hydrogen chloride. However, trace acetylene and ethylene impurities in the feedstock severely compromise product quality. This study innovatively proposes a "stepwise conversion-deep chlorination" synergistic mechanism and successfully develops a bimetallic catalyst (10 %Fe/0.5 %Pd/AC). By tailoring the preparation processes, we precisely controlled the distribution of Fe and Pd active sites, while systematically comparing the performance between Single-metal tandem catalytic system (Pd/AC + Fe/AC) and the bimetallic catalyst. Experimental results combined with DFT calculations demonstrate the superior performance of the 10 %Fe/0.5 %Pd/AC catalyst and confirm the cascade reaction mechanism based on the synergistic tandem effect of Fe/Pd active sites: Acetylene preferentially undergoes hydrochlorination at Pd sites to form vinyl chloride, while ethylene and the resultant vinyl chloride are subsequently converted to chloroethane and more easily removable 1,1-dichloroethane at Fe sites. Under optimized conditions (120 °C, GHSV=180 h −1 ), removal efficiencies exceeding 99 % for both acetylene and ethylene were achieved, with 1,1-dichloroethane selectivity surpassing 99 %. Comprehensive characterizations demonstrated the outstanding stability of the 10 %Fe/0.5 %Pd/AC catalyst. This study presents an innovative catalytic approach for high-efficiency purification of industrial hydrogen chloride.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2018
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IF 2.831
Meilian Wang,Sheng Fang,Xianrui Liang
Reported here is a simple and rapid static headspace gas chromatography (SHS-GC) method for the determination of trace solvents including ethanol, isopropanol, n -butanol, 1,4-dioxane, tetrahydrofuran, acetonitrile, methanol and acetone which commonly used in drug production process. Natural deep eutectic solvents (NADESs) are firstly used as the matrix medium for this method, which provided high sensitivity for residual solvents detection. With the optimized method, validation experiments were performed and the data showed excellent linearity for all the solvents ( R 2 ≥ 0.999, n = 7). The limits of detection (LOD) for ethanol, isopropanol, n -butanol, 1,4-dioxane, tetrahydrofuran, acetonitrile, methanol and acetone are 0.09, 0.08, 0.07, 0.11, 0.06, 0.10, 0.12 and 0.08 μg g −1 , respectively. Accuracy was checked by a recovery experiment at three different levels, and the recoveries of the tested solvents were ranged from 94.3% to 105.4%. The relative standard deviation (RSD) of each solvent for intra- and inter-day precision is in the range of 0.85 to 3.65 and 1.51 to 4.53, respectively. The developed approach can be readily used for determination of the residual solvents in six active pharmaceutical ingredients including pramipexole dihydrochloride, rivaroxaban, lisinopril, ramipril, imatinib mesylate and sitagliptin.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2018
·Vol. 411
·期 3
·787-795
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IF 3.307
Zhang Hua-Yin,Tan Xiao-Xin,Kang Kai,Wang Wei,Lian Kao-Qi,Kang Wei-Jun
Lactic acid and pyruvic acid are important metabolites in the tricarboxylic acid cycle that can reflect the cytoplasmic redox state and mitochondrial respiratory chain function. The combination of these acids is considered as a screening index for mitochondrial disorders. Due to their biological effects, a derivatization method was developed to simultaneously detect pyruvic acid and lactic acid in tissue and cell culture media using gas chromatography. In this work, the combined derivatization method with methoxyamine hydrochloride and isobutyl chloroformate was first proposed. To improve the efficiency of derivatization, in situ derivatization-ultrasound-assisted emulsification microextraction (USAEME) was used in this study. After optimizing the volume of reagents and reaction times, good linearity values were obtained from 50 to 1000 μmol/L and 1 to 100 μmol/L for lactic acid and pyruvic acid, respectively. The limits of detection (LODs) were 0.12 μmol/L for lactic acid and 0.29 μmol/L for pyruvic acid. The recoveries of the two analytes were between 93.60 and 102.80%, and the precisions were less than 6.20%. This method was successfully applied to quantify pyruvic acid and lactic acid in the animal and cellular hypoxia models which provided an auxiliary means for the diagnosis of mitochondrial diseases.
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ENERGY & FUELS
·
2022
·
IF 4.654
Xue-Lei Duan,Yuan-Ming Cao,Chong Gao,Sheng-Li Niu,Yi-Wen Shen,Qi Guo,Jiao-Jiao Xie,Kai-Qiang He,Chun-Gang Yuan
One novel/multifunctional selenium-doped SrFeO3-δ/HNTs composite was fabricated and used for immobilization of gaseous mercury. The composite showed excellent performances for Hg0 removal via adsorption coupled with photocatalytic oxidation in visible-light conditions. The adsorption capacity of 4271.15 μg·g–1, rate of 5.0 μg·g–1·min–1, and removal efficiency of ∼100% were obtained under N2+O2, which was further confirmed by reaction kinetics. SrFeO3-δ was selenized into iron diselenide and a Se–Fe bond with high affinity toward Hg0. In addition, the yielding of •O2– and the separation of photoexcited electrons and holes (h+) promoted the photocatalytic oxidation of mercury. The composite with intrinsic magnetism could be easily recycled for reuse by magnetic separation. Moreover, the composite possessed favorable tolerance to the complicated flue gas. An online lab-built thermal decomposition system demonstrated that the immobilized Hg was primarily HgSe, which exhibited very high stability and low toxicity. Density functional theory (DFT) calculations proved that the composite was half metal with magnetism, indicating that Hg on Se-SrFeO3-δ/HNTs formed the stable structure releasing 1.055 eV. The doping of selenium promoted the charge transfer between O (2p) and Hg (6s), which also favored Hg0 removal. Se-SrFeO3-δ/HNTs with recyclability possess great potentials for Hg0 efficient removal and immobilization/detoxification from flue gas.
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SENSORS AND ACTUATORS B-CHEMICAL
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2022
·
IF 9.221
Liupeng Zhao,Yiwen Li,Yue Zhou,Tianshuang Wang,Peng Sun,Fangmeng Liu,Chenguang Wang,Xu Yan,Nianke Chen,Geyu Lu
The effect of high- and low-valence doping on adsorbed oxygen has been studied and intensely discussed for decades, in which the high-valence dopant can provide more electrons for ionosorbed oxygen species while low-valence dopant can provide more adsorption sites. In this work, this effect is observed directly by Quasi in-situ X-ray photoelectron spectroscopy and CO temperature-programmed reduction, and rationalized by density functional theory calculations. It is found that the oxygen vacancies can be easier to generate on Co-doped SnO 2 surface, but the decrease in surface electron concentration actually reduces the amount of adsorbed oxygen at working temperature while Sb-doped SnO 2 is more conducive to oxygen adsorption but the enormous electron concentration makes the resistance variation caused by the surface reactions insignificant. In order to combine the advantages of both dopants, Sb-doped SnO 2 @Co-doped SnO 2 core-shell structure are designed and prepared. The synergism of the core and shell can enhance sensing reactions on the surface while efficiently converting the surface reactions into a resistance change. On the one hand, the electron diffusion from the electron-rich core to the shell provides the electrons required for oxygen adsorption, which ensures sufficient surface reactions. On the other hand, a potential barrier is formed between the core and shell which can regulate electron transport between adjacent cores, thereby effectively converting the surface reaction into a resistance change.
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ACS Catalysis
·
2022
·
IF 13.7
Xiao-Chen Sun,Kun Yuan,Wang-De Hua,Zi-Rui Gao,Qian Zhang,Chen-Yue Yuan,Hai-Chao Liu,Ya-Wen Zhang
The metal–support interface plays a crucial role in heterogeneous catalysis. The modulation of the metal–support interaction (MSI) affords the possibility of promoting the catalytic efficiency per active site. Here, we report a strategy to modulate the interfacial interaction and then optimize the interfacial activity of Co/CeO2 catalysts for the water–gas shift reaction (WGSR) by a facile NH3 treatment process for the CeO2 support. The sample of Co/800N-CeO2 treated at 800 °C exhibited the highest reaction rate of 260 μmolCO/(gCo s), which was 23.8 times higher than the rate of the untreated Co/CeO2 sample. A combination of ex situ and in situ characterizations suggested that addition of the NH3 treatment process did not only weaken the metal–support interaction between the Co species and CeO2 support to strengthen CO adsorption and CO activation ability but also induced oxygen vacancy generation under reaction conditions to accelerate H2O activation. Both worked together in promoting the catalytic efficiency for the WGSR via the carboxyl pathway at a low temperature. It was worth mentioning that the N species of the CeO2 support introduced by the NH3 treatment was removed after changing the catalyst structure under reaction conditions. The interfacial structure was robust in a 60 h test at 400 °C due to the coexistence mechanism of carboxyl and formate pathways avoiding the poisoning effect of formate species on the active sites. The construction of active interfaces could be extended to Fe/CeO2 and Ni/CeO2 catalysts and could bring great promise in the design of the interfacial structure of supported catalysts in wide applications including chemical transformation reactions and industrial catalysis.
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TALANTA
·
2013
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IF 3.498
Suling Zhang,Zhuo Du,Gongke Li
The hybrid material of a copper-based metal-organic framework (MOF-199) and graphite oxide (GO) was explored as the solid-phase microextraction (SPME) coating for the first time. This fiber was fabricated by using 3-amino-propyltriethoxysilane (APTES) as the cross-linking agent, which enhanced its durability and allowed more than 140 replicate extractions. With the incorporation of GO, the MOF-199/GO fibers with GO contents ranging from 5 to 15 wt% exhibited enhanced adsorption affinity to organochlorine pesticides (OCPs) compared to MOF or GO individually. This improvement was linked to the enhanced dispersive forces (increased volume of small pores) that provided by the dense carbon layers of GO. Combining the superior properties of high porosity of MOFs and the unique layered character of GO, the MOF-199/GO (10 wt%) fiber exhibited higher adsorption affinity to some OCPs than commercial polydimethylsiloxane (PDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibers. This new fiber was developed for headspace (HS) SPME of eight OCPs followed by GC/ECD analysis. The limits of detection were 2.3–6.9 ng/L. The relative standard deviation (RSD) for five replicate extractions using one fiber ranged from 5.3% to 8.8%. The fiber-to-fiber reproducibility was 5.2–12.8%. This method was successfully used for simultaneous determination of eight OCPs from river water, soil, water convolvulus and longan with satisfactory recoveries of 90.6–104.4%, 82.7–96.8%, 72.2–107.7% and 82.8–94.3%, respectively. These results indicated the MOF-199/GO composite provided a promising alternative in sample pretreatment.
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ANALYTICA CHIMICA ACTA
·
2016
·
IF 4.712
Lulu Li,Mian Wu,Yingying Feng,Faqiong Zhao,Baizhao Zeng
In this work, ionic liquid (IL, i.e. 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate), carboxyl multiwall carbon nanotubes (MWCNTs) and reduced graphene oxide (rGO) were used to prepare three-dimensional porous material (MWCNTs-rGO-IL) by one-step self-assembly, then it was co-electrodeposited with polyaniline (PANI) on stainless steel wires by cyclic voltammetry . The resulting coating (PANI-MWCNTs-rGO-IL) was characterized by using FT-IR and scanning electron microscopy etc, and it showed porous structure and had high thermal stability . Furthermore, it was found to be very suitable for the headspace solid-phase microextraction of alcohols (i.e. octanol , nonanol, geraniol , decanol, undecanol and dodecanol). By coupling with gas chromatography , wide linear ranges and low limits of detection (i.e. 2.2–28.3 ng L −1 ) were obtained for the alcohols. The coating also presented good repeatability and reproducibility; the relative standard deviations for intra-fiber and fiber-to-fiber were less than 5.6% (n = 5) and 7.0% (n = 5) respectively. In addition, the proposed method was successfully applied to the determination of alcohols in tea drinks, and the recoveries for standards added were 85.6–114%.
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危险品化学品经营许可证（带存储）