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ANALYTICAL LETTERS · 2016 · IF 1.088

Electro-Filtering Spray Ionization Source for Soil Analysis

Yinjuan Chen,Chongsheng Xu,Fuxing Xu,Kai Yang,Qiang Wang,Xin Zhao,Yuanyuan Wang,Bin Chen,Chuan-Fan Ding

An electro-filtering spray ionization source for ambient mass spectrometry is reported. The ion source was assembled with a conical metal filter with a paper cone. The performance of the new ion source was characterized by the analysis of soil. Soil was directly introduced into the filter-paper cone and solvent was added. Ions were produced at the filter-paper tip when a high voltage was applied. The results by electro-filtering spray ionization were in good agreement with the results using conventional electrospray ionization with complex sample preparation. Advantages of electro-filtering spray ionization include simplicity, speed, and convenient operation that may allow in situ analysis in ambient atmospheric conditions.

CAS / MDL: 50-55-5 9007-43-6
研究领域: 分析化学 · 环境科学
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NEW JOURNAL OF CHEMISTRY · 2023 ·Vol. 47 ·期 29 ·13985-13992 · IF 3.3

One-pot synthesis of polymer SiO2-PNPG electrodes as a transducer for the measurement of Pb(II) in soil

Luo Xu,Fang Yang,Jiagen Li,Qihui Wang,Lin Du,Min Yang,Xiaohong Fu

In this work, an electrochemical sensor based on a highly efficient competitive method is proposed that uses SiO2-PNPG as an adsorbent for the efficient detection of Pb(II) in soil. The silica (SiO2) and N-phenylglycine (NPG) polymer (SiO2-PNPG), synthesized using a one-pot polymer method, was applied to construct specific metal electrochemical sensors with high sensitivity. The high sensitivity and good selectivity were accomplished in the determination of Pb(II) due to the selective penetration and accumulative effect of SiO2-PNPG. The correlation between the current response and the Pb(II) concentration presents a linear range from 2.12 to 15.78 μg mL−1 with a detection limit of 0.166 μg mL−1 (S/N = 3, R2 = 0.9987). The sensitivity, reproducibility and stability of this sensor are promoted due to the facilitated electron transfer.

研究领域: 环境科学 · 材料科学
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MICROCHIMICA ACTA · 2015 ·Vol. 182 ·期 13 ·2353-2359 · IF 3.741

Porous carbon derived from aluminum-based metal organic framework as a fiber coating for the solid-phase microextraction of polycyclic aromatic hydrocarbons from water and soil

Zhang Xi,Zang Xiao Huan,Wang Jun Tao,Wang Chun,Wu Qiu Hua,Wang Zhi

A nanoporous carbon derived from an aluminum-based metal-organic framework was deposited on stainless steel wires in a sol–gel matrix. The resulting fibers were applied to the solid-phase microextraction of the polycyclic aromatic hydrocarbons (PAHs) naphthalene, acenaphthene, fluorene, phenanthrene and anthracene from water and soil samples. The fiber was then directly inserted into the GC injector and the PAHs were quantified by GC-MS. The effects of salt addition, extraction temperature, extraction time, sample volume and desorption conditions on the extraction efficiency were optimized. A linear response to the analytes was observed in the 0.1 to 12 μg∙L −1 range for water samples, and in the 0.6 to 30 μg∙kg −1 for soil samples, with the correlation coefficients ranging from 0.9934 to 0.9985. The limits of detection ranged from 5.0 to 20 ng∙L −1 for water samples, and from 30 to 90 ng∙kg −1 for soil samples. The recoveries of spiked samples were between 72.4 and 108.0 %, and the precision, expressed as the relative standard deviations, is <12.8 %. A MOF derived nanoporous carbon coated fiber for use in solid-phase microextraction was prepared via sol–gel technology. The coated fiber has a porous, rough and wrinkled structure, and shows a high thermal stability, good extraction repeatability and long lifetime. The established HS-SPME-GC-MS method is suitable for the determination of the PAHs from water and soil samples.

研究领域: 分析化学 · 环境科学
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NEW JOURNAL OF CHEMISTRY · 2020 ·Vol. 44 ·期 19 ·7727-7739 · IF 3.288

Magnetic solid phase extraction using Fe3O4@β-cyclodextrin–lipid bilayers as adsorbents followed by GC-QTOF-MS for the analysis of nine pesticides

Hui Wang,Shaowei Yan,Bo Qu,He Liu,Jie Ding,Nanqi Ren

A rapid and efficient magnetic solid phase extraction (MSPE) method, based on Fe3O4@β-cyclodextrin–lipid bilayer nanocomposites (Fe3O4@β-CD–LB), was built. The MSPE method coupled with GC-QTOF-MS has been designed for the trace detection of nine organochlorine pesticides (OCPs) in soil samples. The Fe3O4@β-CD–LB was successfully synthesized and characterized by vibrating sample magnetometry, Fourier transform infrared spectrometry, transmission electron microscopy, field emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. In this experiment, the OCPs in the soil samples were firstly extracted with n-hexane/dichloromethane (v/v 1 : 1) at high pressure and temperature, and then subjected to MSPE for adsorption and purification. Considering the synergy effect between host–guest inclusion complexation and hydrophobic interaction in the adsorption mechanism, the bi-functionalized magnetic nanocomposites exhibited excellent adsorption properties for the OCPs and natural resistance to interference by macromolecules. Under the optimum experimental conditions, the method showed wide linear ranges with low limits of detection (4.5 to 34 pg g−1). The results showed that the mean recoveries of the OCPs in the soil samples were 78–107% with 3.0–6.1% intra-day relative standard deviation (RSD) and 3.5–6.9% inter-day RSD. The method has been applied for the determination of the OCPs in actual samples, and ΣOCPs ranged between 0 and 2.3 ng g−1 in seven soil samples.

研究领域: 分析化学 · 环境科学
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ANALYTICAL LETTERS · 2025 · IF 1.8

Improved Detection Limits for Polycyclic Aromatic Hydrocarbons (PAHs) in Soil and Sediments by Gas Chromatography-Mass Spectrometry (GC-MS) and Pseudo-Multiple Reaction Monitoring (PMRM)

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.

研究领域: 环境化学 · 分析化学 · 质谱学 · 环境科学 · 色谱学
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