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INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH · 2023 · IF 4.2

Continuous Counter-Current Multistage Microextraction in a Novel Tube-In-Tube Microextractor

Junxin Chen,Caijin Zhou,Bingqi Xie,Jisong Zhang

Counter-current operation has been widely applied to enhance the extraction efficiency for systems with low distribution coefficients, which was hindered in microextraction because viscous force and surface tension dominate over gravity and inertial force. In this study, a novel design of a tube-in-tube microextractor relying on a poly tetra fluoroethylene membrane to construct a stable interface was proposed to conduct continuous counter-current extraction. Extraction kinetics for two systems with different distribution coefficients, membranes with different pore radii, and three flow rate ratios were measured as a function of residence time. For the system that toluene was used to extract 0.06 wt % phenol in water, 4.1 stages of extraction efficiency were achieved at a residence time of 9.8 min. A challenging case study (50 wt % acetone–water–toluene) was subsequently conducted to prove the high applicability for emulsion systems of this special microextractor. Lastly, a mathematical model was established and the predicted results of three flow rate ratios are in good agreement with experimental results.

CAS / MDL: 108-95-2
研究领域: 化学工程 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2012 · IF 4.531

Dispersive microextraction based on water-coated Fe3O4 followed by gas chromatography–mass spectrometry for determination of 3-monochloropropane-1,2-diol in edible oils

Qin Zhao,Fang Wei,Neng Xiao,Qiong-Wei Yu,Bi-Feng Yuan,Yu-Qi Feng

In the present work, we developed a novel dispersive microextraction technique by combining the advantages of liquid-phase microextraction (LPME) and magnetic solid-phase extraction (MSPE). In this method, trace amount of water directly absorbed on bare Fe 3 O 4 to form water-coated Fe 3 O 4 (W-Fe 3 O 4 ) and rapid extraction can be achieved while W-Fe 3 O 4 dispersed in the sample solution. The analyte adsorbed W-Fe 3 O 4 can be easily collected and isolated from sample solution by application of a magnet. It was worth noting that in the proposed method water was used as extractant and Fe 3 O 4 served as the supporter and retriever of water. The performance of the method was evaluated by extraction of 3-monochloropropane-1,2-diol (3-MCPD) from edible oils. The extracted 3-MCPD was then derived by a silylanization reagent (1-trimethylsilylimidazole) before gas chromatography–mass spectrometry (GC–MS) analysis. Several parameters that affected the extraction and derivatization efficiency were investigated. Our results showed that the limit of detection for 3-MCPD was 1.1   ng/g. The recoveries in spiked oil samples were in the range of 70.0–104.9% with the RSDs less than 5.6% (intra-day) and 6.4% (inter-day). Taken together, the simple, rapid and cost-effective method developed in current study, offers a potential application for the extraction and preconcentration of hydrophilic analytes from complex fatty samples.

研究领域: 分析化学 · 食品科学
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International Journal of Environmental Research and Public Health · 2023 ·Vol. 20 ·期 2 ·1393 · IF 4.614

The Preparation of Covalent Bonding COF-TpBD Coating in Arrayed Nanopores of Stainless Steel Fiber for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons in Water

Zihan Li,Mengqi Yang,Xuetong Shen,Hongtao Zhu,Baohui Li

Covalent organic framework (COF)-TpBD was grafted on the arrayed nanopores of stainless steel fiber (SSF) with (3-aminopropyl) triethoxysilane as the cross-linking agent. The prepared SSF bonded with COF-TpBD showed high thermal and chemical stability and excellent repeatability. The prepared SSF bonded with COF-TpBD was also used for the solid-phase microextraction (SPME) of seven kinds of polycyclic aromatic hydrocarbons (PAHs) in actual water samples, followed by gas chromatography with flame ionization detection (GC-FID) determination, which exhibited low limits of detection (LODs), good relative standard deviation (RSD) and high recoveries.Keywords:solid-phase microextraction;COF-TpBD;polycyclic aromatic hydrocarbons

研究领域: 分析化学 · 环境科学
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 43 ·期 5 ·896-904 · IF 2.516

Layer-by-layer self-assembly of a novel covalent organic frameworks microextraction coating for analyzing polycyclic aromatic hydrocarbons from aqueous solutions via gas chromatography

Yuan Tian,Yuxia Hou,Quan Yu,Xiaohao Wang,Mengkui Tian

In this study, a new covalent organic framework, consisting of tetra(4-aminophenyl)porphyrin and tris(4-formyl phenyl)amine, was layer-by-layer immobilized on stainless-steel wire as a coating for microextraction. The fabrication process was easy and controllable under mild conditions. The as-grown fiber was applied to extract polycyclic aromatic hydrocarbons in aqueous solution via head-space solid-phase microextraction. Furthermore, it was analyzed by gas chromatography with a flame ionization detector. A wide linear range (0.1–50 µg/L), low limits of detection (0.006–0.024 µg/L, signal-to-noise ratio = 3), good repeatability (intra-fiber, n = 6, 3.1–8.50%), and reproducibility (fiber to fiber; n = 3, 5.79–9.98%), expressed as relative standard deviations, demonstrate the applicability of the newly developed coating. This new material was successfully utilized in real sample extraction with a satisfactory result. Potential parameters affecting the extraction efficiency, including extraction temperature and extraction time, salt concentration, agitation speed, sample volume, desorption temperature, and time, were also optimized and discussed.

研究领域: 分析化学 · 环境科学 · 材料科学
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Nature Sustainability · 2024 · IF 25.7

Direct and efficient in situ rubidium extraction from potassium chloride salts

Chen Xulong,Hu Wenping

Rubidium (Rb) is a valuable rare alkali metal that plays a crucial role in various high-tech applications, but extracting Rb from conventional sources poses sustainability challenges. A considerable amount of Rb is found in potassium chloride (KCl) salts, which can serve as a sustainable source depending on the extraction methods. Current liquid-phase methods are problematic due to the low Rb/K separation factor and high consumption of energy, water and chemicals. Extracting Rb directly from solid KCl salts is a promising approach, but achieving efficient recovery remains a challenge. Here we propose a crystal ripening microextraction strategy that enables in situ extraction of Rb from solid KCl salts with high selectivity, simplicity and high efficiency. By applying this strategy, we recovered 92.37% of Rb from KCl salts with an initial Rb content of 113 ppm. Compared with liquid-phase extraction, our approach results in a 97.57% reduction in energy consumption, a 22.24% increase in recovery efficiency and a 13.46-fold higher Rb/K separation factor, which substantially enhance environmental and economic benefits. In addition, this approach is suitable for recovering other target metals needed for various industrial applications directly from different solid metallic salts, providing a pathway to improve the sustainability of critical metal supply.

CAS / MDL: 7447-40-7 7791-11-9
研究领域: 化学工程 · 环境科学 · 材料科学
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ENVIRONMENTAL SCIENCE & TECHNOLOGY · 2016 · IF 5.393

Ultrasensitive Speciation Analysis of Mercury in Rice by Headspace Solid Phase Microextraction Using Porous Carbons and Gas Chromatography-Dielectric Barrier Discharge Optical Emission Spectrometry

Yao Lin,Yuan Yang,Yuxuan Li,Lu Yang,Xiandeng Hou,Xinbin Feng,Chengbin Zheng

Rice consumption is a primary pathway for human methylmercury (MeHg) exposure in inland mercury mining areas of Asia. In addition, the use of iodomethane, a common fumigant that significantly accelerates the methylation of mercury in soil under sunlight, could increase the MeHg exposure from rice. Conventional hyphenated techniques used for mercury speciation analysis are usually too costly for most developing countries. Consequently, there is an increased interest in the development of sensitive and inexpensive methods for the speciation of mercury in rice. In this work, gas chromatography (GC) coupled to dielectric barrier discharge optical emission spectrometry (DBD-OES) was developed for the speciation analysis of mercury in rice. Prior to GC-DBD-OES analysis, mercury species were derivatized to their volatile species with NaBPh4 and preconcentrated by headspace solid phase microextraction using porous carbons. Limits of detection of 0.5 μg kg–1 (0.16 ng), 0.75 μg kg–1 (0.24 ng), and 1.0 μg kg–1 (0.34 ng) were obtained for Hg2+, CH3Hg+, and CH3CH2Hg+, respectively, with relative standard deviations (RSDs) better than 5.2% and 6.8% for one fiber or fiber-to-fiber mode, respectively. Recoveries of 90–105% were obtained for the rice samples, demonstrating the applicability of the proposed technique. Owing to the small size, low power, and low gas consumption of DBD-OES as well as efficient extraction of mercury species by porous carbons headspace solid phase micro-extraction, the proposed technique provides several advantages including compactness, cost-effectiveness, and potential to couple with miniature GC to accomplish the field speciation of mercury in rice compared to conventional hyphenated techniques.

研究领域: 环境科学 · 分析化学
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FOOD CHEMISTRY · 2018 · IF 4.946

Ferrofluid-based liquid-phase microextraction: Analysis of four phenolic compounds in milks and fruit juices

Dezhi Yang,Guixiang Li,Lan Wu,Yaling Yang

A novel liquid-phase microextraction based on the ferrofluid was successfully applied for the extraction and determination of four phenolic compounds (bisphenol-A, bisphenol-AF, tetrabromobisphenol-A and 4-tert-octylphenol) in milks and fruit juices. In this study, a range of alkyl (C 4 –C 10 ) alcohols as the carrier liquid were used for the preparation of ferrofluids. The study showed that an appropriate chain length of alkyl alcohol may improve the extraction efficiency and maintain the integrity of ferrofluids during extraction, so 1-heptanol (C 7 ) was selected as the optimal carrier liquid. Specifically, the effects of various parameters on the extraction of phenolic compounds were investigated and optimized. Under the optimized conditions, the limits of detection were between 0.35 and 0.66 μg L −1 . The intra-day and inter-day precision (RSD %) for the analytes at 10 and 50 μg L −1 were in the range of 3.2–6.7 % and 2.9–7.1%, respectively.

研究领域: 分析化学 · 环境科学
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Food Analytical Methods · 2021 ·Vol. 14 ·期 7 ·1464-1471 · IF 3.366

Preparation and application of lysozyme aptamer fibre for specific recognition of lysozyme in food samples

Zhang Qianchun,Chen Junyu,Wang Yutong,Xia Guangping,Zheng Yuguo,Wang Xingyi,Wu Yun,Zhang Changbo

A novel aptamer solid-phase microextraction (SPME) fibre-based on poly (methacrylic acid-co-ethylene glycol dimethacrylate) for lysozyme-specific recognition has been successfully prepared. The prepared SPME fibres were characterised by various instrumental methods, including scanning electron microscopy, X-ray photoelectron spectroscopy and Fourier-transform infrared spectrometry. The results showed that the SPME fibre exhibited a porous structure, which is beneficial for the enrichment of the aptamer. The solid-phase microextraction-high-performance liquid chromatography-fluorescence detection (SPME-HPLC-FLD) with the superior selectivity and sensitivity responded linearly to the concentration of lysozyme over the 0.025–10 mg/L range, and the limit of detection was low at 6.8 μg/L, with a linearity of 0.9995. The method showed excellent reproducibility, and the relative standard deviations (RSDs) were less than 5.5%, which facilitated the analysis. The method was applied for the analysis of lysozyme in cow milk and papaya samples, and the recoveries ranged from 86.7–93.5% with RSDs of 4.3–6.1%, which clearly state that the proposed lysozyme aptamer SPME-HPLC-FLD method is a promising analytical tool for the analysis of lysozyme in food samples. Graphical abstract

研究领域: 分析化学 · 食品科学
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JOURNAL OF SEPARATION SCIENCE · 2017 ·Vol. 41 ·期 7 ·1635-1643 · IF 2.557

Air-assisted dispersive liquid–liquid microextraction based on a new hydrophobic deep eutectic solvent for the preconcentration of benzophenone-type UV filters from aqueous samples

Dandan Ge,Yi Zhang,Yixiu Dai,Shumin Yang

Deep eutectic solvents are considered as new and green solvents that can be widely used in analytical chemistry such as microextraction. In the present work, a new dl- menthol-based hydrophobic deep eutectic solvent was synthesized and used as extraction solvents in an air-assisted dispersive liquid–liquid microextraction method for preconcentration and extraction of benzophenone-type UV filters from aqueous samples followed by high-performance liquid chromatography with diode array detection. In an experiment, the deep eutectic solvent formed by dl- menthol and decanoic acid was added to an aqueous solution containing the UV filters, and then the mixture was sucked up and injected five times by using a glass syringe, and a cloudy state was achieved. After extraction, the solution was centrifuged and the upper phase was subjected to high-performance liquid chromatography for analysis. Various parameters such as the type and volume of the deep eutectic solvent, number of pulling, and pushing cycles, solution pH and salt concentration were investigated and optimized. Under the optimum conditions, the developed method exhibited low limits of detection and limits of quantitation, good linearity, and precision. Finally, the proposed method was successfully applied to determine the benzophenone-type filters in environmental water samples with relative recoveries of 88.8–105.9%.

研究领域: 分析化学 · 环境科学
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JOURNAL OF CHROMATOGRAPHY A · 2022 · IF 4.601

Superficially capped amino metal-organic framework for efficient solid-phase microextraction of perfluorinated alkyl substances

Sai Ouyang,Guifeng Liu,Sheng Peng,Jiating Zheng,Yu-Xin Ye,Juan Zheng,Yuanjun Tong,Yalan Hu,Ningbo Zhou,Xinying Gong,Jianqiao Xu,Gangfeng Ouyang

Perfluorinated alkyl substances (PFASs) were ubiquitously in the surface and groundwater. It is crucial and urgent to develop a rapid and ultrasensitive analysis method for the quantification of trace-level PFASs. Herein, a highly hydrophobic sorbent by capping phenylsilane groups on the surfaces of NH 2 -UiO-66(Zr) nanocrystals was used for efficient solid-phase microextraction (SPME) of PFASs in water samples. It was found that the superficially capped nanocrystals (NH 2 -UiO-66(Zr)-hp) exhibited both faster extraction kinetics and higher enrichment capacity than the non-capped nanocrystals. The extraction of eleven kinds of PFASs by NH 2 -UiO-66(Zr)-hp fiber reached equilibrium in 20 min. The enrichment factors of the NH 2 -UiO-66(Zr)-hp fiber ranged from 6.5 to 48, with a preference for long-chain PFASs over short-chain PFASs. It was proposed that superficial capping eliminated competitive moisture adsorption on the surfaces of the non-capped nanocrystals, thus facilitating the adsorption of PFASs through hydrophobic interaction. By using this new sorbent, the limits of detection of the SPME method as low as 0.035 to 0.616 ng·L −1 were achieved for the target PFASs. The recoveries of PFASs in the environmental water samples were 80.9%-120%. This study presents a new strategy for developing an efficient sorbent for PFASs by surface hydrophobic modification.

研究领域: 环境科学 · 分析化学
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RSC Advances · 2021 ·Vol. 11 ·期 48 ·30102-30108 · IF 3.361

Novel hydrophobic deep eutectic solvent for vortex-assisted liquid phase microextraction of common acaricides in fruit juice followed by HPLC-UV determination

Setareh Rostami-Javanroudi,Masoud Moradi,Kiomars Sharafi,Nazir Fattahi

In the present research, several novel and natural hydrophobic deep eutectic solvents (DESs) were prepared using methyltrioctylammonium chloride (MTOAC) as the hydrogen bond acceptor (HBA) and different types of straight chain alcohols as hydrogen bond donors (HBDs). One of the DESs composed of MTOAC and n-butanol was advantageously used to develop a vortex-assisted liquid phase microextraction (VALPME) method combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for the determination of common acaricides in fruit juice samples. Several important parameters influencing extraction efficiency were investigated and optimized, including the type and volume of DES, sample solution pH, effect of salt addition and, extraction and vortex time. Under optimal experimental conditions, the method showed good linearity with the correlation coefficients (R2) of 0.9986–0.9991 in the linear range of 2–300 μg L−1, low limits of detection of 0.5–1 μg L−1 and acceptable extraction recoveries in the range of 85–93%. The proposed method was successfully applied for the extraction and preconcentration of trace acaricides in real fruit juice samples, and the results demonstrated the potential of the synthesized DESs for the extraction and determination of contaminants in aqueous samples.

CAS / MDL: 5137-55-3
研究领域: 分析化学 · 食品安全
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MICROCHIMICA ACTA · 2021 ·Vol. 188 ·期 10 ·1-11 · IF 5.833

MIL-101(Fe)-derived magnetic porous carbon as sorbent for stir bar sorptive-dispersive microextraction of sulfonamides

Qin Peige,Han Lizhen,Zhang Xiaowan,Li Mengyuan,Li Dan,Lu Minghua,Cai Zongwei

Abstract Using MIL-101(Fe) as the source of carbon and Fe, a magnetic porous carbon (MPC) material with Fe 3 C nanoparticles encapsulated in porous carbon was prepared through one-pot pyrolysis under N 2 atmosphere. With MPC as adsorption material, a stir bar sorptive-dispersive microextraction (SBSDME) method was proposed to extract and preconcentrate sulfonamides (SAs) prior to HPLC-DAD determination. To investigate their extraction ability, different MPC materials were prepared under different carbonization temperatures (600, 700, 800, 900, and 1000 °C). The material prepared under 900 °C (MPC-900) exhibited the highest extraction ability for SAs. The as-prepared MPC materials were also characterized by Raman spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, zeta potential, and other techniques. The main parameters that affect extraction were systematically studied. Under optimal conditions, favorable linearity ( R 2  ≥ 0.9938) and detection limits (0.02–0.04 ng mL −1 ) of sulfonamides were obtained. The average recoveries for spiked milk and lake water samples ranged from 76.9 to 109% and from 75.4 to 118% with RSDs of 3.10–9.63% and 1.71–11.3%, respectively. Sulfameter and sulfisoxazole were detected in milk sample. Sulfisoxazole was detected in the lake water sample. The MPC-900 material demonstrated excellent reusability. It can be reused 24 times with peak areas having no obvious decline. The method can be applied to extract ultra-trace compounds in complex sample matrices. Graphical abstract Schematic presentation of a stir bar sorptive-dispersive microextraction (SBSDME) by using magnetic porous carbon (MPC) composites as sorbent combined with high-performance liquid chromatography for sensitive analysis of sulfonamides in milk and lake water samples.

研究领域: 分析化学 · 环境科学 · 材料科学
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