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JOURNAL OF CHROMATOGRAPHY A · 2015 · IF 4.169

A series of strategies for solving the shortage of reference standards for multi-components determination of traditional Chinese medicine, Mahoniae Caulis as a case

Wenguang Wang,Xiaoli Ma,Xiaoyu Guo,Mingbo Zhao,Pengfei Tu,Yong Jiang

In order to solve the bottleneck of reference standards shortage for comprehensive quality control of traditional Chinese medicines (TCMs), a series of strategies, including one single reference standard to determine multi-compounds (SSDMC), quantitative analysis by standardized reference extract (QASRE), and quantitative nuclear magnetic resonance spectroscopy (qNMR) were proposed, and Mahoniae Caulis was selected as an example to develop and validate these methods for simultaneous determination of four alkaloids, columbamine, jatrorrhizine, palmatine, and berberine. Comprehensive comparisons among these methods and with the conventional external standard method (ESM) were carried out. The relative expanded uncertainty of measurement was firstly used to compare their credibility. The results showed that all these three new developed methods can accurately accomplish the quantification by using only one purified reference standard, but each of them has its own advantages and disadvantages as well as the specific application scope, which were also discussed in detail in this paper.

CAS / MDL: 120-12-7
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

Engineered Hydrophobic Porous Fe3O4 Microparticles for Solvent-Confined Dispersive Liquid-Phase Microextraction

Meiijian Wang,Hao Wang,Shiyun Lou,Dexi Tao,Yaolin Tang,Bingfang Zou,Yongqiang Wang

Liquid-phase microextraction (LPME) relies critically on precise solvent control to achieve efficient extractant recovery. To address this, we developed a magnetic microparticle-based dispersive liquid-phase microextraction (MP-DLPME) strategy, employing hydrophobic porous Fe 3 O 4 microparticles (∼1 μm) as solvent-stabilizing microcarriers. These microparticles were functionalized via covalent grafting of 3-chloropropyltriethoxysilane (CPS) and optimized porosity, enabling rigid confinement of organic solvents (e.g., 1-octanol) through dual mechanisms: (I) hydrophobic solvent anchoring to modified surfaces and (II) capillary trapping within mesopores. When applied to hydrophobic polycyclic aromatic hydrocarbons (PAHs) and organophosphorus pesticides (OPPs), the system generates solvent-encapsulated magnetic aggregates that dynamically fragment into microdroplets under vortex-induced shear forces, facilitating efficient analyte extraction via magnetic collection. By integrating the high efficiency of dispersive extraction with the rapid recovery of magnetic separation, the MP-DLPME method provides a robust sample pretreatment solution for environmental water analysis.

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MARINE POLLUTION BULLETIN · 2025 · IF 4.9

Characterization of the vertical distribution of polycyclic aromatic hydrocarbons in mangrove sediments of Guangxi and ecological risk assessment

Ruicong Gao,Jiaqi Lu,Zhixuan Wei,Hao Xu,Siyuan Jing,Minghuo Wu

PAHs, a group of persistent organic pollutants with significant carcinogenic and mutagenic effects, are widely distributed in the environment and can accumulate in sediments, posing potential threats to mangrove ecosystems and human health. This study is one of the most recent studies that presents an analysis of the vertical contamination characteristics of PAHs in mangrove sediments down to a depth of 80 cm, utilizing a combination of solid-phase extraction and gas chromatography–mass spectrometry. The results showed that the mean value of PAHs was 258.82 ng/g (range from 226.41 to 320.07 ng/g) in the studied mangrove areas (Beihai City, Guangxi). The results indicated a decline in PAH concentrations with increasing sediment depth, with values of 259.3 ng/g in surface sediments (0–10 cm), 240.9 ng/g in intermediate sediments (30–40 cm), and 241.1 ng/g in deeper sediments (60–70 cm). This suggests that PAHs not only remain in the surface layer of the sediment, as in previous studies, but also migrate vertically within the sediment. Based on the results, the potential ecological risks of PAHs were also evaluated by the ERL/ERM model. After environmental risk assessment, it was found that among the six PAHs studied, the contents of all except acenaphthene were lower than the ERL, indicating a low ecological risk. This study elucidates the vertical distribution of PAHs in mangrove sediments, offering crucial data for ecological risk assessment and establishing a foundation for future research on PAH transport mechanisms and their ecological impacts, thereby informing environmental management strategies.

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GREEN CHEMISTRY · 2025 · IF 9.2

Porous ionic liquids from cyclodextrin carbon for deep extraction of polycyclic aromatic hydrocarbons

Kaihao Mo,Peng Cui,Dongni Liu,Cailan Chen,Hanyu Zhang,Minmeng Tang,Peiwen Wu,Yan Huang,Haiyan Ji,Wenshuai Zhu

In extraction processes, the low mass transfer efficiency of conventional ionic liquids is a refractory problem. Herein, a porous ionic liquid (PIL), β-CD-900-PIL, was innovatively constructed by combining a porous carbon material (β-CD-900) derived from β-cyclodextrin polymer with imidazole bis-trifluoromethylsulfonylimide ionic liquid ([C12mim][NTf2]). The N2 sorption isotherm and CO2 adsorption confirmed the porosity of β-CD-900 and the PIL. With the dispersion amount of β-CD-900 as 20 wt%, the extraction efficiency of naphthalene by β-CD-900-PIL reached 66.6%, which was 24% higher than that of the ionic liquid. After three extractions, the naphthalene content decreased from 500 mg L−1 to 5 mg L−1. The high extraction efficiency was attributed to the high porosity and abundant π–π and C–H⋯π interactions between PILs and naphthalene. The more than 99% extraction performance, low viscosity and low preparation cost make β-CD-900-PIL an ideal extractant for polycyclic aromatic hydrocarbons in the petrochemical industry.

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JOURNAL OF CHROMATOGRAPHY A · 2018 · IF 3.716

Preparation of silica colloidal crystal column and its application in pressurized capillary electrochromatography

Qing Liu,Kevin Yan,Qiaomei Chen,Soumia Cheddah,Lin Shen,Han Xiao,Yan Wang,Chao Yan

Capillary column packed with silica colloidal crystals (SCC) exhibits great efficiency in liquid chromatography because of its highly-ordered structure and extremely narrow channels (about hundred nanometer in diameter) between the particles. However, problems arise due to the extremely high back-pressure created with its dense packings. It is also a challenge to prepare a stable SCC column with an appropriate length for chromatographic separation on a commercial instrument. We have synthesized monodispersed, sub-micron SiO 2 particles bonded with C18 functionality and fabricated SCC capillary columns up to 100 mm in length. The packing materials in the column displayed Bragg diffraction with blueish color under irradiation with white light, indicating the formation of SCC. The column performance was evaluated using pressurized capillary electrochromatography (pCEC) and column efficiencies of more than a hundred thousand plates per column (plate height < 1 μm) were achieved using peptide as a sample. The run-to-run reproducibility expressed with RSD in terms of retention time and peak area for aromatic compounds were less than 0.076% and 1.96%, respectively. These results demonstrate that the combination of pCEC and SCC columns may provide an innovative analytical technique with extraordinary efficiency, resolution and speed for the separation of complex samples.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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CHEMICAL ENGINEERING JOURNAL · 2025 · IF 13.2

Interface selectivity-based biochar: Directional evolution of properties, application & carbon neutralization evaluation

Wang Kai Tong,Chaomeng Dai,Jiajun Hu,Mei Ru Yue,Yun Dong Liu,Bu Li,Jia Jie Zou,Jia Wang,Han Tang,Min-tian Gao,Yucang Liang,Wenjuan Wang,Jixiang Li

Hydrophobic organic contaminants (HOCs) threaten human health and ecosystems. The most economical and low-carbon remediation method employs surfactants to mobilize HOCs, followed by separation using carbon-based materials. A carbon-structure superimposition strategy (CSSS) was developed to prepare interface selectivity-based colloidal biochar (CBC-AO). In a solution with a pollutant concentration of 2.5 mg/L phenanthrene, a 99 % removal efficiency was achieved, and a 100 % recovery rate was obtained for common anionic surfactants. Notably, CSSS offers a unique approach to using lignocellulose-based biomass (LB)-derived biochar as an alternative to activated carbon (AC). The uniqueness of CSSS lies in revealing the carbon structure transfer mechanism, where cellulase pretreatment converts LB into aromatic carbon substrates, followed by air oxidation and colloidal treatment to transform unfavorable carbon structures into those beneficial for selective adsorption. This modification grants biochar selectivity and stability, addressing the challenge of balancing different carbon structures and functions. CBC-AO achieved a 90 % reuse rate after six cycles. Compared with traditional biochar, its acute biological toxicity was reduced by 77 %, and its environmental friendliness was further increased. In terms of carbon emissions and cost, CBC-AO outperforms AC, reducing emissions by 0.62 tons of CO 2 per year, whereas AC increases emissions. CSSS overcomes traditional biomass selection limitations, broadening biomass options and providing efficient, economical, and carbon-negative alternatives to conventional carbon-based materials. Furthermore, integrating CSSS with biofuel production results in biochar performance comparable to commercial AC, potentially advancing both industries.

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ANALYTICA CHIMICA ACTA · 2015 · IF 4.513

Monodisperse microporous carbon nanospheres: An efficient and stable solid phase microextraction coating material

Juan Zheng,Kun Wang,Erlun Luo,Dingcai Wu,Fang Zhu,Ruifen Jiang,Chengyong Su,Chaohai Wei,Gangfeng Ouyang

The monodisperse microporous carbon nanospheres (MMCNSs) were applied in solid phase microextraction for the first time. The MMCNSs-fiber was prepared by sol–gel technique and good repeatability and reproducibility were obtained, due to the excellent monodispersity of the MMCNSs . The sol–gel-MMCNSs fiber exhibited superior extraction ability for polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs), compared with the commercial polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber and the fiber prepared with its precursor, the monodisperse microporous polystyrene nanospheres (MMPNSs). Moreover, the fiber has good thermostability and strong acid/base durability. The sol–gel-MMCNSs fiber was then employed to detect PAHs and OCPs in aqueous samples by combining with gas chromatography–mass spectrometer (GC–MS). Under the optimized conditions, the detection limits of the proposed method ranged from 0.10 to 5.5   ng   L −1 . Furthermore, the method was successfully utilized for the analysis of PAHs and OCPs in real samples, with satisfactory recoveries in the range of 81.0–120% for the Pearl River water samples and 72.8–118% for the coking wastewater samples.

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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2017 ·Vol. 409 ·期 19 ·4559-4569 · IF 3.431

Hexafluoroisopropanol-mediated cloud point extraction of organic pollutants in water with analysis by high-performance liquid chromatography

Xu Jia,Li Yunfang,Li Cao,Zhang Rui,Xiao Yuxiu

A hexafluoroisopropanol (HFIP)-mediated cloud point extraction (CPE) system was established. A small amount of HFIP (even 1%, v / v ) can dramatically reduce the cloud point of Triton X-100 (TX-100) aqueous solution (even to 1 °C) and make liquid-liquid two-phase separation (coacervate phase and aqueous phase) occur at room temperature over a wide range of TX-100 concentration (0.5∼10%, g/mL). HFIP-mediated coacervate phase has smaller volume (volume ratio is 1.8∼8.9% relative to the volume of the total solution with 1∼5% TX-100) and larger micelle aggregates (30∼80 nm in diameter) compared to temperature-induced coacervate phase (volume ratio at 2.8∼14.0%, the diameter of micelle aggregates at 5∼30 nm). HFIP-mediated CPE was coupled to high-performance liquid chromatography with ultraviolet detection (HPLC-UV) for the extraction and detection of organic pollutants in water, namely, polycyclic aromatic hydrocarbons (PAHs), fluoroquinolones (FQs), and sulfonamides (SAs) with different polarities, charges, and hydrogen-bonding properties. HFIP-mediated CPE provides much higher extraction rates (ERs) and enrichment factors (EFs) for FQs (91∼106%, 50∼59), PAHs (63∼90%, 33∼49), and SAs (26∼55%, 16∼34) compared with the temperature-induced one (ERs: 4∼8% for FQs, 25∼46% for PAHs, and 4∼37% for SAs; EFs: 1∼3 for FQs, 6∼12 for PAHs, and 8∼13 for SAs). The limit of detection ranges from 0.24 to 0.33 ng/mL for FQs, 0.04 to 0.38 ng/mL for PAHs, and 0.63 to 1.31 ng/mL for SAs. The proposed method was applied in the analysis of real water samples, and the recovery of 79.4∼110.8% and the relative standard deviation of 0.2∼16.3% were achieved for the three types of pollutants. Schematic illustration of HFIP-mediated cloud point extraction

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JOURNAL OF CHROMATOGRAPHY A · 2015 · IF 4.169

Magnetic nanoparticles with hydrophobicity and hydrophilicity for solid-phase extraction of polycyclic aromatic hydrocarbons from environmental water samples

Shu-Wen Xue,Min-Qiong Tang,Li Xu,Zhi-guo Shi

Magnetic nanoparticles (MNPs) featured with divinylbenzene (DVB) and sulfonate functionalities (Fe 3 O 4 –DVB–SO 3 − ) were prepared via “thiol-ene” click chemistry. The hydrophobic DVB moieties were dedicated for extraction while the hydrophilic sulfonate groups were designed for dispersing the MNPs in aqueous sample solution. Thus, the specially designed material could ensure operational convenience and improve reproducibility during extraction. The application of the material was demonstrated by the extraction of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples followed by gas chromatography–mass spectrometric analysis. The main factors influencing the extraction, including the type of the desorption solvent, the agitation mode, the amount of MNPs, extraction and desorption time and salt addition in sample solution, were investigated in detail. Under the optimized conditions, the proposed method showed satisfactory reproducibility with intra-day and inter-day relative standard deviations less than 16.5% and 21.2%, and low limits of detection of 1.1   pg   mL −1 , 0.8   pg   mL −1 , 1.1   pg   mL −1 , 1.4   pg   mL −1 , 0.6   pg   mL −1 , 2.1   pg   mL −1 and 0.7   pg   mL −1 for naphthalene, acenaphthene, fluorine, phenanthrene, anthracene, fluoranthene and pyrene, respectively. The developed method was also successfully used for determination of the PAHs in genuine lake and river environmental water samples by standard addition method. All the studied PAHs were detected in these waters with comparable results by the standard liquid–liquid extraction method. The developed MNPs with dual property of hydrophobicity and hydrophilicity were suitable for the treatment of water samples. The magnetic solid phase extraction based on this material was reliable and convenient. It has great potential in the preconcentration of trace analytes in complex matrix.

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JOURNAL OF CHROMATOGRAPHY A · 2014 · IF 4.258

A novel urea-functionalized surface-confined octadecylimidazolium ionic liquid silica stationary phase for reversed-phase liquid chromatography

Mingliang Zhang,Ting Tan,Zhan Li,Tongnian Gu,Jia Chen,Hongdeng Qiu

One-pot synthesis of surface-confined ionic liquid functionalized silica spheres was proposed using N -(3-aminopropyl)imidazole, γ- iso propyltriethoxysilane and 1-bromooctadecane as starting materials. The surface modification of the silica spheres was successful with a high surface density of octadecylimidazolium, enabling the utilization of this new urea-functionalized ionic liquid-grafted silica material as stationary phase for high-performance liquid chromatography in reversed-phase mode. The long aliphatic chain combined with the multiple polar group embedded in the ligands imparted the new stationary phase fine selectivity towards PAH isomers and polar aromatics and higher affinity for phenolic compounds. The unique features of the new material, especially the effect of the urea group on the retention were elucidated by mathematic modeling.

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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2019 ·Vol. 411 ·期 18 ·4073-4084 · IF 3.286

An online field-assisted micro-solid-phase extraction device coupled with high-performance liquid chromatography for the direct analysis of solid samples

Xia Ling,He Yuanyuan,Xiao Xiaohua,Li Gongke

Herein, a total online device based on field-assisted extraction (FAE), micro-solid-phase extraction (μ-SPE), and high-performance liquid chromatography (HPLC) was designed. Solid samples were pretreated with ultrasound-microwave synergic effects, and then the extract was cleaned up online with a monolithic column, followed by HPLC analysis. The cross-actions between ultrasound and microwave along with other extraction parameters were studied systematically. The efficiency of this online method was verified in the determination of polycyclic aromatic hydrocarbons (PAHs) in foods and tetracycline antibiotics (TCAs) in cosmetic samples. The detection limits of nine PAHs including fluorene, phenanthrene, anthracene, fluoranthene, benzo[k]fluoranthene, benz[a]anthracene, benzo[b]fluoranthene, pyrene, and benzo[a]pyrene were all within 0.075–0.30 μg/kg, as well as four TCAs including oxytetracycline, tetracycline, chlortetracycline, and doxycycline were within 0.02–0.06 μg/kg. Six PAHs were found in roast potatoes and baked fish and the recoveries were in the range of 71.5–119.7% with RSDs of 0.2–10.9% ( n  = 3). The recoveries for TCAs in cosmetic samples were in the range of 75.3–118.0% with RSDs lower than 8.2% ( n  = 3). Compared with those offline methods, this total online FAE-μ-SPE-HPLC method not only simplifies the operation process, but also increases the precision and accuracy. Beyond trace analytes analysis in solid and semi-solid matrixes, application of this total online analysis method can also be extended to investigate field-assisted extraction mechanisms. Graphical abstract

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JOURNAL OF MOLECULAR LIQUIDS · 2025 · IF 5.2

Dissolution of anthracene in aromatics: Solubility, correlation and thermodynamic analysis

Yixuan Wang,Zhenmin Cheng,Quanjie Liu,Chao Yang,Liming Jia,Chen Yang,Hongxin Bai

Anthracene is characterized by its unique electronic and organic properties as the cornerstone for various applications. Particularly in the synthesis of anthraquinone derivatives, anthracene serves as the key raw materials in the alkylation and oxidation, acting as the hydrogen carrier for hydrogen peroxide production via AO process. However, inadequate knowledge about its dissolution behavior in solvents has been one of the main limitations for its purification and practical applications, commonly resulting in its unsatisfactory commercial products and thus leads to insufficient efficiency of chemical synthesis. In this study, the solubility behavior of anthracene in various solvents was specifically investigated by the synthetic method at temperatures ranging from 304.15 to 338.15 K under atmospheric pressure. To facilitate decent solvent s screening, aromatics such as benzene and its derivatives were specifically exploited as the working solution components in this work. The experimental solubility values and their corresponding activity coefficient of anthracene were analyzed and correlated on the basis of modified Apelblat and λ-h models. Furthermore, thermodynamic analysis, including the changes of enthalpy, entropy, and Gibbs free energy, was subsequently conducted using the modified Van’t Hoff equation. As a result, the dissolution of anthracene is an endothermic and entropy-driven process in studied solvents, among which chlorobenzene seems to be the most actively interactive with anthracene and thus results to the best dissolving capacity for anthracene.

CAS / MDL: 120-12-7
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