JOURNAL OF HAZARDOUS MATERIALS
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2025
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IF 11.3
Wendi Huo,Jincheng Li,Yupeng Wen,Xinyuan Zhang,Huan Liu,Yingchun Mu,Chunhui Zhao,Chaoying Zhang,Rongyue Zhang
In this study, we present a simple and rapid boronate affinity extraction methodology for the HPLC-MS/MS analysis of four nitrofuran metabolites (NFMs) including SEM, AOZ, AHD and AMOZ in fish samples. To enhance the efficacy of this approach, mesoporous poly(GMA-EGDMA) microspheres, abundant in cis-diols, were synthesized for boronate affinity extraction. Meanwhile, 4-fluoro-3-formylphenyl boronic acid was utilized for the derivatization of NFMs, facilitating the immobilization of boronate ligands onto their molecular structures. Compared to the Chinese national food safety standard GB 31656.13–2021, the boronate affinity extraction eliminates the need for extraction solvents and centrifugation, streamlines the pretreatment process, and maintains a mild extraction environment. Furthermore, the poly(GMA-EGDMA) microspheres exhibited excellent reusability, retaining their performance over six adsorption-desorption cycles. The NFMs demonstrated excellent linearity (R² > 0.999) across the range of 0.5 to 50 µg kg⁻¹ . The quantitative limit was established at 0.5 µg kg⁻¹ . The recoveries of spiked tilapia samples ranged from 94.2 % to 110.7 %, while intra-day and inter-day RSDs were below 5.9 %. This method emerges as an economical, straightforward, rapid, and sensitive alternative for monitoring of NFM residues in aquatic products.
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY
·
2020
·Vol. 246
·期 9
·1857-1865
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IF 2.366
Yang Fanfan,Xu Long,Liu Xiang,Chen Chen,Dias Alberto C. P.,Zhang Xiaoying
Abstract Bisphenol S (BPS) is a major alternative to Bisphenol A (BPA) newly applied in food packing material and disrupts reproductive and developmental endpoints through endocrine pathways. This study aimed to develop a rapid, sensitive, and accurate chemiluminescence immunoassay (CLIA) for the detection of BPS in canned beverage. Anti-BPS monoclonal antibody (mAb) was generated by immunizing Balb/c mice with immunogen (BPS–BSA conjugation). CLIA assay conditions, including 3-[9-(((3-( N -succinimidyloxycarboxypropyl) [4-methxylphenyl] sulfonyl) amine) carboxyl]-10-acridiniumyl)-1-propanesulfonate inner salt (NSP-SA-NHS) labeling ratio (1:40), antigen concentration (1 μg mL −1 ) and antibody titer (1:8000; 125 ng mL −1 in PBS (0.01 M, pH 7.4)) were determined, respectively. The half inhibition concentration (IC 50 ), detection limit (IC 10 ), and working range of the CLIA in canned beverage were 0.04, 1.48, and 0.32–5 ng mL −1 , respectively. Cross-reactivity with other bisphenols (4,4′-thiodiphenol, Bisphenol F, 4,4′- dihydroxy benzophenone, Bisphenol A and Bisphenol B) was less than 0.56%, and the recovery rates of BPS in canned beverage ranged from 80 to 109.2% (intra-assay) and from 82 to 108.4% (inter-assay). The results of CLIA were compared with high-performance liquid chromatography–UV (HPLC–UV) analysis, showing a good correlation of 0.956. After proper sample pre-treatment, this method allows relatively large amounts of sample analysis in a limited time period (30 min). Thus, it was deemed suitable and efficient for routine screening of BPS in canned beverage. Graphic abstract
研究领域:
分析化学
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环境科学
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食品安全
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免疫学
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毒理学
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JOURNAL OF CHROMATOGRAPHY A
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2019
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IF 3.858
Xiaolan Wang,Tao Feng,Juntao Wang,Lin Hao,Chun Wang,Qiuhua Wu,Zhi Wang
A magnetic porous covalent triazine-based organic polymer (M-PCTP) was synthesized by co-precipitation method. The M-PCTP combined both the properties of the PCTP and the magnetism of Fe 3 O 4 nanoparticles, possessing highly porous structure and good magnetism. It was used as a magnetic solid phase extraction (MSPE) adsorbent to extract carbamate pesticides (propoxur, carbaryl, isoprocarb, fenobcarb and diethofencarb) from lemonade and grape juice samples prior to high performance liquid chromatography-mass spectrometric detection. Under the optimal conditions, a good linearity for the real samples was received in the range from 0.10–0.90 to 80.00 ng mL −1 with the correlation coefficients of 0.9882–0.9983. The method recoveries for the five carbamates were 86.3–108.0%. The limits of detection were 0.02–0.20 ng mL −1 for lemonade sample, and 0.04-0.30 ng mL −1 for grape juice sample. The M-PCTP also demonstrated good extraction capabilities for other different kinds of organic compounds including chlorophenols and polycyclic aromatic hydrocarbons.
研究领域:
分析化学
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环境科学
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材料科学
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食品科学
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Food Bioscience
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2024
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IF 4.8
Yanbo Hu,Yiming Li,Yuzhu Shen,Baochun Zhang,Jiaxin Liu,Yi Cao,Jun Zhao
In this study, six rare protopanaxadiol (PPD)-type ginsenosides, namely, F2, CK, C-Mc1, C-Mc, CO, and CY, were prepared using enzymatic hydrolysis. Firstly, major (PPD)-type ginsenosides, including Rb1, Rb2, Rc, and Rd, were biotransformed by employing single and combined β-glucosidases BaBgl1A and BaBgl3A. Thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) analyses revealed that ginsenosides F2, CO, and C-Mc1 could be produced by BaBgl1A, while rare ginsenosides CK, CY, and C-Mc could be produced by the combined use of BaBgl1A and BaBgl3A. Furthermore, optimal preparation conditions for these rare ginsenosides were elucidated, with yields exceeding 76.34%. Additionally, large quantities of rare ginsenosides were prepared to determine their structures. Characteristic absorption peaks in 13 C NMR spectra and ion peaks in MALDI-TOF-MS suggested that the six high-purity rare ginsenosides (i.e., F2, CO and C-Mc1, CK, CY, and C-Mc) could be produced at high-efficiency. The findings of this study offer insights into novel enzymolysis methods for the targeted preparation of rare PPD-type ginsenosides, thus widening the range of raw materials that could be directed to in-depth biological activity research.
研究领域:
生物化学
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药理学
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生物技术
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SCIENCE OF THE TOTAL ENVIRONMENT
·
2020
·
IF 6.551
Yanping Xian,Ming Liang,Yuluan Wu,Bin Wang,Xiangchang Hou,Hao Dong,Liya Wang
Most of the reported magnetic adsorbents are difficult to absorb multi-class of per - and polyfluoroalkyl substances (PFASs), especially the short-chain PFASs. In this work, a novel fluorine and nitrogen functionalized magnetic graphene (G-NH-FBC/Fe 2 O 3 ) was first synthesized and characterized by scanning electron microscope (SEM), Fourier Transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). The as-prepared G-NH-FBC/Fe 2 O 3 was utilized as adsorbents for the magnetic solid-phase extraction (MSPE) of 19 PFASs from water and functional beverages and showed excellent adsorption capacity probably due to the hydrophobic interaction. Under the optimal pretreatment and instrumental conditions, a selective and sensitive high performance liquid chromatography Orbitrap high resolution mass spectrometry (HPLC-Orbitrap HRMS) method was developed for the determination of PFASs. Results indicated that the proposed method had favorable linearity (R 2 ≥ 0.994) within a wide range of concentrations. Limit of detection (LOD) and limit of quantification (LOQ) for the developed method ranged from 3 ng/L to 15 ng/L and 10 ng/L to 49 ng/L, respectively. Finally, the method was successfully applied to determine PFASs in drinking water , river water, tap water , factory drainage and functional beverages with recoveries ranging from 71.9% to 117.6% and relative standard deviation of <10%. The prepared G-NH-FBC/Fe 2 O 3 was easy to recycle and could be reused for five times without significant decrease in extraction recoveries of PFASs. These results demonstrated that this novel magnetic G-NH-FBC/Fe 2 O 3 could efficiently enrich PFASs and the proposed method is reliable and robust for the determination of PFASs in water and beverage samples.
研究领域:
环境科学
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分析化学
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MICROCHEMICAL JOURNAL
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2022
·
IF 5.304
Kaige Zhang,Rong Guo,Yunhe Wang,Jing Wang,Qiujun Nie,Bin Li,Guifen Zhu
A novel and green microextraction technique, temperature-controlled air-assisted liquid–liquid microextraction based on the solidification of floating deep eutectic solvents (DESs), was developed and applied for the extraction of triclosan and alkylphenols in different environmental waters. Hydrophobic DESs composed of menthol and myristic acid with melting points slightly higher than room temperature (25 ± 2 °C) were prepared and used as extraction solvent . First, the solid DES was transformed into liquid DES while the aqueous sample was heated in a water bath. Then, fine droplets were formed by withdrawing and injecting the mixture of aqueous sample and DES with a 1 mL pipette several times. After extraction, the solidified DES phase was obtained in an ice water bath. And then the analyses were performed by HPLC-UV. The microextraction parameters were investigated by the Plackett-Burman design and central composite design. The analytical parameters of this method were investigated and good linear ranges (0.5/1.0–400 μg/L, R 2 ≥ 0.9950), limits of detection (0.1–0.5 μg/L) and precision (≤5.9 %) were obtained. This method was successfully applied for the determination of triclosan and alkylphenols from five water samples with satisfactory recoveries (80.0–104.3 %). Subsequently, the green profile of the method was assessed by analytical Eco-Scale and Complementary Green Analytical Procedure Index. This method has the advantages of simplicity, rapidity, low cost, high sensitivity and green, which expands the application of solid solvents in liquid–liquid microextraction and has a wide application prospect.
研究领域:
分析化学
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环境科学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2026
·
IF 4.1
Liu Feng,Yu Decong,He Kun,Song Yanan,Li Yichao,Gao Haoxuan,Wu Bing,Li Xiaoyu,Zhao Ji,Xu Fei,Yang Huifang
The widespread use of neonicotinoids has raised growing concerns about their potential health risks. In this study, we developed a robust and high-throughput analytical method based on liquid-liquid extraction (LLE) and dispersive solid-phase extraction (dSPE), followed by high-performance liquid chromatography-quadrupole-Orbitrap high-resolution mass spectrometry (HPLC-Q-Orbitrap HRMS) for the simultaneous determination of 11 neonicotinoids and their 6 metabolites in human urine. After pretreatment of LLE and dSPE, qualitative and confirmatory analysis was achieved using tMS 2 acquisition of HPLC-Q-Orbitrap HRMS, and quantitative analysis was performed using isotope-labeled internal standards and matrix-matched calibration curves. The method was validated with good linearity ( R 2 > 0.9975), recoveries of 75.8%~118.9% (RSDs < 15%), and detection limits of 0.001~0.06 μg/L. The established method was successfully applied to urine samples of community-dwelling elderly population individuals ( n = 150) and to a suspected case of acute acetamiprid poisoning in Ningxia, China. The results showed that thirteen neonicotinoids and metabolites were detected in the elderly cohort, and the poisoning incident was confirmed to be caused by acetamiprid and its metabolite N-desmethyl-acetamiprid. Meanwhile, Spearman correlation analysis indicated significant positive correlations between parent compounds and their metabolites for all analytes except acetamiprid, and a strong correlation between clothianidin and thiamethoxam, suggesting shared exposure sources or common metabolic pathways. The established method is sensitive, accurate, and high-throughput, and has proven reliable for human biomonitoring and health risk assessment of neonicotinoid exposure. Graphical
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
Jing Sun,Dan-Yi Jiang,Hui-Min Qiang,You-Long Feng,Yao-Zuo Yuan,Yun-Jing Zhang
Novel DART-HRMS & HPLC workflow screens 8 additives in cosmetics • Ambient MS inherently bypasses ZnPT/PO metal-chelation artifacts • High-throughput screening handles surfactant matrices under 2 min • Green method with simple extraction and minimal solvents • 3-year survey of 150 samples tracks regulatory phase-out of ZnPT Unregistered and excessive use of restricted anti-dandruff agents and the illegal addition of prohibited antibiotics in hair care products pose growing concerns, but monitoring is complicated by lack of integrated screening workflows, as well as the presence of surfactant-rich matrices and metal-chelating properties of some anti-dandruff agents like zinc pyrithione (ZnPT) and piroctone olamine (PO). This study presents a high-throughput “profile-and-quantify” strategy combining direct analysis in real-time high-resolution mass spectrometry (DART-HRMS) with high-performance liquid chromatography (HPLC) to monitor eight targets in shampoos and conditioners. After acetonitrile-methanol ultrasonic extraction, samples were screened using DART-HRMS under optimized parameters. Samples containing the target analytes were subsequently quantified using high-performance liquid chromatography with diode array detector (HPLC-DAD). Validation of this dual-platform approach demonstrated limits of detection ranging from 0.1 to 4 μg/g for the target analytes. For quantitative analysis, the HPLC-DAD assay exhibited good linearity ( r ² ≥ 0.9995). Spiked recoveries ranged from 96.1% to 107.2% with precision (RSD) ≤ 3.22%. This integrated strategy was applied to a longitudinal survey of 150 commercial products collected from 2022 to 2024. Screening revealed a widespread occurrence of ZnPT, salicylic acid, climbazole, and PO, while also identifying illicit additions of antifungal drugs including miconazole, elubiol, ketoconazole, and clotrimazole in cosmetic formulations. Featuring a rapid screening step of under 2 min per sample prior to targeted quantification, this integrated workflow offers a highly efficient, sensitive, and eco-friendly solution for large-scale regulatory monitoring of cosmetic safety and compliance. Download: Download high-res image (325KB) Download: Download full-size image
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Foods
·
2026
·Vol. 15
·期 19
·3570
·
IF 6
Chenyang Deng,Mengqing Liu,Kaiwen Chen,Cetao Tang,Yue Kang,Hao Zhang,Yazhong Zhang,Chuanshan Jin,Deling Wu,Xiaoli Wang
Semen Cuscutaeis commonly used as a medicinal and edible functional food ingredient. Salt-processing can significantly alter its sensory quality and endogenous components. Currently, salt-processedSemen Cuscutaemainly adopts hyperoside as the quality evaluation indicator, which fails to meet the requirements for the identification of processing intensity (heat level) during the development of the traditional Chinese medicine industry. This study aims to construct a comprehensive quality evaluation framework for identifying the optimal processing degree of salt-processedSemen Cuscutae. Multi-dimensional bionic technologies including machine vision, electronic nose and electronic tongue, combined with HPLC and GC-IMS, were applied to analyze the changes in sensory characteristics and endogenous components of salt-processedSemen Cuscutaeacross different processing degrees. Characteristic indicators were comprehensively scored using the AHP-TOPSIS method. Compared with other groups, appropriately processed salt-processedSemen Cuscutaeexhibited a brown appearance, significantly different W1W/W2W sensor responses, resulting in a more harmonious taste profile and distinct volatile chemical markers. Further correlation analysis was performed among bionic sensing indicators, endogenous components and GC-IMS-derived volatile data. AHP-TOPSIS results demonstrated that salt-processedSemen Cuscutaewith an appropriate processing degree exhibits optimal comprehensive quality. The comprehensive quality evaluation framework established in this study provides scientific support for the process control and quality assessment ofSemen Cuscutaeas a functional food ingredient, and also offers a methodological reference for the processing evaluation of similar medicinal and edible food materials.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Shuo Xie,Wenbin Zhang,Yike Han,Xinyan Dong,Wanning Li,Penghui Li,Liyun Kong
The accurate determination of pharmaceuticals and personal care products (PPCPs) in wastewater is crucial for comprehensive environmental risk assessment and human exposure evaluation. Given the complex matrices of aqueous environmental samples, efficient sample preparation remains a critical challenge in analytical procedures. This study presents an ionic liquid-based aqueous two-phase system (IL-ATPS) extraction methodology used as a pretreatment step prior to high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of 38 PPCPs. A mechanistic investigation revealed that target analytes with more hydrogen-bonding sites and higher hydrogen-bond donor (HBD) capacity exhibited enhanced solubility in ILs. In addition, IL anions with stronger hydrogen-bond acceptor (HBA) capacity further improved the solubility of the 38 PPCPs. These findings indicate that hydrogen bonding between analytes and ILs likely played a critical role in the dissolution mechanism. The established IL-salt ATPS extraction method utilized a 15 mL aqueous sample, 0.2 g tetraethylammonium acetate ([N 2222 ][OAc]), and 12 g K 2 HPO 4 , with a 1-minute vortex mixing. Compared with traditional solid phase extraction (SPE), this approach significantly reduced the sample volume from 1 L to 15 mL, avoided the use of volatile organic solvents, simplified the overall processing, and enabled rapid (<15 minutes) pretreatment. The method demonstrated excellent sensitivity with limits of detection (LODs) ranging from 0.00013 to 0.11 ng/mL. Method validation via standard addition experiments demonstrated satisfactory accuracy, yielding recoveries between 74.3 and 129.8 %. Precision was assessed using both intra-day and inter-day measurements. The intra-day relative standard deviations (RSDs) ranged from 0.7 % to 19.9 %, while the inter-day RSDs ranged from 1.4 % to 18.4 %, demonstrating that the method provides consistent and reproducible results under controlled laboratory conditions. These findings underscore the present IL-based ATPS extraction method, followed by HPLC-MS/MS analysis, as an eco-friendly, robust, and scalable approach for PPCPs monitoring in aqueous environmental samples, offering potential applications in environmental monitoring and risk assessment.
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ANALYTICAL LETTERS
·
2021
·
IF 2.329
Zhaoxue Zhang,Yi Lu,Haipu Li,Nan Zhang,Junfei Cao,Bo Qiu,Zhaoguang Yang
The simultaneous separation and determination of inorganic trivalent antimony Sb(III) and pentavalent antimony Sb(V) in plant, soil, and sediment samples was carried out by high performance liquid chromatography – inductively coupled plasma – mass spectrometry (HPLC-ICP-MS). The chromatographic conditions (composition and concentration of competing ion, pH value and flow rate of mobile phase) and the operating parameters for inductively coupled plasma – mass spectrometry were optimized by single factor experiments. The separation of the Sb species was achieved within 6 min using the optimized chromatographic conditions. The detection limits of the method were 0.016 μg/L and 0.021 μg/L for Sb(III) and Sb(V), respectively. The retention times of Sb(V) and Sb(III) were 2.7 min and 4.5 min, respectively. The relative standard deviations for replicate measurements (n = 6) of low (5 μg/L), medium (20 μg/L), and high (40 μg/L) concentrations of Sb(III) and Sb(V) were less than 4%. The results of spiking and recovery experiments for the extracting solutions of soil, sediments, and plants showed that the spiked recoveries of the two species ranged from 92% to 103%. This method has been used to determine the antimony species in extracts of environmental samples.
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Liyan Jia,Xin Huang,Wenfei Zhao,Huihui Wang,Xu Jing
In this study, a simple, efficient, and green effervescence tablet-assisted microextraction method based on the solidification of deep eutectic solvent (ETA-ME-SDES) was developed to determine picoxystrobin, pyraclostrobin, and trifloxystrobin in water, juice, wine, and vinegar samples by HPLC. An eco-friendly, hydrophobic, deep eutectic solvent (DES, acting as the extraction solvent) was synthesized by thymol and octanoic acid in the molar ratio of 1:5. The extraction solvent dispersed in sample solutions with the assistance of pH adjustment and effervescence reaction, and was collected after solidification in an ice bath. Several essential conditions, including the type and the volume of DESs, the amount of ammonia hydroxide, and the components of effervescence tablets were optimized. The limits of detection ranged from 0.15 to 0.38 μg L −1 . Extraction recovery ranged from 77.4 to 106.9%. The proposed method was successful in determining the amount of strobilurin fungicides in water, juice, wine, and vinegar samples.
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