JOURNAL OF HAZARDOUS MATERIALS
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2026
·
IF 10.6
Fenghong Wei,Pei Wang,Junjun Hu,Yanping Zheng,Xiaojia Huang
Sample preparation is critical in developing a sensitive and accurate method for the monitoring of ultrashort- to long-chain perfluorocarboxylic acids (PFCAs) in complex samples. However, it remains a formidable challenge in the simultaneous and efficient extraction of ultrashort- to long-chain PFCAs (U-L@PFCAs) due to their significantly different polarity. In this connection, the electric field-assisted microextraction (EFAM) was introduced for the first time to efficiently co-extract ultrashort- to long-chain species. According to the chemical properties of the studied U-L@PFCAs, a new microelectrode based on a monolithic adsorbent (MEMA) was tailored using diallylamine and 1,1,1,3,3,3-hexafluoroisopropyl acrylate as dual monomers and employed as the microelectrode of EFAM. Results disclosed that the application of opposite directions and different intensities of electric field at adsorption and desorption stages enhanced the increase of extraction efficiencies by 78.6–131% in comparison with the omission of electric field. In addition, the adsorption characteristics, behavior, and mechanism of MEMA@EFAM towards the investigated U-L@PFCAs were explored. Under the selected microextraction conditions, a sensitive and reliable method based on an isotope internal standard calibration curve technique for monitoring ultra-trace U-L@PFCAs in various environmental water and human urine samples was established by combining MEMA@EFAM with HPLC-MS/MS detection. Low detection limits of 0.13–1.4 ng/L and superior precision (RSDs varied from 2.8% to 9.1%) were achieved with minimum background interference. The present study provides a highly competitive alternative for the broad-spectrum monitoring of PFCAs.
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Qi Zhou,Lihong Wang,Canping Pan,Congcong Yu,Jin Hua,Tao Lan
Considering the matrix characteristics of honeysuckle and chrysanthemum, a comprehensive and systematic extraction and purification processes study for pesticide residue analysis in these two Traditional Chinese Medicine (TCM) were conducted based on a nanomaterial-modified QuEChERS method. For honeysuckle, a combination of 60 mg FeN-MWCNTs and 60 mg PSA provided the best purification effect. For chrysanthemum, 70 mg GCB and 30 mg PSA achieved the optimal results. Our initial exploration into the purification mechanism of the nanomaterials revealed that micropores and smaller mesopores in the adsorbents play a crucial role, while amino groups primarily govern the adsorption process, with matrix impurities adhering to the surface of the nano-adsorbents. The limit of quantification (LOQ) for honeysuckle in this method ranged from 0.12 to 18.86 µg/kg, with recovery rates between 60.1 % and 128.6 %, and relative standard deviations (RSD) less than 12 %. For chrysanthemum, the LOQ was between 0.10 and 8.56 µg/kg, and the recovery rates for 27 pesticides were in the range of 61.6 % to 118.9 %. Applying this method, 105 honeysuckle and 111 chrysanthemum market samples were analyzed, detecting five pesticides in 18 honeysuckle and 12 chrysanthemum samples respectively. This study offers a targeted strategy for the development of analytical methods for trace substances in complex matrices.
研究领域:
分析化学
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中药学
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环境科学
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高影响因子
JOURNAL OF HAZARDOUS MATERIALS
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2023
·
IF 13.6
Nan Li,Juan Zheng,Lu-Dan Yu,Yuan-Jun Tong,Xinying Gong,Yu Hou,Guosheng Chen,Jianqiao Xu,Fang Zhu,Gangfeng Ouyang
The complex sample matrix and low environmental concentration make it challenging to effectively determine the polar glucocorticoids. In particular, a green, economical, and environmentally friendly method is urgently needed, since a large amount of extraction solvents, samples, and extraction materials have been commonly used to improve the sensitivity of the reported methods. In this study, a green and robust phenol and bismuth-based MOF of SU101 was mildly synthesized and fabricated as a brand new solid-phase microextraction (SPME) fiber. Only tiny amounts of SU101 and desorption solvents were employed to realize the high-efficiency enrichments of glucocorticoids from water samples. The detection performance of proposed SU101 fiber towards glucocorticoids was much superior to the single-component and multi-component commercial fibers. It indicated that SU101 fiber could be an excellent candidate for the enrichments of polar pharmaceuticals. After it was coupled with the instrument of high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), the linear range of 5–10000 ng L −1 with detection limits low to 0.070–1.5 ng L −1 and satisfactory recoveries were achieved by the developed method. Benefiting from the environmental friendliness of SU101 and the less-solvent consumption of SPME technique, this work presented a green and economical strategy for determinations of trace glucocorticoids.
研究领域:
环境科学
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分析化学
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材料科学
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2026
·
IF 5.2
Chaoying Zhang,Bohao Qi,Xin Huang,Jincheng Li,Yingchun Mu,Huan Liu
A residue accumulation-guided strategy was developed for preparing grass carp matrix candidate reference materials. • Parent nitrofuran drugs were introduced by medicated bath to generate four marker metabolites in fish muscle. • HPLC–MS/MS enabled reliable quantification of nitrofuran marker metabolites in grass carp powder. • A 10 h bath exposure at 25 °C achieved target residue levels of 5–10 μg/kg. • The prepared candidate materials showed acceptable homogeneity, stability, and batch-to-batch reproducibility. The preparation of incurred aquatic matrix candidate reference materials remains challenging because residue formation is influenced by biological exposure processes and matrix interactions. In this study, a residue accumulation-guided strategy was developed for the preparation of a grass carp matrix candidate reference material containing four nitrofuran marker metabolites, including semicarbazide (SEM), 3-amino-2-oxazolidinone (AOZ), 1-aminohydantoin (AHD), and 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ). The relationship between medicated-bath exposure conditions and muscle residue levels was evaluated and used to determine practical preparation conditions. Under the optimized exposure conditions, grass carp samples were collected, homogenized, freeze-dried, ground, sieved, and blended to obtain a homogeneous candidate material. The prepared candidate material showed acceptable homogeneity and stability under the investigated conditions and yielded batch-to-batch reproducibility with RSD values of 1.9–3.2% for 0.4 g freeze-dried test portions. The developed material exhibited suitable characteristics for potential applications in analytical quality assurance, method comparison, and related scientific studies. This study provides an alternative strategy for preparing grass carp matrix candidate reference materials containing incurred nitrofuran marker metabolites through controlled biological exposure and residue accumulation-guided preparation. Download: Download high-res image (172KB) Download: Download full-size image
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Dongqin Tan,Yue Wang,Haocheng Fan,Jing Jin,Xiaoli Sun,Dhanjai,Degao Wang
Magnetic surface imprinted polymer microspheres (Fe 3 O 4 @MIPs) were successfully synthesized via Pickering emulsion polymerization, utilizing N-Methylphenethylamine as a surrogate template for amphetamine-type drugs. Fe 3 O 4 @MIPs not only possessed excellent dispersibility and enough magnetic properties in aqueous solutions, but also displayed good selectivity towards six amphetamines, with an imprinting factor ranging from 1.8 to 2.6. The adsorption kinetics closely aligned with the pseudo-second-order model, and the adsorption efficiency exceeds 80 % for each amphetamine at equilibrium. Fe 3 O 4 @MIPs were then employed as the efficient adsorbents for the extraction of amphetamine drugs. Extraction parameters, including sample pH, the mass of adsorbent, and the type and volume of eluting solvent, were carefully optimized. In combination with the high performance liquid chromatography tandem triple quadrupole mass spectrometry (HPLC-MS/MS), a selective magnetic solid-phase extraction (MISPE) method utilizing Fe 3 O 4 @MIPs was developed for the detection of six amphetamines in water samples. The limits of detection and limits of quantitation were determined to be 5.2∼23 ng L −1 and 17∼77 ng L −1 , respectively. Recoveries for the six target drugs from lake water and sewage samples fell within the range of 87.2∼110 %. Additionally, the MISPE-HPLC-MS/MS method exhibited excellent repeatability, with a precision below 8.5 % at two spiking levels. The prepared Fe 3 O 4 @MIPs possessed the advantages of high selectivity, straightforward preparation, facile separation and good reusability, and was highly suitable for the efficient extraction of amphetamine-type substances in complex environmental water.
研究领域:
环境科学
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分析化学
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PubMed
高影响因子
FOOD CHEMISTRY
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2021
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IF 7.514
Yue-Hong Pang,Zhi-Yang Lv,Ji-Cheng Sun,Cheng Yang,Xiao-Fang Shen
Metal-organic frameworks (MOFs), a sort of dispersive solid-phase extraction (d-SPE) material, has shown considerable prospects in the pretreatment of food, biological and other complex samples. Herein, we developed a method for compounding MOFs for d-SPE and trace determination of tetracyclines (TCs) in honey. When the compounding ratio of MIL-101 (Cr), MIL-100 (Fe) and MIL-53 (Al) was 7:1:2, adsorption–extraction was effective. Followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS), the limits of detection were 0.073–0.435 ng/g and the limits of quantitation ranged from 0.239 to 1.449 ng/g for oxytetracycline, tetracycline, chlortetracycline and doxycycline. The method was applied to four kinds of honey samples with recoveries from 88.1% to 126.2%. The compounding of MOFs provides a strategy for purification and multi-target extraction from complex food matrices by d-SPE.
研究领域:
分析化学
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食品安全
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DOI
高影响因子
GEODERMA
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2015
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IF 2.772
Meng Zhu,Chen Tu,Haibo Zhang,Yongming Luo,Peter Christie
A solvent extraction method coupled to high-performance liquid chromatography with tandem mass spectrometry detection (HPLC–MS/MS) was developed and validated for the simultaneous determination of soil diphenylarsinic acid (DPAA) and phenylarsinic acid (PAA). Several extraction solvents were evaluated with respect to the degree of soil extract-induced matrix effects and the recovery values for DPAA and PAA in the four studied soil matrices. Validation data showed that solvent extraction had a negligible impact on the accurate quantification of DPAA. In contrast, only with disodium hydrogen phosphate extraction did the method give both limited matrix effects (102–107%) with a coefficient of variation < 3% ( n = 4) and efficient recoveries (77–109%) at two spiking levels (20 and 50 mg kg − 1 ) for PAA. The selection of an appropriate extractant was the approach to reduce matrix effects while guaranteeing satisfactory recoveries of soil DPAA and PAA. Chromatographic separation was completed in 37 min and the analytes were detected in positive mode using selected reaction monitoring . MS/MS operating conditions were optimized for both electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) sources. Under optimal conditions the detection limit was 0.01 and 1.00 μg L − 1 for DPAA and PAA. The method detection limits (MDLs) obtained ranged from 2.52 to 3.42 μg kg − 1 for DPAA and from 0.23 to 0.33 mg kg − 1 for PAA depending on the soil types, and the intraday and interday precision was less than 5% for both analytes at two different concentrations. The method was successfully applied for the simultaneous determination of DPAA and PAA in one-month aged soils, satisfactory recoveries (> 74.03%) were obtained for both analytes. The results show that the proposed solvent extraction method coupled to HPLC–MS/MS analysis can provide accurate and reliable determinations of DPAA and PAA in soil samples.
研究领域:
环境科学
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分析化学
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高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 25
·2522-2530
·
IF 3.532
Ling-Juan Wang,Zhi-Wei Chen,Teng-Zhou Ma,Jiang Qing,Fang Liu,Zhou Xu,Ye Jiao,Shi-Hua Luo,Yun-Hui Cheng,Li Ding
In this study, a core–shell-structured magnetic metal–organic framework (MMOF) composite material (Fe3O4@UiO-66-NH2) was synthesized by the solvothermal method. It was employed as a new absorbent in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous detection of four aflatoxins (AFs) in rice. This method could shorten the pre-processing time by exploiting the advantageous characteristics of magnetic cores. The impurity was removed quickly. The effects of extraction solution, extraction time, adsorbent types, and amount of adsorbent on the extraction rate of target compounds were optimized. Under optimized conditions, AFs were validated and showed a good linear relationship within the 0.375–20 μg kg−1 concentration range (r2 > 0.9992). The limit of detection (LOD) was 0.0188–0.1250 μg kg−1 and the limit of quantification (LOQ) was 0.0375–0.3750 μg kg−1. At three spiking levels (0.375, 2, and 10 μg kg−1), the average recovery values for the four AFs ranged from 85.1% to 111.0%. The relative standard deviation ranged from 3.4% to 7.7%. The new method proved to be simple, fast, efficient, and suitable for the determination of AFs in rice samples.
研究领域:
食品科学
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分析化学
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DOI
PubMed
高影响因子
Chemical Engineering Journal Advances
·
2026
·
IF 6.9
Chaoying Zhang,Bohao Qi,Xin Hu,Jincheng Li,Yingchun Mu,Huan Liu
Sensitive determination of multiclass veterinary drug residues in aquaculture water requires efficient sample preparation capable of handling trace contaminants while minimizing sample consumption and manual operation. Here, a periodic magnetic actuation-assisted microfluidic enrichment platform was integrated online with HPLC–MS/MS for the determination of quinolones, sulfonamides, tetracyclines, and malachite green. Fe₃O₄@GO was magnetically confined within a multi-serpentine microchannel, and the effects of channel geometry and magnetic operating conditions on sorbent retention and flow-through capture were systematically evaluated. The multi-serpentine configuration limited Fe₃O₄@GO loss to 3.82% after ten operating cycles, while 200 mT and 10 Hz provided effective magnetic confinement and capture performance. In the final workflow, 50 μL of sample was loaded at 5 μL min⁻¹ for 10 min, followed by mobile-phase-mediated release and transfer through an online C 18 cleanup/trapping column for chromatographic analysis. The method achieved limits of detection of 0.02–0.17 μg L⁻¹, limits of quantification of 0.07–0.53 μg L⁻¹, recoveries of 79.84–97.66% in spiked real aquaculture water, and RSDs of 3.41–7.24%. These results demonstrate a low-volume and integrated sample-preparation strategy for multiclass veterinary drug determination in aquaculture-water matrices.
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高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Yuejiao Yang,Xitian Peng,Guiyou Chen,Huaming Xiao,Qiongwei Yu
Perfluorinated compounds (PFCs) are persistent in urban water systems, threatening the safety of drinking water and aquatic food chains. In this study, fluorinated loofah sponge (FLS) was prepared for selective solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination of 16 PFCs in urban water. The limits of detection (LODs) and limits of quantification (LOQs) of the established method (FLS-based SPE-LC-MS/MS) were 0.006–5 ng/mL and 0.01–10 ng/mL, respectively. This method exhibited a desirable precision with relative standard deviations (RSDs) less than 8.83 % and recoveries in the range of 85.4 %–107.2 %. Finally, this method was successfully applied to investigate the distribution of 16 PFCs in real urban water samples (such as tap water, bottled water, and lake water) collected in Wuhan, China, which enables sensitive dynamic monitoring of PFC migration in urban water networks and identification of potential sources so as to safeguard drinking water quality against emerging PFC contamination.
研究领域:
环境分析化学
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环境污染与控制
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水质安全
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分析化学
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环境健康
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DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Wenrui Li,Yike Dang,Ruihong Wang,Weizhong Jin,Xiangli Chen,Yafei Zhai,Zhuoqun Su,Guoliang Li
Fluoroquinolones (FQs) are widely used to treat various animal diseases. The high residue of veterinary drugs in animal-origin food are new pollutants that seriously threaten human health. In this work, Fe 3 O 4 @LDH/ZIF was prepared by the in situ growth of zeolitic imidazolium skeletons (ZIFs) on Fe 3 O 4 @Zn/Al-layered double hydroxides (Fe 3 O 4 @Zn/Al-LDH), which was used as the adsorbent of FQs for magnetic solid phase extraction (MSPE). The prepared materials were characterized by using FT-IR, XRD, TEM, SEM, VSM, zeta, and nitrogen adsorption-desorption analyses. Under the optimized conditions, the limit of detections (LODs) of proposed methods for FQs is determined as low as 0.1–0.6 μg·kg −1 with good linearity (R 2 ≥0.9972). Furthermore, the MSPE approach has been effectively utilized to extract of FQs from a range of meat varieties including fish, pork, chicken, bullfrog, and beef. The recoveries from the spiked samples ranged from 86.5 % to 107 %, with relative standard deviations (RSD) below 8.8 %. These results demonstrated that the prepared nanoparticles hold unique advantages for trace FQs analysis in foodstuffs. This study provides a magnetic adsorbent for food sample pretreatment, which can rapidly enrich compounds similar in structure to fluoroquinolones.
研究领域:
食品科学
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分析化学
·
纳米材料科学
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DOI
高影响因子
MOLECULES
·
2021
·Vol. 26
·期 11
·3344
·
IF 4.412
Shunyu Yao,Zixi Zhao,Wang Lu,Xin Dong,Jiye Hu,Xiaolu Liu
The chemical fungicide fludioxonil is widely used to control post-harvest fungal disease in cherries. This study was implemented to investigate the dissipation behaviours and residues of fludioxonil on cherries. A reliable and efficient analytical method was established. Cherry samples from four product areas were analyzed by QuEChERS and HPLC-MS/MS methods with acceptable linearity (R2> 0.99), accuracy (recoveries of 81–94%), and precision (relative standard deviation of 2.5–11.9%). The limits of quantification (LOQs) and limits of detection (LODs) of cherries were 0.01 mg/kg and 0.005 mg/kg. The dissipation of fludioxonil on cherries followed first order kinetics with half-lives of 33.7–44.7 days. The terminal residues of fludioxonil were all lower than 5.00 mg/kg, which is the MRL recommended by the European Commission. According to Chinese dietary patterns and terminal residue distributions, the risk quotient (RQs) of fludioxonil was 0.61%, revealing that the evaluated cherries exhibited an acceptably low dietary risk to consumers.Keywords:fludioxonil;cherry;HPLC-MS/MS;dissipation behaviour;residues;dietary risk assessment
研究领域:
食品科学
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农业化学
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毒理学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）