MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 10
·4091-4098
·
IF 4.58
Liu Haochi,Chen Ligang,Ding Jie
The authors describe an efficient method for the extraction of tetracycline antibiotics (TCs) from water samples by using a new kind of core-shell adsorbent. It consists of a magnetite (Fe 3 O 4 ) core and a metal-organic framework (type ZIF-8) as the shell. The sorbent has a large specific surface and superparamagnetic response. The sorbent was characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, nitrogen adsorption, and X-ray diffraction. The adsorption isotherms, dynamic adsorption, and mechanisms of interactions between tetracycline and sorbent were studied. Various parameters affecting the extraction efficiency were optimized. Following desorption of the TCs with methanol (containing 1% of acetic acid), they were quantified by using ultra-high performance liquid chromatography combined with mass spectrometry. The method has a linear range that extends from 0.5 to 50 ng·L −1 , and the limits of detection for tetracycline, chlortetracycline, and oxytetracycline are 0.125, 0.122 and 0.143 ng·L −1 , respectively. The relative standard deviations of intra-day and inter-day assays range from 3.3% to 8.5%, and from 2.8% to 8.3%, respectively. The recoveries of TCs (at spiking levels of 0.5, 5.0 and 50 ng·L −1 ) are in the range between 78.3% and 93.7%. The method was successfully applied to the determination of TCs in spiked river water, fish pond water, and livestock wastewater.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2025
·
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.
研究领域:
食品科学
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分析化学
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环境科学
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2715-2721
·
IF 4.58
Wang Chenlu,Zhou Wei,Liao Xiaoyan,Zhang Wenpeng,Chen Zilin
Polyether ether ketone (PEEK) is an ideal substrate for in tube solid-phase microextraction (SPME) because it overcomes the shortcomings of conventional silica fibers in terms of fragility and poor flexibility. Commonly used bare PEEK tubes suffer from difficult modification with selective sorbents and low inner surface areas. This problem was solved by etching with concentrated sulfuric acid, which dissolves the amorphous regions of the PEEK surface and yields a rough inner surface with plenty of microscopically small holes. The etched tube was then stepwise functionalized with polydopamine and graphene oxide which was in-situ immobilized. The modified tube displays excellent efficiency for the extraction of positively charged quaternary alkaloids by a mixed-mode extraction. Enrichment factors from 221 to 275 can be obtained for the extraction of the alkaloids jatrorrhizine, palmatine and berberine. The alkaloiods were then quantified by online SPME-HPLC-MS/MS detection. The method has detection limits of 0.1 pg mL −1 , good linearity, and good intra-day reproducibility (≤ 2.4%). It was applied to the analysis of the three alkaloids in Cortex Phellodendri herb and rat plasma after oral administration.
A concentrated sulfuric acid etching method was used for enhance the workability of polyether ether ketone tube (PEEK) in solid phase microextraction (SPME). The etched tube was covered with graphene oxide (GO) for extraction of protoberberines.
研究领域:
分析化学
·
药学
✓ 已验证
产品关联
DOI
高影响因子
Drug Design Development and Therapy
·
2020
·
IF 3.216
Hao-Zhen Zheng,Xiao Shen,Ying-Ying He,Xiang-Li Yan,Sheng-Xin Wang,Ai-Ming Yu,Li-Sheng Wang
Objective The aim of our research was to analyze and compare the pharmacokinetics of paeoniflorin, calycosin, calycosin-7-o-β-d-6-glucoside, and 6-gingerol in the blood and brain tissue of normal and cerebral ischemia-reperfusion injury rats by HPLC-MS/MS method.Methods The blood and brain tissue samples of normal and middle cerebral artery occlusion (MCAO) rats were compared. The blood and brain tissue samples were collected by using microdialysis technique. The concentrations of paeoniflorin, calycosin, calycosin-7-o-β-d-6-glucoside, and 6-gingerol in blood and brain tissues were determined by the HPLC-MS/MS internal standard method.Results Compared with the normal group, the model group after the administration of the Huangqi Guizhi Wuwu Decoction showed that Cmax blood, AUC0-t blood, and AUC0-inf blood of paeoniflorin were increased, CLblood, t1/2 brain, and Vbrain of paeoniflorin were decreased; Cmaxblood, AUC0-tblood, AUC0-infblood, and average residence time (MRTbrain) of calycosin-7-o-β-d-6-glucoside were decreased and the CLblood and Cmax brain of calycosin-7-o-β-d-6-glucoside were increased; Cmax blood of calycosin was decreased, Vblood and Vbrain of calycosin were increased; Cmax blood, AUC0-t blood, AUC0-inf blood, and MRTbrain of 6-gingerol were decreased, CLblood of 6-gingerol was increased.Conclusion This method is simple, rapid, and sensitive. It is suitable for the pharmacokinetic study of Huangqi Guizhi Wuwu Decoction in the blood and brain tissue of rats. Cerebral ischemia-reperfusion injury increased the content of paeoniflorin, calycosin, calycosin-7-o-β-d-6-glucoside, and 6-gingerol in the blood, affecting the clearance rate of paeoniflorin in the brain, the detention time of calycosin-7-o-β-d-6-glucoside and the 6-gingerol in the brain. In normal and cerebral ischemia-reperfusion rats, the content of paeoniflorin and 6-gingerol in the blood was higher than that in brain tissue, while the content of calycosin, calycosin-7-o-β-d-6-glucoside in the brain tissue was higher than that in blood, suggesting that calycosin and calycosin-7-o-β-d-6-glucoside have brain targeting properties.
研究领域:
中药学
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药理学
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神经科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2021
·Vol. 44
·期 11
·2269-2278
·
IF 3.645
Xuelei Chen,Wei Li,Jingguang Li,Sai Fan,Zhixiong Shi
Organophosphorus flame retardants are a class of widely used plasticizers and flame retardants. In this study, an analytical methodology for the simultaneous determination of 13 organophosphorus flame retardants in milk was developed by using high-performance liquid chromatography-tandem mass spectrometry in combination with a modified quick, easy, cheap, effective, rugged, and safe technique and solid-phase extraction. The experimental parameters of the sample purification procedure and high-performance liquid chromatography-tandem mass spectrometry were optimized. The developed method was validated in terms of linearity, limits of detection, recovery, and precision. The method showed a linear response in the 1–100 ng/mL concentration range and the limits of detection ranged from 0.001 to 0.3 ng/mL. The mean recoveries for most organophosphorus flame retardants were in the ranges of 75.0–115.8% (spiked at 2.5 ng/mL) and 76.7–124.8% (spiked at 25 ng/mL), with relative standard deviations of <13.09%. The developed methodology was successfully applied to the analysis of nine human milk samples and nine commercial cow milk samples. Eleven organophosphorus flame retardants were detected in the human milk samples, with median concentrations that ranged from lower than the limit of detection to 1.47 ng/mL, and only nine organophosphorus flame retardants were detected in cow milk samples, with median levels of <0.32 ng/mL.
研究领域:
分析化学
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食品安全
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环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2021
·
IF 7.514
Meng-Jun Li,Na Li,Guiju Xu,Ling-Xi Zhao,Xiangfeng Chen,Yanfang Zhao,Ru-Song Zhao
A novel magnetic boron nitride nanosheets (Fe 3 O 4 @BNNSs) composite-based magnetic solid-phase extraction (MSPE) method was employed to analyse six plant growth regulators (PGRs) in tomatoes combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The novel Fe 3 O 4 @BNNSs composite was prepared via an in situ chemical coprecipitation process and characterized by scanning electron microscopy (SEM), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and vibrating sample magnetometry (VSM). Several factors that may affect the extraction efficiencies were optimized. Under the optimal factors, low limits of detection (0.002–0.010 ng g −1 ), good linear ranges (0.05–10 ng g −1 ) and satisfactory precisions (intra-day: 1.2%-3.9%; inter-day: 2.1%-6.9%) were achieved. The established approach was successfully employed to extract and determine PGRs in tomatoes, and the spiked recoveries were between 85.2 and 109.0%.
研究领域:
分析化学
·
纳米技术
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食品科学
·
农业化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Rujia Shen,Lijin Huang,Ruiqi Liu,Qin Shuai
In this work, hierarchical porous covalent organic frameworks (HP-COFs) foam, named as HP-TpBD, was prepared by using 1,3,5-trimethylphloroglucinol (Tp) and benzidine (BD) as building blocks under the assistant of NaCl template. Its potential application as the sorbent for solid phase extraction (SPE) of sulfonamides (SAs) in meat products were explored by coupling with high performance liquid chromatography-mass spectrum (HPLC-MS) analysis. The key factors affecting extraction efficiency were well studied. Under the optimum conditions, the proposed method exhibited high preconcentration factors of 100, low limit of detection (0.10-0.23 μg/kg), and wide linear ranges (0.5-200 μg/kg). In addition, the determination of SAs in real samples were realized with satisfactory recoveries (82.8-119.9%), demonstrating the applicability of the proposed method. The easy operation, superior extraction affinity and good recycle performance demonstrated the resulting HP-COF foam is a promising adsorbent for the preconcentration of trace organic compounds from complex matrix.
研究领域:
分析化学
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食品科学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Yutao Lou,Mengting Cheng,Qin Cao,Kening Li,Hui Qin,Meihua Bao,Yuan Zhang,Sisi Lin,Yiwen Zhang
Mirabegron and vibegron, both newly identified beta-3 adrenergic agonists, have significantly improved the quality of life for patients suffering from overactive bladder. In order to comprehensively assess the plasma exposure levels of these agents, the development of a rapid and highly sensitive bioanalytical method becomes imperative. The primary objective of this study was to establish a robust high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the concurrent quantification of mirabegron and vibegron in human plasma. The analytes were extracted from a 100 μL plasma sample through protein precipitation, employing 300 μL of methanol. Subsequently, samples underwent separation and quantification using a Waters XBridge C 18 column (2.1 × 100 mm, 3.5 µm), with a mobile phase consisting of 0.1% formic acid in water and 0.1% formic acid in acetonitrile. The mass analysis was conducted using positive electrospray ionization (ESI+) operated in a multiple reaction monitoring (MRM) mode. The proposed method was meticulously validated in accordance with the guidelines set forth by the U.S. Food and Drug Administration (FDA) for bioanalytical method validation. The regression equations demonstrated exceptional linearity for both mirabegron (r² ≥ 0.994) and vibegron (r² ≥ 0.996) across the concentration range of 0.5 – 200 ng/mL. Furthermore, the assay exhibited accuracy (inter-day relative error ≤ 6.90%) and precision (inter-day coefficient of variation ≤ 8.88%). The average recoveries of the analytes were found to range from 81.94% to 102.02%, with mean matrix effects falling within the range of 89.77% to 110.58%. As a result, this method was deemed highly suitable for the precise determination of the concentrations of both mirabegron and vibegron in the context of therapeutic drug monitoring and bioequivalence studies.
研究领域:
药理学
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临床医学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2025
·
IF 13.2
Yichan Huo,Xiong Wang,Yang Yi,Zhirong Yang,Wenchang Wang,Huaijie Yao,Pingping Liu,Wenfen Zhang,Shusheng Zhang
p -Phenylenediamine antioxidants (PPDs) and their quinone derivatives (PPDQs) have emerged as concerning environmental contaminants due to their widespread presence and biological toxicity. Herein, a novel tetraazacalix[2]arene[2]triazine functionalized 2D transition metal carbide (TCT@MXene) with electron-rich and electron-deficient sites, porous structures, abundant adsorption sites was first synthesized and characterized. Combining the advantages of extraordinary adsorption capacities and rates towards PPDs and PPDQs, a dispersive solid-phase extraction coupled with high-performance liquid chromatography-mass spectrometry (HPLC-MS/MS) strategy was developed for highly sensitive and selective determination of PPDs and PPDQs in environmental water. The method featured acceptable linearity (R 2 ≥ 0.999), high sensitivity (LOD ranged from 0.10 to 2.96 ng L −1 ), and qualified precision (RSD ≤ 5.90 %). Compared with published works, the LODs of the developed technique were improved 3.8–250 times. Furthermore, its exceptional thermal and chemical stability allows for at least 10 reuse cycles under varying pH conditions. The adsorption mechanism revealed that the complementary charge distribution and robust conjugated system of TCT@MXene enabled the simultaneous and efficient co-adsorption of both PPDs and PPDQs. Besides, the established method was successfully applied to the analysis of trace targets in Yellow River basin in Henan Province. All these results proved the promising application of the developed method for organic pollutants analysis in water samples.
研究领域:
环境科学
·
分析化学
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材料科学
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色谱学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Xiaofan Wang,Xu Zhao,Liqiang Gu,Chunxiao Lv,Bosai He,Zhenzhen Liu,Pengyi Hou,Kaishun Bi,Xiaohui Chen
A simple and rapid ultra-high performance liquid chromatography–tandem mass spectrometry (uHPLC–MS/MS) method has been developed for the simultaneous determination of five free flavonoids (amentoflavone, isorhamnetin, naringenin, kaempferol and quercetin) and their total (free and conjugated) forms, and to compare the pharmacokinetics of these active ingredients in normal and hyperlipidemic rats. The free and total forms of these flavonoids were extracted by liquid–liquid extraction with ethyl acetate. The conjugated flavonoids were deconjugated by the enzyme β-Glucuronidase and Sulfatase. Chromatographic separation was accomplished on a ZORBAX Eclipse XDB-C 8 USP L7 column using gradient elution. Detection was performed on a 4000Q uHPLC–MS/MS system from AB Sciex using negative ion mode in the multiple reaction monitoring (MRM) mode. The lower limits of quantification were 2.0–5.0 ng/mL for all the analytes. Intra-day and inter-day precision were less than 15% and accuracy ranged from −9.3% to 11.0%, and the mean extraction recoveries of analytes and internal standard (IS) from rat plasma were all more than 81.7%. The validated method was successfully applied to a comparative pharmacokinetic study of five free and total analytes in rat plasma. The results indicated that the absorption of five total flavonoids in hyperlipidemia group were significantly higher than those in normal group with similar concentration–time curves.
研究领域:
药物分析
·
药理学
·
临床医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
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
·
食品科学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）