MICROCHIMICA ACTA
·
2023
·Vol. 190
·期 10
·1-13
·
IF 5.7
Bian Yu,Zhang Yuan,Liu Tong,Zhang Feng,Gao Hui-yuan
A novel imine-linked magnetic covalent organic polymer, Fe 3 O 4 @TAB-TFPT, was synthesized using environmentally friendly deep eutectic solvents as the reaction medium instead of conventional organic solvents. The materials were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), FT-IR, N 2 adsorption-desorption isotherms, energy dispersive spectrometer (EDS), X-ray photoelectron spectra (XPS), and thermo gravimetric analysis (TGA). Subsequently, the materials were employed as an adsorbent for magnetic solid-phase extraction (MSPE) of flavonoids, including Kurarinone, Norkurarinone, Xanthohumol, and Isoxanthohumol, prior to their determination by HPLC–MS/MS. The validation results demonstrate good linearity within the concentration range 0.1–1000 ng∙mL −1 ( R 2 ≥ 0.9963), high enrichment factors ranging from 18.9 to 30.7, and low LODs (0.01–0.05 ng∙mL −1 ) and LOQs (0.05–0.1 ng∙mL −1 ). Furthermore, recoveries between 80.60% and 108.40% with relative standard deviations ≤ 8.49% were achieved. The proposed MSPE-HPLC–MS/MS method was successfully applied to the determination of flavonoids in Sophora flavescens Aition sample. Graphical Abstract
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Frontiers in Environmental Science
·
2022
·
IF 5.411
Wang Siwei,Sun Haibin,Liu Yanping,Wang Xiaonan,Chang Hong
A modified-QuEChERS method to determine kresoxim-methyl in banana and soil was developed and validated via high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). The dissipation behavior, residue distribution, and risk assessment of kresoxim-methyl in banana were further investigated based on this method. The dissipation behavior of kresoxim-methyl in banana and soil was described by using first-order kinetics and its half-life, 4.8–5.7 days and 5.5–6.5 days, respectively. The concentrations of kresoxim-methyl were 0.03–0.08 mg kg−1, 0.06–0.17 mg kg−1, and <0.01 mg kg−1 for a whole banana, peel, and pulp, respectively, on the basis of spraying three times the recommended dosage and pre-harvest interval (PHI, 42 days). The results showed that the risk quotient of kresoxim-methyl in banana to people exhibited an acceptable low dietary risk. This current study could help in guiding the scientific and proper usage of this formulation.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 11
·1-8
·
IF 5.479
Jiang Yanxiao,Ma Pinyi,Piao Huilan,Qin Zucheng,Tao Shuo,Sun Ying,Wang Xinghua,Song Daqian
Cellulose paper was coated with the metal-organic framework MIL-101(Cr) in a chitosan matrix and utilized for thin-film microextraction (TFME). The coated paper possesses excellent extraction efficiency for the triazine herbicides atraton, desmetryn, secbumeton, prometon, ametryn, dipropetryn, and dimethametryn. High-performance liquid chromatography-tandem mass spectrometry was applied to quantify target analytes. The effects of mass ratio of MIL-101(Cr) to chitosan, sample pH value, time of adsorption and desorption, and type and volume of desorption solvent on extraction efficiency were optimized. Under the optimal conditions, the method has limits of detection between 1.5 and 22 ng·L −1 . The recoveries of triazines from spiked tap water, drinking water, lake water and river water range from 77.0 to 125.3%, with relative standard deviations of <17.4%.
Cellulose paper was modified with metal-organic framework MIL-101(Cr)/chitosan by using a simple, efficient and environmentally friendly approach. The modified cellulose paper was then used as a novel extraction phase in thin-film microextraction (TFME).
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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
·
分析化学
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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
·
分析化学
·
环境科学
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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.
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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.
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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
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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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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.
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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
·
材料科学
·
食品科学
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ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Chen-Yu Xue,Ya-Hong Liu,Yue Yu,Ying Liu,Ying-Lin Zhou,Xin-Xiang Zhang
The apurinic/apyrimidinic (AP) site is an important intermediate in the DNA base excision repair (BER) pathway, having the potential of being a biomarker for DNA damage. AP sites could lead to the stalling of polymerases, the misincorporation of bases and DNA strand breaks, which might affect physiological function of cells. However, the abundance of AP sites in genomic DNA is very low (less than 2 AP sites/10 6 nts), which requires a sensitive and accurate method to meet its detection requirements. Here, we described an ultrasensitive quantification method based on a hydrazine- s -triazine reagent (i-Pr 2 N) labeling for AP sites combining with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The limit of detection reached an ultralow level (40 amol), realizing the most sensitive MS-based quantification for the AP site. To guarantee the accuracy of the quantitative results, the labeling reaction was carried out directly on DNA strands instead of labeling after DNA enzymatic digestion to reduce artifacts that might be produced during the enzymatic process of DNA strands. And selective detection was realized by MS to avoid introducing the false-positive signals from other aldehyde species, which could also react with i-Pr 2 N. Genomic DNA samples from different mammalian cell lines were successfully analyzed using this method. There were 0.4–0.8 AP sites per 10 6 nucleotides, and the values would increase 16.1 and 2.75 times when cells were treated with genotoxic substances methyl methanesulfonate and 5-fluorouracil, respectively. This method has good potential in the analysis of a small number of cell samples and clinical samples, is expected to be useful for evaluating the damage level of DNA bases, the genotoxicity of compounds and the drug resistance of cancer cells, and provides a new tool for cell function research and clinical precise treatment.
研究领域:
分子生物学
·
分析化学
·
毒理学
·
药理学
·
临床研究
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