JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Jiaming Yuan,Jincai Wang,Zhixu Chen,Yuexiang Chang,Litong Chen,Zhizeng Gao,Jacques Crommen,Tingting Zhang,Zhengjin Jiang
In this study, a novel at-line nanofractionation platform was established for screening SARS-CoV-2 fusion inhibitors from natural products for the first time by combining HPLC-MS/MS with high-throughput fluorescence polarization (FP) bioassay. A time-course FP bioassay in 384 well-plates was conducted in parallel with MS/MS to simultaneously obtain chemical and biological information of potential fusion inhibitors in Lonicerae Japonicae Flos (LJF) and Lianhua Qingwen capsules (LHQW). Semi-preparative liquid chromatography and orthogonal HPLC separation were employed to enrich and better identify the co-eluted components. After comprehensive evaluation and validation, 28 potential SARS-CoV-2 fusion inhibitors were screened out and identified. Several compounds at low micromolar activity were validated by in vitro inhibitory assay, molecular docking, cytotoxicity test, and pseudovirus assay. Moreover, four potential dual-target inhibitors against influenza and COVID-19 were discovered from LJF using this method, offering novel insights for the development of future pharmaceuticals targeting epidemic respiratory diseases.
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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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Analytical Methods
·
2016
·Vol. 8
·期 6
·1405-1414
·
IF 1.915
Na Cao,Lei Liu,Yuan-bin Hao,Li-li Sun,Qiao-gen Zou,Xing-ling Ma,Kai-he Xiong
A sensitive, rapid and stable HPLC-MS/MS method has been developed and validated for the determination of rabeprazole enantiomers and their four metabolites, namely rabeprazole thioether, rabeprazole sulfone and desmethyl rabeprazole enantiomers, in beagle dog plasma using esomeprazole as the internal standard. The analytes and the internal standard were extracted from plasma samples by liquid–liquid extraction and separated on a Chiral-HSA column using acetonitrile-10 mmol L−1 ammonium acetate as the mobile phase by gradient elution. The method was validated with respect to sensitivity, specificity, linearity, precision, accuracy and especially the stability of analytes under various conditions, and was successfully applied in evaluating the pharmacokinetic profiles of racemic rabeprazole, the pure enantiomers and their metabolites in beagle dogs after single intravenous administration of (R)-rabeprazole sodium injection (at 0.33, 1 and 3 mg kg−1), (S)-rabeprazole sodium injection (at 1 mg kg−1) and racemic rabeprazole sodium injection (at 2 mg kg−1). The two enantiomers showed different profiles of pharmacokinetic parameters. The AUC0–t and t1/2 values of (R)-rabeprazole were higher and the clearance (CL) value of (R)-rabeprazole was lower than that of (S)-rabeprazole. Compared to (S)-rabeprazole, the higher absorption and slower elimination of (R)-rabeprazole explain why (R)-rabeprazole is more effective than the racemate.
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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
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分析化学
·
毒理学
·
药理学
·
临床研究
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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
·
材料科学
·
色谱学
·
毒理学
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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.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Yupeng Wen,Wendi Huo,Xinyuan Zhang,Yingchun Mu,Huan Liu,Chaoying Zhang,Lu Qiao,Jincheng Li
In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 1.0 to 50.0 μg/kg and a correlation coefficient > 0.99. The detection and quantification limits were 0.5 and 1–2 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 104.88 %, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2020
·
IF 2.34
Kai Cui,Xiaohu Wu,Lusheng Zhu,Ying Zhang,Gaochen Dai,Junli Cao,Jun Xu,Fengshou Dong,Xingang Liu,Yongquan Zheng
In this study, we established a rapid and sensitive HPLC-MS/MS method for quantitative determination of tembotrione and its metabolite AE 1417268 (M5) in corn, corn oil, beef, pork, chicken, and eggs. Both analytes eluted from a C18 column within 6 min. The electrospray ionisation–positive mode was used for tembotrione, whereas the negative mode was used for M5. Acetonitrile was the extractant for all samples, and the addition of 2 g NaCl to each homogenised sample facilitated the extraction of the analytes into acetonitrile. The extracted analytes were further purified by the addition of 50 mg of C18 sorbent (25 mg GCB was also added to corn samples) for subsequent HPLC-MS/MS analysis. Satisfactory calibration-curve linearities (R2 ≥ 0.997) were obtained for the two analytes at concentrations of 1–500 μg/L. Mean recoveries in different matrices ranged from 73.7% to 110.4%, whereas intra-day and inter-day relative standard deviations were <15% for all concentrations of spiked analytes. The limit of quantification was 2 μg/kg for each analyte in all matrices. In food samples obtained from markets, residual tembotrione and M5 were all below the limits of quantification. These results confirm that the method is suitable for the routine monitoring of residual tembotrione and M5 in a variety of food matrices.
研究领域:
食品科学
·
分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Rong-Fa Xu,Hang Mei,Li Chen,Bin Tang,Qi-Yuan Lu,Feng-Shan Cai,Xiao Yan,Jing Zheng,Xian-Tao Shen,Yun-Jiang Yu
Humans are widely and concurrently exposed to volatile organic compounds (VOCs) and polycyclic aromatic hydrocarbons (PAHs). However, few studies have reported the internal co-exposure levels of these chemicals in occupational and general populations. Specifically, the associations revealed between the urinary levels of metabolites of VOCs (mVOCs), hydroxylated PAHs (OH-PAHs), and oxidative stress biomarkers for humans remain limited. In this study, a method based on solid-phase extraction (SPE) and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous analysis of 22 mVOCs, 12 OH-PAHs, and 8-hydroxy-2′-deoxyguanosine (8-OHdG) in human urine samples. The method was validated with all target analyte accuracies and precisions in the range of 76 %–120 % and 1 %–14 % at three levels of spiked urine samples, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the target analytes were 0.01–0.34 ng/mL and 0.01–7.57 ng/mL, respectively. And the method was applied to measure urinary levels of target analytes from 38 petrochemical workers in Guangzhou, South China. Except for 3-hydroxy-benzo[a]pyrene, all target analytes were detected in the urine samples. The average levels were 0.05–12.6 ng/mL for individual OH-PAHs, 0.20–73620 ng/mL for individual mVOCs, and 1.00 ng/mL for 8-OHdG. Additionally, 3-hydroxy-phenanthrene, 1-hydroxy-pyrene, 6-hydroxy-chrysene, N-acetyl-S-(trichlorovinyl)-L-cysteine, 2-methylhippuric acid, thiodiacetic acid, trans, trans -Muconic acid, and N-acetyl-S-(3,4-dihydroxybutyl)-L-cysteine had statistically significant positive effects on 8-OHdG levels, while 1-hydroxy-naphthalene, 1,2-dihydroxybenzene, and hippuric acid showed a negative effect on 8-OHdG, indicating these metabolites could lead to synergistic or antagonistic oxidative DNA damage. This study provides a robust analytical method that permits a comprehensive assessment of co-exposure to PAHs and VOCs and their potential adverse health effects.
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ANALYTICAL LETTERS
·
2022
·
IF 2.267
Xu-Feng Wang,Qiang Wang,Jin-Lan Yang,Dong-Hao Zhao
An amino-modified multiwalled carbon nanotube (MWCNT) solid-phase extraction-based hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC–MS/MS) method was developed for simultaneous determination of 13 paralytic shellfish toxins (PSTs) in bivalve mollusks. Shellfish samples were extracted with 1% acetic acid followed by cleanup using optimized MWCNT-NH2 based solid-phase extraction. Absorbed PSTs were eluted with 2 mL 1% acetic acid–acetonitrile (70/30, v/v). The separation was performed on a Waters BEH Amide column within 7.5 min utilizing 0.1% formic acid–acetonitrile and 2 mM ammonium acetate containing 0.1% formic acid as the mobile phase. The analytes were quantified by matrix-matched external standard curves with correlation coefficients® exceeding 0.997 acquired in multiple reaction-monitoring mode. The limits of detection and quantitation in shellfish samples were from 2.76 to 9.8 μg/kg and 9.11 to 39.3 μg/kg, respectively. Recoveries at three spiked levels ranged from 71.4% to 97.8% with relative standard deviations less than 12.6%. The developed method was satisfactorily applied to the analysis of shellfish.
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JOURNAL OF HAZARDOUS MATERIALS
·
2024
·
IF 12.2
Jinling Pang,Hongzhe Chen,Huige Guo,Kunning Lin,Shuyuan Huang,Beichen Lin,Yuanbiao Zhang
Microplastics (MPs) act as carriers for organic pollutants ( e.g. antibiotics) and microorganisms ( e.g. bacteria) in waters, leading to the proliferation of antibiotic resistance genes. Moreover, the antibiotics adsorbed on MPs may exacerbate this process. For further research, it is necessary to understand the types and amounts of antibiotics adsorbed on MPs. However, due to the heavy work of MPs collection and sample pretreatment, there is a lack of analytical methods and relevant data. In this study, an in-tube solid phase microextraction (IT-SPME) on-line coupled to HPLC-MS/MS method based on amorphous precursor polymer of three-dimensional covalent organic frameworks/monolith-based composite adsorbent was developed, which could efficiently capture, enrich and analyze tetracycline (TCs) antibiotics. Under the optimal extraction parameters, the developed method was capable of detecting TCs at levels as low as 0.48–1.76 pg. This method was applied to analyze the TCs adsorbed on MPs of different particle sizes in mariculture water for the first time, requiring a minimum amount of MPs of only 1 mg. Furthermore, it was observed that there could be an antagonistic relationship between algal biofilm and TCs loaded on MPs. This approach could open up new possibilities for analyzing pollutants on MPs and support deeper research on MPs.
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危险品化学品经营许可证（带存储）