CHEMICAL ENGINEERING JOURNAL
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2026
·
IF 12.5
Yanmei Shi,Liqin Chao,Xiaobing Liu,Zhihong Chen,Zhenghui Chang,Sisen Zhang,Shusheng Zhang,Kai Hu
Development of advanced in vivo sampling tools for the synchronous monitoring of drugs and endogenous biomarkers is critical for integrated pharmacokinetic-pharmacodynamic (PK-PD) studies. Herein, a novel solid-phase microextraction (SPME) fiber coating was engineered based on a zwitterionic covalent organic framework (EB-TTB-DABSA COF), strategically functionalized with sulfonate and quaternary ammonium groups. This rationally designed coating provides synergistic electrostatic, π–π, and hydrophobic interactions, enabling the efficient and simultaneous extraction of both cationic alkaloids and neurotransmitters. Coupled with LC-MS/MS, the developed platform achieved highly sensitive (limits of detection down to 3.3 × 10 −3 ng·mL −1 ), minimally invasive, and synchronous monitoring of these analytes in paired blood and brain matrices of living rats. Application in a Parkinson's disease (PSD) model revealed altered pharmacokinetics of Coptis chinensis alkaloids, including significantly increased area under the curve (AUC) values ( p < 0.01) and prolonged elimination half-lives compared to controls. These findings indicate enhanced systemic absorption and improved bioavailability of alkaloids under PSD conditions. Crucially, pharmacodynamic analysis showed that alkaloid administration triggered a synchronized restoration of key depleted neurotransmitters in PSD brains. A correlation with a characteristic hysteresis pattern further established a delayed neuroprotective relationship between alkaloid concentrations and neurotransmitter levels. This study not only introduces a robust zwitterionic COF-SPME platform for concurrent in vivo biosampling but also provides the first quantitative neuropharmacological perspective on Coptis chinensis alkaloids, offering a foundational framework for mechanistic research and therapeutic development in PSD.
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FOOD CHEMISTRY
·
2022
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IF 9.231
Xiaoli Guo,Tingze Ren,Jianchun Ji,Yan Yang,Xin Di
In this work, a combination of QuEChERS and dispersive micro-solid phase extraction (D-μ-SPE) based on dissolvable layered double hydroxide (LDH) has been established for preconcentration and enrichment of sulfonylurea herbicides (SUHs) in wolfberry samples. The QuEChERS was used for extraction and purification of SUHs, followed by D-μ-SPE for further enrichment of targeted analytes to obtain superior extraction performance. Dissolvable LDH nanosheets were used as absorbents, thus eliminating the elution step needed in traditional D-μ-SPE. The main influence experimental variables including pH of sample solution, amount of LDH, vortex time and volume of acidic solution were optimized in detail. Under the optimized conditions, the proposed method shows high precision (RSDs < 12 .7%), low limits of detection (0.01–0.5 ng/g) and limits of quantitation (0.1–2.0 ng/g), acceptable recovery (80.1%–97.1%), thus making it a good alternative analytical strategy for the determination of SUHs residues at the low nanogram per gram range with desirable sensitivity.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 413
·期 7
·1799-1807
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IF 4.157
Ouyang Zhonghua,Huang Jing,Ren Yi,Li Huanhuan,Ding Yao,Zhang Ke,Jiang Lei,Yu Peng
High-dose methotrexate (HDMTX) combined with leucovorin (LV) is the first-line drug therapy for many kinds of malignant tumors. However, the specific treatment plans, such as dosage and duration of administration, are usually formulated according to the clinician’s experience and therapeutic drug monitoring (TDM) of methotrexate in patients’ plasma, which are responsible for strong individual differences of drug usage. A large number of studies have shown that methotrexate targets the inside of the cell. The key cytotoxic component is the methotrexate polyglutamates (MTXPGs) in the cell. The concentration of methotrexate in plasma does not reflect the efficacy and side effects well. Based on mass spectrometry technology, we developed and validated an accurate, sensitive, and stable method to quantify the intracellular MTX (MTXPG 1 ) and its metabolites MTXPG 2–7 simultaneously. The lower limit of quantification was 0.100 ng/ml, and the run time was only 3 min. Moreover, our team has already developed two LC-MS/MS-based methods to respectively quantify methotrexate in plasma samples and two key proteins (γ-glutamyl hydrolase [GGH] and folylpolyglutamate synthetase [FPGS]) in peripheral blood mononuclear cells (PBMC). Through these highly sensitive and accurate approaches, we have gained a deep understanding of the whole pharmacokinetic process of MTX and explored the key factors affecting the accumulation process of intracellular active components (MTXPGs). Based on this research, it is possible to find a more effective way to provide an accurate reference for clinical drug use than traditional therapeutic drug monitoring (TDM).
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
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IF 3.4
Mingxia Liu,Jing He,Canjun Ruan,Weigang Pan,Peixian Mao,Zuoli Sun,Gang Wang,Jian Yang
D -amino acids may be indicators of late-life depression but separation and quantification of enantiomers which differ only by optical rotation sign remain challenging due to their identical physical and chemical properties. A convenient LC-MS/MS method was developed for the simultaneous measurement of l - and d -amino acids based on the chiral derivatization reagent, N α -(5-fluoro-2,4-dinitrophenyl)- L -leucinamide, and conventional octadecylsilane reversed-phase column. Methanol was used as the extraction solvent and a single-step derivatization reaction using volatile triethylamine eliminated the requirement for desalination prior to LC-MS/MS. Simultaneous separation and identification of 21 amino acids and the enantiomeric compositions of the 18 chiral proteogenic entities were achieved. Low limits of detection (0.03–4.0 nM), wide linear range (0.01–20 μM), good precision (RSDs < 10 %) and negligible matrix effects indicated the suitability of the method. Application of the method to the quantification of serum chiral amino acids in late-life depression patients (n = 40) and controls (n = 35) found a total of 17 L -amino acids, 14 D -amino acids, D L -asparagine, glycine and γ-aminobutyric acid. The statistical evaluation showed significant differences of glycine, L -threonine and D -methionine between late-life depression patients and controls, indicating that these are potential biomarkers of late-life depression.
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Analytical Methods
·
2018
·Vol. 11
·期 4
·507-516
·
IF 2.073
Chang Liu,Diandian Deng,Di Xu,Kang Wu,Hong Yang,Kang Zhao,Jianguo Li,Anping Deng
In this study, a monoclonal antibody (mAb)-based enzyme-linked immunosorbent assay (ELISA) for the determination of chloramphenicol (CAP) in shrimp, feed and milk samples was developed and validated by LC-MS/MS coupled with immunoaffinity clean-up (LC-MS/MS-IAC). Three immunogens were synthesized and used to immunize mice. Spleen cells from the immunized mice with the highest titer were selected for cell fusion. Two lines of hybridoma cells (1B1 and 2D2) secreting specific antibodies against CAP were successfully screened. Under optimal conditions, the values of the 50% inhibitory concentration (IC50) and limit of detection (LOD) of the ELISA in phosphate-buffered saline (PBS) based on 2D2 mAb for the detection of CAP were 0.46 ng mL−1 and 0.06 ng mL−1, respectively. There was no cross-reactivity (CR) of the ELISA with other antibiotics (florfenicol, thiamphenicol, etc.). Shrimp, feed and milk samples were spiked with different contents of CAP and detected by ELISA. The recoveries and coefficients of variation (CVs) of the ELISA for CAP from three spiked samples were 80.6–116.0% and 5.5–15.4% (n = 3), 96.2–111.0% and 7.0–13.5% (n = 3), and 79.7–109.8% and 5.8–13.3% (n = 3), respectively. As the CAP concentrations in spiked samples measured by LC-MS/MS coupled with solid phase extraction (LC-MS/MS-SPE) were significantly lower than those measured by ELISA, we established an immunoaffinity clean-up (IAC) for CAP by covalently immobilizing our mAb against CAP on the CNBr-activated Sepharose-4B gel and directly mixing the mAb-immobilized gel with the spiked samples sufficiently. The recoveries of CAP from the spiked samples measured by LC-MS/MS-IAC were 78.6–106.7% with the CV less than 11.1% (n = 3).
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Xinran Cui,Yongbin Wang,Yan Zhan,Xiaoyan Chen
Dimethoxyethyl phthalate (DMEP) is an industrial phthalates reagent exposed to human body. Its hydrolytic metabolite ethylene glycol methyl ether (EGME) and further oxidative metabolite methoxyacetic acid (MAA) have reproductive and developmental toxicity, and the latter is more toxic than the former. However, due to the lack of sensitive and reliable analytical method, the in vivo clearance and biotransformation of EGME and MAA is poorly understood. In order to evaluate their toxicokinetic profiles, a precolumn derivatization liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous determination of EGME and MAA in rat plasma. After a simple protein precipitation procedure, the sample was derivatized with p -toluene sulfonyl isocyanate (PTSI) and 4-bromo- N -methylbenzylamine (4-BNMA), separated by gradient elution on HSS T3 column, and detected by electrospray ionization (ESI) source in positive multiple reaction monitoring (MRM) mode. The results of the method validation showed that EGME had good linearity in the range of 2.00–400 ng/mL and MAA in the range of 5.00–1000 ng/mL. The intra- and inter-day accuracy and precision were within acceptable limits ( ± 15 %) at all concentrations. This validated method was successfully applied to characterize the toxicokinetics of EGME and MAA in rats following a gavage administration of 50 mg/kg DMEP.
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FITOTERAPIA
·
2018
·
IF 2.642
Hong-Bo Xu,Tong-Hua Yang,Pei Xie,Zhi-Shu Tang,Xiao Song,Huai-Li Xu,Yan-Hong Li,Dong-Bo Zhang,Yan-Ru Liu,Yan-Ni Liang,Yu Zhang,Shi-Jun Liu,Si-Min Wei,Chen Sun,Hong-Bo Liu,Chong Deng,Wei Wang
Gracilistones A ( 1 ) and B ( 2 ), two new eudesmane-type sesquiterpenoids with an unusual tetrahydrofuran-fused 6/6/5 tricyclic ring system, were obtained from Acanthopanax gracilistylus under the guidance of LC-MS investigation. Their structures and absolute configurations were assigned by extensive spectroscopic analyses and quantum calculation methods. Compounds 1 and 2 showed potent inhibitory activity against LPS-induced nitric oxide production in RAW 264.7 macrophages, compared with the positive control L-NMMA. In addition, compounds 1 and 2 were also evaluated for their antioxidant (DPPH • and ABTS •+ ) and xanthine oxidase (XO) inhibitory activities, and they exhibited weak inhibitory effects at 100 μM.
研究领域:
药用植物学
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药物化学
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炎症研究
·
天然产物化学
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Biochemistry and Biophysics Reports
·
2026
·
IF 3.3
Wenyuan Wan,Yuntao Zhang,Xiaotong Yang,Jinyao Li,Jun Lu,Yu Zhao
This study investigated the reparative effects of Brassica rapa L. ethanolic extract (BREE) on H 2 O 2 -induced oxidative injury in PC-12 cells. Brassica rapa L. , a cruciferous plant rich in bioactive flavonoids, exhibits potent antioxidant and neuroprotective properties against oxidative stress, a key pathological driver in neurodegenerative diseases. This study investigated the reparative effects of Brassica rapa L. ethanolic extract (BREE) on H 2 O 2 -induced oxidative injury in PC-12 cells, employing a multi-omics approach integrating LC-MS/MS metabolite profiling, molecular docking, and transcriptomic validation. BREE demonstrated robust radical-scavenging activity. Molecular docking identified direct interactions among flavonoids within BREE, suggesting a role in redox modulation. Subsequent experiments confirmed the activation of the PI3K/Akt, Keap1-Nrf2, and cell cycle pathways. Functionally, BREE significantly restored cell viability to 162.3% ± 6.9% of that in the control group. These findings validate BREE's dual action in scavenging ROS and reprogramming redox signaling networks, positioning it as a candidate for combating oxidative stress-associated neurodegeneration and as a potential functional food for age-related cognitive decline.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Hong Pan,Yi Li,Linyan Huang,Xumei Zhou,Yuanfu Lu,Fuguo Shi
Arecoline is the primary active and toxic constituent of areca nut. Arecaidine and arecoline N -oxide are two major active metabolites of arecoline. In this work, an accurate and simple high performance liquid chromatography tandem mass spectrometry method for simultaneous quantification of arecoline, arecaidine and arecoline N -oxide in rat plasma was developed and fully validated to study their pharmacokinetic behaviors in rats. After extracted from rat plasma by protein precipitation with methanol and then concentrated, the analytes were chromatographic separated on a Sepax Sapphire C 18 analytical column. The mobile phase consisted of methanol and 2 mM ammonium acetate buffer solution containing 0.2% ( v/v ) formic acid (8:92, v/v ) under isocratic elution. The analytes were detected by multiple reaction monitoring (MRM) with an electrospray ionization source in the positive ion mode. The transitions of m / z 156.2 → 53.2, m / z 142.2 → 44.2 and m / z 172.2 → 60.2 were selected for arecoline, arecaidine and arecoline N -oxide, respectively. The method was linear over the concentration range of 0.5–100 ng/mL for arecoline, 5–5000 ng/mL for arecaidine and arecoline N -oxide with no carry-over effect. The accuracies and intra- and inter-batch precisions were all within the acceptance limits. No matrix effect and potential interconversion between the analytes and other metabolites were observed in this method. The validated method was further employed to a preclinical pharmacokinetic study of arecoline, arecaidine and arecoline N -oxide after oral treatment with 20 mg/kg arecoline to rats.
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BIOMEDICAL CHROMATOGRAPHY
·
2013
·Vol. 28
·期 7
·994-1002
·
IF 1.945
Ting Zhou,Ting Zhao,Qing Cheng,Shan Liu,Ling Xu,Wen Tan
A sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of R -bambuterol and its active metabolite R -terbutaline in human plasma and urine was established. The inhibition for the biotransformation of R -bambuterol in plasma was fully investigated. Plasma samples were prepared on ice and neostigmine metilsulfate added as a cholinesterase inhibitor immediately after sample collection. All samples were extracted with ethyl acetate and separated on a C 18 column under gradient elution with a mobile phase consisting of methanol and water containing 5 m m ammonium acetate at a flow rate of 0.6 mL/min. The analytes were detected by an API 4000 tandem mass spectrometer with positive electrospray ionization in multiple reaction monitoring mode. The established method was highly sensitive with the lower limit of quantification (LLOQ) of 10.00 pg/mL for each analyte in plasma. In urine samples, the LLOQs were 20.00 and 500.0 pg/mL for R -bambuterol and R -terbutaline, respectively. The intra- and inter-day precisions were <12.7 and <8.6% for plasma and urine, respectively. The analytical runtime within 6.0 min per sample made this method suitable for high-throughput determination. The validated method has been successfully applied to the human pharmacokinetic study of R -bambuterol involving 10 healthy volunteers. Copyright © 2013 John Wiley & Sons, Ltd.
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MICROCHIMICA ACTA
·
2019
·Vol. 187
·期 1
·1-10
·
IF 5.479
Chen Dan,Xu Hui
A method is described for automatted on-line micro-solid phase extraction using polydopamine-modified polystyrene/silica electrospun nanofibers as an adsorbent for monohydroxy metabolites of polycyclic aromatic hydrocarbons (OH-PAHs). They were then quantified by liquid chromatography-mass spectrometry. The sorbent has a network structure, high porosity, stability, hydrophilicity and good extraction capacity. Under optimal experimental conditions, the method has (a) wide linear ranges (0.03–25 ng·mL −1 for 3-hydroxyphenanthrene and 1-hydroxypyrene; and 0.05–25 ng·mL −1 for 2-naphthol), (b) good precision (with relative standard deviations from 2.0 to 12.4%), (c) high enrichment factors (24–112), (d) low limits of detection (2–21 pg·mL −1 ), and (e) acceptable recoveries from spiked samples (79.1 to 108%). The method was successfully applied for the analysis of trace OH-PAHs in urine.
Schematic illustration of online micro-solid phase extraction using polydopamine-modified polystyrene/silica electrospun nanofibers as adsorbent for the enrichment and determination of monohydroxy metabolites of polycyclic aromatic hydrocarbons (OH-PAHs) prior to LC-MS analysis.
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XENOBIOTICA
·
2026
·
IF 1.5
Jia Yao,Shunjun Yang,Ying Liu,Rong Ye,Yufen Liao,Yong Guo,Rong Tan,Tiantai Wu,Yang Jin,Gangyan Yu,Chang Lin,Weiwei Li,Shiyu Zhang,Jia Yu
Quantitative analytical method was developed for six coumarin constituents in Angelicae pubescentis radix (APR), and the inhibitory effect of the herb’s extract on cytochrome P450 enzymes was investigated.A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous quantification of six coumarins (imperatorin, 8-methoxypsoralen, isopimpinellin, isoimperatorin, bergapten, and cnidilin) in APR. Concurrently, the inhibitory effects of its aqueous extract on multiple P450s were evaluated in rat liver microsomes using a ‘Pittsburgh cocktail’ approach.The method demonstrated excellent linearity (R2 > 0.999), precision, stability, repeatability (RSD < 3.0%), and recovery (95.15-102.36%). The extract exhibited significant time-dependent inhibition of CYP1A2 (residual activity 58.2%), with weaker effects on other P450s.A robust LC-MS/MS method was successfully established. The extract of APR was identified as a potent time-dependent inhibitor of CYP1A2 in rat liver microsomes (RLMs), suggesting a potential risk for metabolism-based drug interactions in rats that warrants further investigation in human systems.
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