RSC Advances
·
2022
·Vol. 12
·期 17
·10460-10466
·
IF 4.036
Zhichao Jin,Chunhua Yan,Huimin Chu,Qing Huang,Zhizhong Wang
Among the cyclodextrins screened for the synthesis of 2-hydroxy-1,2-diphenylethanone (benzoin) in water, 2-hydroxypropyl-β-cyclodextrin (HP-β-CD) exhibited the highest yield in the benzoin condensation reactions, and HP-β-CD can be recycled several times with little loss of activity through the addition of fresh VB1. As an example of supramolecular catalysis, the methodology was applied to the “green” synthesis of the antiepileptic drug phenytoin through benzoin condensation, oxidation, and cyclization reactions in the presence of HP-β-CD, without the use of any harmful organic solvent. Moreover, the complexation behaviors of HP-β-CD with benzaldehyde and intermediates were studied by UV-vis and 2D-ROESY NMR spectroscopies to reveal the plausible mechanisms of the reactions, and HP-β-CD did not act as a simple phase transfer agent.
研究领域:
有机化学
·
药物化学
·
绿色化学
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DOI
高影响因子
TALANTA
·
2024
·
IF 5.6
Chun-Ying Xu,Yi-Xin Zhong,Yuan-Yuan Cui,Cheng-Xiong Yang
Owing to their incomplete digestion in the human body and inadequate removal by sewage treatment plants, antiepileptic drugs (AEDs) accumulate in water bodies, potentially affecting the exposed humans and aquatic organisms . Therefore, sensitive and reliable detection methods must be urgently developed for monitoring trace AEDs in environmental water samples. Herein, a novel phenylboronic acid-functionalized magnetic cyclodextrin microporous organic network (Fe 3 O 4 @CD-MON-PBA) was designed and synthesized via the thiol-yne click post-modification strategy for selective and efficient magnetic solid-phase extraction (MSPE) of trace AEDs from complex sample matrices through the specific B–N coordination, π-π, hydrogen bonding , electrostatic, and host-guest interactions. Fe 3 O 4 @CD-MON-PBA exhibited a large surface area (118.5 m 2 g −1 ), rapid magnetic responsiveness (38.6 emu g −1 , 15 s), good stability and reusability (at least 8 times), and abundant binding sites for AEDs. Under optimal extraction conditions, the proposed Fe 3 O 4 @CD-MON-PBA-MSPE-HPLC-UV method exhibited a wide linear range (0.5–1000 μg L −1 ), low limits of detection (0.1–0.5 μg L −1 ) and quantitation (0.3–2 μg L −1 ), good anti-interference ability, and large enrichment factors (92.2–104.3 to 92.3–98.0) for four typical AEDs. This work confirmed the feasibility of the thiol-yne click post-synthesis strategy for constructing novel and efficient multifunctional magnetic CD-MONs for sample pretreatment and elucidated the significance of B–N coordination between PBA and N-containing AEDs.
研究领域:
环境科学
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分析化学
·
药学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2025
·
IF 2.6
Xiao-han Peng,Fan Zhang,Xin-feng Xia,Kun Wang,Yan-Lin Zhao,Yan Du,Daoquan Tang
Pharmacological treatment with antiepileptic drugs (AEDs) remains a primary selection for most patients with epilepsy, while therapeutic drug monitoring is an important strategy to ensure the efficacy and safety of AEDs. The aim of this study was to optimize and develop a green high-performance liquid chromatography (HPLC) method suitable for simultaneous detection of 8 AEDs and 2 active metabolites including primidone (PRM), lamotrigine (LTG), carbamazepine (CBZ) and its active metabolite 10,11-epoxide (CBZE), oxcarbazepine (OXC) and its active metabolite 10, 11-dihydro-10-hydroxyl carbamazepine (MHD), phenobarbital (PHB), eslicarbazepine acetate (ESLA), clonazepam (CZP) and diazepam (DZP) in human serum. The results showed that using chlorzoxazone as the internal standard, ethanol as protein precipitant of serum, ZORBAX Eclipse Plus-C18 (150 × 4.6 mm, 3.5 μm) column as stationary phase, and gradient ethanol and 15 mM potassium dihydrogen phosphate water solution as green alternative mobile phase, good chromatographic separation for 10 target analytes could be obtained. The calibration curves of 10 analytes demonstrated good linearity within the test range (r > 0.996). The intra- and inter-batch precision and accuracy were all less than 15%, while extraction recoveries were in the range of 74.57-90.89 % with the relative standard deviation values less than 15%. The results of greenness assessment showed that the proposed method was ecofriendly. Finally, the validated method was successfully applied in the determination of real serum samples.
研究领域:
药理学
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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
Scientific Reports
·
2016
·Vol. 6
·期 1
·1-10
·
IF 5.228
Zhou Haidong,Ying Tianqi,Wang Xuelian,Liu Jianbo
Twelve selected pharmaceuticals including antibiotics, analgesics, antiepileptics and lipid regulators were analysed and detected in water samples collected from 18 sampling sections along the three main urban rivers in Yangpu District of Shanghai, China during four sampling campaigns. Besides, algal growth inhibition test was conducted to preliminarily assess the eco-toxicology induced by the target pharmaceuticals in the rivers. Mean levels for most of target compounds were generally below 100 ng/L at sampling sections, with the exception of caffeine and paracetamol presenting considerably high concentration. The detected pharmaceuticals in the urban rivers ranged from
研究领域:
环境科学
·
毒理学
·
药理学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Xiao-han Peng,Yan-lin Zhao,Zhong Huang,Xin-feng Xia,Kun Wang,Peng Jin,Yan Du,Dao-quan Tang
Currently, treatment with antiepileptic drugs (AEDs) is still the first choice for epileptic patients, while monitoring their blood concentrations is undoubtedly beneficial for minimizing their adverse side effects and optimizing their therapeutic effects. In this study, an ultra-high performance liquid chromatography coupled with tandem mass spectrometry with polarity switching was developed and validated for simultaneous determination of 14 AEDs and 2 active metabolites in human serum. Olanzapine was selected as the internal standard. One-step protein precipitation using methanol containing 0.05 % formic acid was used to treat sample, and the supernatant was injected for analysis without further evaporation and reconstitution. Chromatographic separation was performed on an Aglient Zorbax Eclipse Plus C18 (50 mm × 2.1 mm, 1.8 μm) column with gradient methanol and 0.1 % formic acid in water as mobile phase. Multi-reaction monitoring was performed for quantification of 16 analytes in polarity switching mode. Matrix-matched calibration curves of 16 analytes presented good linearity within the test concentration range ( r > 0.99). The intra- and inter-run accuracies and precisions at the lower limit of quantification, and low, medium and high quality control levels were all less than 20 % or 15 %, respectively. The extraction recovery, matrix effect, and stability were all acceptable under detected conditions. Finally, this method was successfully applied in the quantitation of target analytes in the serum of patients received AEDs.
研究领域:
药理学
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临床医学
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分析化学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2020
·
IF 6.785
Zhen Zou,Xiaodou Liao,Le Yang,Ziyun Huang,Hua Yang,Qi Yan,Yufei Zhang,Zhihe Qing,Lihua Zhang,Feng Feng,Ronghua Yang
Tiagabine hydrochloride (TGB) is a clinically frequently used drug for anticonvulsion and reducing epileptic frequency. Over administration of TGB could bring about adverse effects, such as speech disorder, depression, and even suicidal tendencies. Therefore, accessible and sensitive assay for analysis of TGB becomes an urgent need toward guiding clinical medication. Here, we present the first report on fluorescence turn-on detection of TGB in urine testing. In this protocol, a fluorescent dye, perylene tetracarboxylic acid imide derivative (PTAI), is found specifically occupying the Sudlow site II of human serum albumin (HSA) and displays a new phenomenon of binding-induced quenching (BIQ). In presence of TGB, competitive binding of the TGB to the site II of HSA will trigger release of PTAI, thus successfully lighting up the fluorescence of PTAI. This label-free assay enjoys a broader working range (1–350 μM) and lower detection limit (0.218 μM) than the traditional liquid chromatography method and is uninterfered by the miscellaneous in the artificial urine. The BIQ probe highlights the merits of HSA as a quencher and a molecular recognition unit, and it opens up a way for studying drug-HSA interaction mechanism and noninvasive pharmaceutical testing.
研究领域:
生物化学
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医学检测
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药物分析
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产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2022
·
IF 6.911
Wei Hu,Wei Zhou,Chenlu Wang,Zichun Liu,Zilin Chen
Development of high-throughput and rapid screening analytical method is in high demand for anti-doping and clinical point-of-care (POC) analysis. Solid-phase microextraction and mass spectrometry direct coupling (SPME-MS) has been proved as a rapid and effective way for target analysis in complex sample matrixes. An online direct coupling of in-tube SPME (IT-SPME) with MS using polymer coated open-tubular column has been developed in this work. A sharp stainless-steel needle was attached at the end of the SPME column, which enables the direct ionization of the analytes after elution from the IT-SPME column. Itaconic acid-benzene co-polymer was in-situ grown on the inner surface of the fused silica capillary and used as extraction phase. This column has low backpressure and provides both hydrophobic and weak cationic exchange interaction with the target analytes due to the chemical properties. The developed online IT-SPME-MS method showed good extraction performance towards various target analytes and good reusability at least for 60 times. As a proof-of-concept application, the above method was applied for the analysis of antiepileptic drugs (AEDs) in both plasma and urine samples with linear range (1 ng/mL-200 ng/mL), good linearity (R 2 ≥ 0.99), and good reproducibility (intra-day RSDs less than 4.36%, inter-day RSDs less than 6.55%). The method exhibited high enrichment factors between 187 and 204 for the two AEDs and high sensitivity for the analysis of human plasma samples and urine samples.
研究领域:
分析化学
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临床医学
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药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Qing Wang,Xinyu Shi,Shao-Feng Tang,Huanhuan Wang,Yuan Chen,Na Zhang
Simultaneous monitoring of plasma concentration levels of multiple antiepileptic drugs (AEDs) is essential for dose adjustment in comprehensive epilepsy treatment, necessitating a sensitive technique for accurate extraction and determination of AEDs. Herein, a magnetic solid-phase extraction (MSPE) technique on the basis of modified biochar (BC) is investigated to extract four AEDs from plasma, in conjunction with high performance liquid chromatography. BC derived from Zizyphus jujuba seed shells was activated by phosphoric acid (PBC) and magnetized via coprecipitation to produce MPBC. The MPBC-CD obtained after modification with β-cyclodextrin (CD) was characterized and evaluated for adsorption. It exhibited fast adsorption kinetics based on second-order kinetics and satisfactory adsorption capacity for AEDs. Then it was employed as the MSPE adsorbent and the influencing parameters were optimized. The enrichment factor was 18.75. The validation analysis revealed a favorable linearity that ranged from 0.04 to 20 μg·mL −1 along with a low limit of detection of 6.85 to 10.19 ng·mL −1 . The recovery of the AEDs ranged from 78.7 to 109.2%, with relative standard deviations below 6.7%. Using quantum chemistry theory calculations and experimental results analysis, the adsorption mechanism was investigated. It disclosed that the suggested strategy built upon MPBC-CD was appropriate for the assessment of AEDs in plasma and expanded the usage of BC as the environmentally favorable matrix for the analysis of biological samples.
研究领域:
分析化学
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药学
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材料科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Jingyi Zhang,Donghao Liu,Xiaoyan Meng,Yi Shi,Ruya Wang,Deli Xiao,Hua He
In this study, a novel solid phase extraction based on porous magnetic graphene oxide-cyclodextrin polymers (MGO-CD) was developed with aromatic linker and used for the simultaneous extraction and preconcentration of trace antiepileptic drugs in plasma. The characteristics of MGO-CD were assessed by Fourier transform infrared spectroscopy (FT-IR), Brunauer-Emmett-Teller surface areas (BET), Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). Magnetic cyclodextrin polymeric material exhibited a high specific surface area (187 m 2 g −1 ), large pore volume (0.12 cm 3 g −1 ), good saturated magnetization (37.68 emu g −1 ), and excellent dispersibility in aqueous solution. Various parameters influencing the extraction recovery of drugs were studied. The method exhibited good linearity in the range of 1–50 μg mL −1 , and the limit of quantitation of carbamazepine, phenytoin, diazepam was 11.89, 47.10 and 16.17 ng mL −1 , respectively. The recoveries of three antiepileptic drugs range from 78.49 to 100.93% with relative standard deviations less than 5.5%. These analytical results demonstrated that the proposed approach based on MGO-CD was applicable for analysis of antiepileptic drugs in plasma samples.
研究领域:
分析化学
·
药物分析
·
材料科学
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产品关联
DOI
PubMed
高影响因子
ACS Chemical Neuroscience
·
2025
·
IF 3.9
Ying Sun,Yajun Bai,Bin Li,Peinan Fan,Haiyan Lu,Pu Jia,Ye Zhao,Yujun Bai,Shixiang Wang,Kechun Liu,Meng Jin,Tai-Ping Fan,Xiaohui Zheng
Developmental epileptic encephalopathies (DEEs), including Dravet syndrome (DS), require antiseizure medications (ASMs) that balance efficacy with developmental safety. There is an urgent clinical need for novel therapeutic agents that combine potent anticonvulsant activity with developmental safety. β-Asarone, an active constituent of Acorus plants, has demonstrated antiepileptic potential, but its toxicities severely limit clinical application. Notably, β-asaronol, a hydroxylated metabolite of β-asarone, may exhibit improved safety; however, its pharmacological properties and therapeutic potential remain systematically unelucidated. To evaluate the developmental safety and antiseizure efficacy of β-asaronol for pediatric refractory epilepsy, developmental toxicity, antiseizure activity, and neuroprotective effects were systematically assessed using zebrafish models (Tg vmat2:GFP, Tg lfabp:EGFP, pentylenetetrazole (PTZ)-induced seizures, and scn1lab–/– mutants). Electrophysiology, molecular docking, and biomarker analyses elucidated mechanisms. β-Asaronol (5–150 μM) exhibited no significant developmental toxicity in zebrafish, with normal hatching rate, mortality, malformation rate, and no abnormalities in neurotoxicity or hepatotoxicity indicators. Its lethal concentration 50 (LC50) value was 3.5-fold higher than that of the parent compound β-asarone. It prolonged seizure latency, suppressed PTZ-induced hyperactivity (150 μM restoring baseline locomotion), and reduced neuronal apoptosis (lactate dehydrogenase (LDH)/c-fos normalization). In scn1lab–/– mutants, β-asaronol outperformed stiripentol and cannabidiol, reducing epileptiform discharges by about 93%. Mechanistically, β-asaronol potentiated γ-aminobutyric acid type A (GABAA) receptor currents (EC50 = 20.8 μM) via benzodiazepine-binding site interactions. β-Asaronol combines superior developmental safety with potent antiseizure efficacy, positioning it as a promising candidate for Dravet syndrome and refractory epilepsy.
研究领域:
神经药理学
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发育毒理学
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癫痫研究
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民族药理学
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分子模拟
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神经科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 4
·e70151
·
IF 2.8
Yu-Fei Zhang,Zheng Yu,Zhao Zhao,Le-Qing Xu,Xun-Yi Wu,Chun-Lai Ma
Monotherapy or combination therapy with anti-seizure medications (ASMs) remains the cornerstone of epilepsy treatment. Therapeutic drug monitoring is important for individualized ASM treatment and for optimizing outcomes in patients with epilepsy. Therefore, the simultaneous and accurate quantification of ASMs is necessary and helpful for clinical use. In this study, a new method was developed to simultaneously quantify carbamazepine, lacosamide, lamotrigine, levetiracetam, oxcarbazepine, perampanel, sodium valproate, topiramate, and an active metabolite of oxcarbazepine, 10, 11-dihydro-10-hydroxycarbamazepine, in human plasma by high-performance liquid chromatography-tandem mass spectrometry using the positive/negative ion-switching ionization mode. The method was assessed for accuracy, precision, linearity, recovery, and matrix effects according to the criteria of the U.S. Food and Drug Administration Bioanalytical Method Validation Guidelines for Industry for Bioanalytical Methods. The lower limit of quantification was determined to be 0.001–25 µg/mL for each analyte. The intra- and inter-day precision values had <14.6% coefficients of variation, and the accuracy ranged from 85.3% to 113% at the three levels of quality control. In addition, this method was successfully applied to therapeutic drug monitoring of ASMs in patients with epilepsy. This method allows for simple preparation, accurate quantification, and the determination of different ASMs without requiring analytical method switching, making it particularly suitable for therapeutic drug monitoring in busy clinical and hospital laboratory settings.
研究领域:
临床药理学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CNS Neuroscience & Therapeutics
·
2025
·Vol. 31
·期 7
·e70499
·
IF 5
Xinqi Fang,Junhan Wu,Yuan Hong,Jiexun Bu,Wenpeng Zhang,Zheng Ouyang,Wei Hua,Ying Mao
We present a novel point‐of‐care mass spectrometry system enabling rapid, real‐time quantification of valproic acid directly from whole blood. This bedside platform delivers serum‐equivalent results within 3 min and captures pharmacokinetic variability perioperatively, supporting individualized antiseizure therapy and timely clinical decision‐making in neurosurgical patients.
研究领域:
临床神经科学
·
药物分析
·
神经外科
·
质谱技术
·
个体化医疗
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）