ACS Applied Materials & Interfaces
·
2023
·
IF 9.5
Jianwen Wang,Meiyang Hu,Yingying Zhu,Mengyang Cao,Rashid Khan,Xianwen Wang,Lu Huang,Yingpeng Wu
The safety issues caused by sodium dendrites limit the widespread application of sodium metal batteries. Herein, a self-healing polymer electrolyte (SPE) is prepared by immersing the self-healing polymer in a liquid electrolyte. Benefiting from the self-healing properties, elastic interface, and dense nonporous structure of the SPE, the fabricated NaK|MC SPE|NaK symmetric battery presents a long battery life (∼590 h) and low polarization voltage (192 mV). Moreover, the PTCDA|MC SPE|NaK full cell also delivers stable long cycles and outstanding rate performance.
研究领域:
材料科学
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电化学
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能源存储
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产品关联
DOI
PubMed
高影响因子
Foods
·
2021
·Vol. 10
·期 11
·2735
·
IF 4.35
Chujun Liu,Yawen Guo,Bo Wang,Lan Chen,Kaizhou Xie,Chenggen Yang
A simple and sensitive gas chromatography–tandem mass spectrometry (GC–MS/MS) method was established for the quantitative screening of penicillin G residues in chicken and duck eggs (whole egg, yolk and albumen). The analyte was separated on a TG-1MS capillary column (30.0 m × 0.25 mm i.d., 0.25 μm) with an external calibration method and electron impact (EI) ionization. Samples were pretreated using an accelerated solvent extraction (ASE) procedure followed by solid-phase extraction (SPE) on HLB cartridges (60 mg/3 mL). The derivative, which was safer and easier to store than penicillin G, was obtained by reacting trimethylsilyl diazomethane (TMSD) with penicillin G. The method was validated by the following parameters: linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). The matrix-matched calibration curves had good linearity (R2 ≥ 0.9994) within the concentration range of LOQ–200.0 µg/kg for penicillin G in the sample matrices. In the same concentration range, the accuracy, in terms of recovery, was 80.31–94.50%; the relative standard deviation (RSD), intra-day RSD and inter-day RSD ranged from 1.24 to 3.44%, 2.13 to 4.82% and 2.74 to 6.13%, respectively. The LODs and LOQs of penicillin G in the matrices were in the ranges of 1.70–3.20 and 6.10–8.50 μg/kg, respectively. The applicability of the GC–MS/MS method was demonstrated by the determination of poultry eggs obtained from local markets with no penicillin G residues.Keywords:penicillin G;GC–MS/MS;ASE;poultry eggs;SPE
研究领域:
分析化学
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食品安全
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
Sun Zhi,Wang Fangfang,Li Wenxuan,Ren Ruobing,Zhou Peipei,Jia Qingquan,Zhao Lingguo,Chen Di,Zuo Lihua
Therapeutic drug monitoring is essential for ensuring the efficacy and safety of medications. This study introduces a streamlined approach that combines pipette-tip solid-phase extraction (PT-SPE) with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), facilitating rapid and high-throughput monitoring of drug concentrations. As a demonstration, this method was applied to the extraction and quantification of antidepressants in serum. Utilizing Zip-Tip C18, the method enabled the extraction of antidepressants from complex biological matrices in less than 2 min, with the subsequent MALDI-MS analysis yielding results in just 1 min. Optimal extraction recoveries were achieved using a sampling solution at pH 9.0 and a 10 μL ethanol desorption solution containing 0.1% phosphoric acid. For MALDI analysis, 2,5-dihydroxybenzoic acid was identified as the most effective matrix for producing the highest signal intensity. The quantification strategy exhibited robust linearities ( R 2 ≥ 0.997) and satisfactory limits of quantification, ranging from 0.05 to 0.5 μg/mL for a suite of antidepressants. The application for monitoring dynamic concentration changes of antidepressants in rat serum emphasized the method’s efficacy. This strategy offers the advantages of high throughput, minimal sample usage, environmental sustainability, and simplicity, providing ideas and a reference basis for the subsequent development of methods for therapeutic drug monitoring. Graphical Abstract
研究领域:
药物分析
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临床医学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Xiaoqian Chen,Luyao Yu,Yingxia Guo,Jiansong You,Meiyun Shi,Yalin Xi,Lei Yin
An analytical assay based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technique for absolute quantification of vancomycin in complexed biological matrix was developed in this study. Reversed phase column with gradient elution was chosen for chromatographic separation of vancomycin and internal standard (IS) norancomycin. Sample pretreatment was performed by micro-solid phase extraction (μ-SPE) with Oasis® MAX μElution Plate (I.D., 30 μm). Multiple reaction monitoring (MRM) transition was chosen for monitoring of the analytes. For vancomycin, mass-to-charge ratio ( m/z ) of the MRM transition was 725.3→144.1; For norvancomycin, m/z of the MRM transition was 718.3→144.2. The running time was 3 minutes for each sample. The UHPLC-MS/MS method showed a good linear relationship (R 2 ≥0.995) in the concentration range of 0.5–100 μg/mL. The intra- and inter-day accuracies (relative error, RE) are within the range of −3.44 %-1.50 % and precisions are between 3.48 % and 10.19 %. μ-SPE could enrich the analytes and decrease the endogenous interferences, thereby improving the selectivity and sensitivity of the method. The analytical assay is selective, accurate and reproducible. The assay was successfully applied to therapeutic drug monitoring of vancomycin in clinical application.
研究领域:
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
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2022
·Vol. 36
·期 20
·e9358
·
IF 2.586
Donghai Xu,Fangfang Pan,Hao Ruan,Nan Sun
Rationale Hydroxychloroquine sulfate is effective in the treatment of malaria and autoimmune diseases and as an antiviral drug. However, unreported impurities are often detected in this drug, which pose a health risk. In this study, the structures of hydroxychloroquine and six unknown impurities were analyzed using ultra-high-performance liquid chromatography-quadrupole/time-of-flight-tandem mass spectrometry (UHPLCQ/TOF/MS/MS), and the structures were characterized using liquid chromatography-solid-phase extraction-nuclear magnetic resonance (LC-SPE-NMR) spectroscopy. Methods An Agilent InfinityLad Poroshell HPH-C18 column (100 × 4.6 mm, 2.7 μm) was used. For the analysis of hydroxychloroquine and six unknown impurities, the mobile phase was 20 mM ammonium formate aqueous solution and methanol/acetonitrile (80:20, v/v) using gradient elution. Full-scan MS and MS 2 were performed to obtain as much structural information as possible. In addition, six unknown impurities were separated by semipreparative liquid chromatography and characterized using LC-SPE-NMR. Results The MS 2 fragmentation patterns of the impurities were investigated, leading to more structural information and an understanding of the fragmentation pathways of the impurities. The structures of the unknown impurities were confirmed using NMR. In addition, some possible pathways of the formation of the impurities in the drugs were outlined, and these impurities were found to be process impurities. Conclusions Based on the identification and characterization of these impurities, this study also describes the cause of the production of the impurities and provides insights for companies to improve their production processes and a scientific basis for the improvement of the related pharmacopoeias.
研究领域:
药学
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分析化学
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医学
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产品关联
DOI
PubMed
高影响因子
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
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2023
·
IF 1.2
Ke-Han XU,Long LI,Zhen-Bang TIAN,Hui LI,Yi-Ping DU,Zuo-Hua HUANG,Liang ZHAO
This work developed a novel membrane SPE coupling solid-phase fluorescence detection method. An integrated device was generated to realize continuous sample pretreatment and in-situ solid-phase fluorescence detection. The proposed method can recognize trace p -phenylenediamine (PPD) based on its reaction with fluorescamine (FA). The reaction can produce a fluorescent derivative FA@PPD, generating a strong fluorescence emission at 506.5 nm. The membrane SPE can effectively enrich the FA@PPD, offering a unique sensing technique for solid-phase fluorescence detection of PPD in the ranges of 2.0–100.0 μg/L. The detection limit of PPD was 0.5 µg/L and RSD < 6.4%. Common coexisting substances in samples had minimal impact on PPD detection. The proposed technique and apparatus displayed quick detection and applicability in environmental and biological analysis in assertive agreement with the HPLC-MS system. The developed device realized the combination of solid-phase extraction and solid-phase fluorescence detection. It is feasible to combine the high sensitivity and efficiency of solid-phase fluorescence spectra with the advantageous enrichment efficiency of SPE. This strategy can achieve the quick analysis of trace contaminants and offer technological support for automatic sample pretreatment and online detection because of the synergistic coupling of these two methods.
研究领域:
分析化学
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环境科学
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生物分析
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产品关联
DOI
高影响因子
ULTRASONICS SONOCHEMISTRY
·
2022
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IF 9.336
Yeqing Ruan,Jiahuan Xu,Jianbo Chu,Jing Shi,Qiyuan Shi
Nuciferine is an important drug candidate for the treatment of many diseases. However, there is no general method for its low - cost production. In this work, a feasible method for the production of nuciferine from lotus leaf, using ultrasonic-assisted extraction-solid phase extraction (UAE-SPE) as extraction and cleanup procedure, was developed. Petroleum ether and silica gel have been successfully used as extraction solvent and adsorbent to integrate UAE with SPE, respectively. Except for filtration, no treatment (e.g. concentration and redissolution, etc) was needed on UAE extract before SPE and the effluents obtained in the loading process of SPE could be used as UAE extraction solvent without purification. No obvious decline in the extraction efficiency of UAE and adsorption capacity of SPE was observed at least for 5 runs, which provides a feasible way for the continuous production of nuciferine in industry, i.e. Cyclic UAE-SPE. Moreover, SPE column could be conveniently regenerated and reused without significant decline in its adsorption capacity at least for 5 cycles, which can be used to reduce the cost of the whole system further. In comparison with other cleanup procedures, Cyclic UAE-SPE showed apparent advantages in energy conservation and emission reduction. LLE and crystallization were applied to separate nuciferine from other impurities further. Under optimum conditions, the total recovery rate of nuciferine with a purity over 90.0% from lotus leaf reached 50.1%. All in all, the developed method has advantages in convenient operation, low cost, and high efficiency, thus, is fitting for the production of high purity nuciferine.
研究领域:
药物化学
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提取技术
·
天然产物
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产品关联
DOI
PubMed
高影响因子
SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY
·
2019
·
IF 2.931
Long Li,Wanchao Chen,Hui Li,Jibran Iqbal,Ying Zhu,Ting Wu,Yiping Du
Fumonisin B 1 is the most prevalent member of a family of toxins, known as fumonisins , which occurs mainly in maize, wheat and other cereals. Due to its hepatotoxic and nephrotoxic in all animal species, very strict regulations have been imposed on the levels of fumonisin B 1 in cereal and cereal-based foods worldwide. In this work, a rapid determination method of fumonisin B 1 by membrane solid phase extraction coupled with solid-phase fluorescence analysis is developed. A rhodamine based fluorescent probe was used for derivatization with fumonisin B 1 . After derivatization and extraction by nylon membrane, the enriched fumonisin B 1 can be detected directly on the membrane without further elution process that is placed in a designed spectra collection device. The established method showed a linear relationship in concentration range of 0.5–5.0 μg/L, with the R 2 = 0.991, and a limit of detection of 0.119 μg/L. Method accuracy was further confirmed using LC-MS method by comparing the detection results of 3 corn powder samples spiked with FB 1 , that demonstrated equivalent results. The results of this study indicated that the proposed method was simple, sensitive, reliable and suitable for trace fumonisins B 1 quantitation in corn-based feeds.
研究领域:
食品安全
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分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2024
·
IF 5.6
Lvhong Gong,Shengxi Wu,Junjie Liu,Mingjun Zhang,Jinghao Zhuang,Doudou Xu
An ultrasensitive immunosensor of Cys/Au@TiO 2 based on disposable screen-printed electrodes (SPE) for PIVKA-II detection for hepatocellular carcinoma (HCC) diagnosis was developed by utilizing Cystine (Cys) and nanocomposite Au@TiO 2 . Firstly, HAuCl 4 underwent a reduction reaction with NaBH 4 , then Au nanoparticles were coated onto TiO 2 nanoparticles. Followed, Cys/Au@TiO 2 was formed through self-assembly of cysteine to allow the monoclonal antibody of abnormal thrombospondin to bound to the amino group on the surface of the composite by covalent bonding. The mechanism is to determine the changes in the current of the sensor caused by the specific binding of the abnormal prothrombin monoclonal antibody adsorbed by the complex with its antigen. The Cys/Au@TiO 2 immunosensor was fully characterized by various analytical approaches and it showed a wide linear testing range of 1–10000 pg mL −1 (R 2 = 0.991) and the limit of detection down to 0.77 pg ml −1 , with highly sensitivity and specificity. The results showed that the developed immunosensor platform can effectively detect trace amounts of PIVKA-II protein and has potent clinical application for HCC diagnosis.
研究领域:
生物医学工程
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分析化学
·
癌症诊断
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2014
·
IF 3.583
Haiyun Zhai,Jiangmei Li,Zuanguang Chen,Zihao Su,Zhenping Liu,Xiao Yu
A simple glass/PDMS microfluidic chip for on-line sample pretreatment and contactless conductivity detection, which consisted of a 0.17 mm-thick glass cover and a PDMS substrate embedded with an SPE monolithic column, was presented in this paper. Using this integrated microchip system, sample extraction, injection, separation and detection were automatically performed in sequence. A sample of auramine O was concentrated by molecularly imprinted SPE (MISPE), eluted to sample reservoir, and injected by electromigration into separation channel for electrophoresis separation and contactless conductivity detection, with the calculated detection limit (S/N = 3) being 2.5 μg mL − 1 . The monolithic column was utilized to quantitatively extract auramine O , yielding an on-line enrichment factor of about 12. The microchip system is reliable and applicable to the analysis of auramine O in food sample.
研究领域:
分析化学
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微流控技术
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食品安全
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分子印迹技术
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电泳学
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生物医学工程
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2016
·
IF 2.687
Pengfei Zhu,Xia Ling,Wenwei Liu,Lingcan Kong,Yuyang Yao
A simple and fast analytical method for determination of eleven Polyfluorinated Compounds (PFCs) in source water was developed in the present work. The water sample was prepared without filtered through microfiltration membrane and 500 mL of source water was enriched by the solid phase extraction (SPE). The targent compounds were analyzed by ultra high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). The optimized analytical method was validated in terms of recovery, precision and method detection limits (MDLs). The recovery values after correction with the corresponding labeled standard were between 97.3 and 113.0% for samples spiked at 5 ng/L, 10 ng/L and 20 ng/L. All PFCs showed good linearity and the linear correlation coefficient was over 0.99. The precisions were 1.0–9.0% (n = 6). As the result of the enrichment, the MDL values ranged from 0.03 to 1.9 ng/L and were enough for analysis of the trace levels of PFCs in the Taihu Lake. The method was further validated in determining the source water and the results showed that PFHxS, PFHxA, PFOA and PFOS were the primary PFCs in Taihu Lake which might be different from the other researches. The method can be used for determination of PFCs in water with a stable recovery, good reproducibility, low detection limit, less solvent consumption, time saving and labor saving. To our knowledge, this is the first method that describes the effect of the filter membrane on the determination of PFCs in water which might acquire more accurate concentration of PFCs in Taihu Lake.
研究领域:
环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF APPLIED POLYMER SCIENCE
·
2022
·Vol. 139
·期 38
·e52905
·
IF 3.057
Jin Wang,Jingjing Bian,Bin Pu,Yuanlu Wang,Mengde Deng
Polyelectrolyte hydrogel used for supercapacitors have the roles of both electrolyte and separator, the morphology and the strength of gel polyelectrolyte (GPE) are the keys for ionic transport properties therein. Here, the P(NVP- co -SPE)/polyvinyl alcohol (PVA) IPN hydrogel was prepared by photopolymerization and thermal polymerization, respectively. The influences of preparation method on morphology, mechanical strength and electrochemical performances were studied. Photopolymerized IPN GPE (UV-GPE) exhibits a special regular microphase separation structure, and therefore has outstanding strength-toughness and better electrochemical performance. The tensile strength and the toughness increased intensively from the 6.2 MPa and 3.4 MJ m −3 of thermal polymerized IPN GPE (TH-GPE) to 28.5 MPa and 24.9 MJ m −3 , respectively. The maximum swelling ratio of UV-GPE is increased from 327% of TH-GPE to 630%. The ionic conductivity of UV-GPE increased from 4.29 × 10 −2 S/cm of TH-GPE to 5.82 × 10 −2 S/cm. UV-GPE has higher response current and specific capacitance. It also has the obviously better charge–discharge symmetry and cycling stability, and the capacity retention rate is still 92.3% after 1000 cycles. Thus, it brings out the fast, eco-economic photopolymerization method is an effective way to prepare high-performance polyelectrolyte hydrogel.
研究领域:
材料科学
·
电化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）