MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Xin-Li Song,Hui Lv,Dong-Dong Wang,Ke-Chao Liao,Yi-Yao Wu,Gui-Mei Li,Yue Chen
Novel graphene oxide on polystyrene microspheres were fabricated via layer-by-layer assembly and initially applied to extract four bisphenol endocrine disruptors (bisphenol A, bisphenol B, bisphenol AF, tetrabromobisphenol A) in various environmental water samples following high performance liquid chromatography-tandem mass spectrometry determination. The as-synthesized adsorbent was then applied for dispersive solid-phase extraction. The as-prepared GO@PS was characterized using scanning electron microscopy and Fourier transform infrared spectroscopy. Furthermore, the main parameters governing the extraction efficiency were optimized in detail, and under the optimized conditions, attractive results were obtained. The developed method exhibited high enrichment factors ranging from 73 (BPB) to103 (BPA), low detection limits (0.02–0.11 μg·L −1 ) and wide linear ranges (0.1–1000 μg·L −1 ) for enriching and detecting the four bisphenol endocrine disruptors. Meanwhile, acceptable results were obtained when the developed technique was used to determine four target pollutants in real water samples, with spiked recoveries in the range of 71.1%–104.8%. This indicated that GO@PS was a powerful material for the enrichment and determination of bisphenols in complex matrices.
研究领域:
分析化学
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环境科学
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材料科学
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高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Hao Wang,Jianbin Ju,Yuji Ruan,Guihua Ruan,Yipeng Huang
Pre-oxidation‑carbonization regulated PAN-derived porous carbon flowers, preventing collapse and enabling N/O co-doping. • PCF-400's 400 °C carbonization retains active sites, enhancing adsorption efficiency of NSAIDs. • PCF-400 exhibits superior NSAIDs selectivity, high NSAIDs adsorption (Qe ≥ 12.69 mg g −1 ) and fast kinetics (5 min equilibrium). Flower-shaped porous carbons are attractive in separation science. Herein, the controlled synthesis of porous carbon flowers (PCF) was realized by pre-oxidation and carbonization treatments of flower-shaped polyacrylonitrile (PAN) particles. The pre-oxidation treatment at 230 °C transferred the linear polymer chain of PAN to six-membered ring structure, enhancing the thermal stability to avoid the collapse of flower-shape in carbonization process. Then, the subsequent carbonization promoted the crosslinking and formation of alicyclic and graphitic structures. The carbonization at moderate temperature (400 °C) enabled the remaining of some oxygen-containing groups and the formation of nitrogen-doped carbon structure, which was responsible for the improved adsorption efficiency for non-steroidal anti-inflammatory drugs (NSAIDs). In addition, higher adsorption efficiency of PCF than that of porous carbons in other morphologies for NSAIDs was demonstrated. The PCF carbonized at 400 °C (PCF-400) showed sufficient adsorption capacity (12.69–18.59 mg g −1 ) and selectivity for NSAIDs. An SPE-HPLC method based on PCF-400 was proposed for extraction and analysis of trace NSAIDs in environmental water samples. The SPE-HPLC method showed a wide linear range (1–400 ng mL −1 ) and low detection limits (0.38–0.56 ng mL −1 ) for three kinds of NSAIDs. The intra-day and inter-day relative standard deviations (RSDs) of this method were 1.85%–2.77% and 3.17%–3.63%, respectively. The recoveries of NSAIDs in spiked samples ranged from 89% to 103% by the SPE-HPLC method. This study not only provides a simple synthetic method for preparing carbon materials with controllable morphology and adjustable heteroatom content, but also offers an analytical method for detection of trace NSAIDs in complex environmental matrices. Download: Download high-res image (126KB) Download: Download full-size image
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MOLECULES
·
2026
·Vol. 31
·期 8
·1238
·
IF 5.1
Cui-Cui Sun,Yi-Ting Chen,Hai-Xia Xu,Yu-Xian Guo,Qing-Feng Zhang
The flowers ofSophora japonicaL. (SJF) andRobinia pseudoacaciaL. (RPF) are edible and similar in appearance. The chemical constituents of SJF and RPF were compared by UPLC-Q-TOF-MS/MS and HPLC analysis in this study. A total of 29 and 19 constituents were identified in SJF and RPF, respectively. Flavonoid glycosides were the main constituents found in both flowers. The main aglycon moieties found in SJF were quercetin, kaempferol and isorhamnetin, whereas acacetin and kaempferol were the main ones found in RPF. Additionally, the content of flavonoids in SJF was significantly higher than that in RPF, as determined by HPLC. Rutin was the most dominant flavonoid in SJF with a content range of 72.31~88.15 mg/g, followed by quercetin (13.05~20.30 mg/g). Kaempferol-di(rhamnoside)-hexoside was the most dominant flavonoid in RPF with a content range of 25.94~30.00 mg/g. The distinct flavonoid profiles indicated the chemical non-equivalence of SJF and RPF. Therefore, RPF should not be considered a direct substitute for SJF in herbal medicine without further pharmacological and clinical validation.
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PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
·
2026
·
IF 8.8
Qi Zhao,Yicheng Zhou,Cong Wang,Mingxuan Li,Shan Zhu,Chang Xue,De Ji,Yuwen Qin,Chengxi Jiang
Gastrodia elata Bl. ( GE ), a widely utilized edible and functional material, exhibits notable quality variations due to distinct growing conditions across different geographical origins, making reliable methods for origin authentication and quality evaluation essential. This study integrated machine vision, flash GC e-nose and HPLC to analyze GE samples from Anhui (AH), Shaanxi (SN), and Yunnan (YN) provinces in China. Results showed comparable color characteristics among geographical origins, but distinct textural differences: SN samples displayed more complex textures with higher surface roughness, YN samples showed richer textural details but less distinct edges and lower periodicity, while AH samples exhibited smoother surfaces. Eleven flavor compounds were identified as potential flavor markers. Although no significant differences were found in the total content of six marker components, three linear machine learning models (PLS, SVM, and LDA) established based on multidimensional features achieved 100% classification accuracy in training and prediction sets, providing a reliable approach for GE geographical origin traceability.
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高影响因子
ANALYTICA CHIMICA ACTA
·
2026
·
IF 6.1
Keqiang Shi,Jiancong Liao,Cuirong Sun,Hongru Feng,Yuanjiang Pan
RNA modifications are vital for all living organisms. A total of at least 63 types of uridine modification have been discovered, accounting for the largest proportion of all reported RNA modifications. Uridine modifications have also been shown to be dysregulated in various human diseases. However, it's well known that mass spectrometry analysis of uridine modifications is limited by their low ionization efficiencies. Here, we developed a simple and robust method for the simultaneous identification and quantification of 22 uridine modifications in biological samples. In fact, uridine and lots of its modifications are more easily ionized in negative ion mode, compared with positive ion mode commonly used. Besides, the fragmentation patterns of uridine modifications in negative ion mode could provide more structural information, compared with well-known glycosidic bond cleavage in positive ion mode. Furthermore, simply by adding 0.2 mM acetic acid into the mobile phase, the peak areas of uridine and all 22 uridine modifications in negative ion mode could be improved by 4.1-55.4 folds. With this novel method, we quantified 16, 14, 10, 12 and 16 uridine modifications in 293T total RNA, 293T small RNA, E. coli tRNA, S. cerevisiae tRNA and wheat germ tRNA, accordingly. This study provides a general good method for researchers interested in the identification and quantification of uridine modifications in various biological samples.
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2026
·
IF 8.7
Xiaona Cao,Gailing Tang,Xing Fan,Xinyu Gao,Tianxin Wang,Xiaohan Zhang,Wenjie Wang,Hao Wang
Establishing a chitosan microsphere-immobilized α-amylase system. • Identifying procyanidin B 2 as the core α-amylase inhibitory component within apple polyphenols. • Elucidating the inhibitory mechanism of procyanidin B 2 through multi-technique integration. Inhibition of α-amylase (PPA) delays starch digestion and glucose absorption, serving as an effective means to regulate postprandial hyperglycemia. Apple polyphenols (APE) exhibits PPA inhibitory activity, but their core active components and mechanisms of action remain unclear. This study employed immobilized enzyme coupled with HPLC-Q-TOF-MS/MS to screen PPA inhibitors from APE and elucidate their mechanisms of action.Using amino-modified chitosan microspheres as carriers, PPA was covalently immobilized via genipin-mediated Schiff base reaction. The optimal immobilization conditions were optimized (crosslinking agent concentration 0.17%, enzyme concentration 1 mg/mL, crosslinking 6 h, immobilization 14 h), establishing a stable screening system. APE was fractionated into 9 components by solvent precipitation, with component F 3 exhibiting the most potent inhibitory activity. Based on the aforementioned techniques, 4 active compounds were identified from F 3 , and validation confirmed that procyanidin B 2 (PC B 2 ) demonstrated the most effective inhibitory effect. In vitro experiments and multi-technology validation demonstrated that PC B 2 could delay starch hydrolysis and reduce the production of reducing sugars to regulate postprandial blood glucose, exhibiting reversible competitive inhibition against PPA (IC 50 = 0.25 mg/mL). It could bind to PPA and alter its secondary and tertiary structures, inducing intrinsic protein fluorescence quenching through static quenching. The binding of the two components triggered an exothermic reaction, forming a stable complex. Download: Download high-res image (140KB) Download: Download full-size image
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高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2025
·
IF 1.2
Jinhao Li,Yuanyuan Wang,Juan Du,Huanhuan Meng,Yingchao Wang,Xingchu Gong
A high-performance liquid chromatography-mass spectrometry (HPLC-MS) method was developed to quantify protocatechuic acid (PA), p-hydroxybenzoic acid (PHA), quercetin (QR), kaempferol (KP), isorhamnetin (ISO), Ginkgolide A (GA), Ginkgolide B (GB), Ginkgolide C (GC) and Bilobalide (BB) in Ginkgo biloba leaf concentrate based on (AQbD) concept. The response values of each compound were selected as the critical method attributes (CMAs).A risk assessment and Plackett–Burman design approach was performed to screen the critical method parameters (CMPs) . Box–Behnken designed experiments were were conducted to explore the relationship between the CMPs and the CMAs,and a stepwise regression method was used to build quantitative models . The method operable design region (MODR) was established and verified . The final method used an Agilent Infinitylab Poroshell 120 column (4.6 mm × 100 mm, 2.7 μm). The Mobile phase A was 0.1% formic acid-water and the mobile B was 0.1% formic acid-methanol. The flow rate was 0.66 mL/min. The column temperature was 30 °C. The gradient elution ratio was: 0–15 min, 0–35%B; 15–30 min, 35–80%B; 30–41 min, 95–95%B. The nebulizer pressure was 50 psi and the capillary voltage was 2000 V. The gas temperature was 325 °C. The fragmentor voltage of PA, PHA, BB and GA was 90 eV. The fragmentor voltage of GB and GC was 100 eV. The fragmentor voltage of QR, KP and ISO was 140 eV. The method has passed the methodology verification and can be used for the determination of flavonoid glycosides, terpenoid lactones and organic acids in Ginkgo biloba leaves concentrate.
研究领域:
药学
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分析化学
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高影响因子
TALANTA
·
2013
·
IF 3.498
Di Pan,Jianping Wang,Chunyan Chen,Chen'an Huang,Qingyun Cai,Shouzhuo Yao
In this work, ultrasonic assisted extraction combined with solid phase extraction (SPE) was applied in the analysis of polycyclic aromatic hydrocarbons (PAHs) in environment samples. A titania nanotubes/titanium plate was modified with n-octadecanethiol monolayer-protected Ag nanoparticles , and developed as the adsorbent in SPE of PAHs. Six different PAHs in soil samples were analyzed with high performance liquid chromatography-fluorescence detection. The experiment conditions including the deposition time of Ag nanoparticles, extraction solvent properties, the amount of extraction solvent, the amount of organic modifier, extraction time, and desorption solvent properties were optimized. Under the optimized conditions, good linearity and low limits of detection of 0.0015–0.4 ng g −1 were obtained. The analysis of PAHs in real soil samples gave satisfactory recoveries ranging from 70.32% to 115.51% with 3.14%–13.56% intra-day relative standard deviations (RSD) and 4.92%–14.87% inter-day RSD.
研究领域:
环境科学
·
分析化学
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高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
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2026
·
IF 7.1
Jian Gao,Jialong Wang,Jiejin Song,Yue Xing,Yuzhao Hou,Fengchao Wang,Jinghui Du,Jiang Wu,Liming Wang
The illegal addition of statins to tea-based products presents significant analytical challenges due to the complexity of the matrices involved. To address these challenges, we developed an ionic liquid-assisted magnetic solid-phase extraction (IL-MSPE) method coupled with HPLC-UV for the simultaneous determination of five statins. This protocol facilitates the rapid batch extraction of analytes within 6 min. The method demonstrated excellent linearity (R 2 ≥ 0.999, 0.1 to 20 μg/mL) and sensitivity, with limits of detection ranging from 0.022 to 0.054 μg/mL, and recovery rates between 89.2% and 117.5%. Density functional theory provided insights into a synergistic “dual-site” recognition mechanism, which is driven by π–π stacking, hydrogen bonding, and electrostatic interactions. Importantly, the method's compliance with green chemistry principles was validated by AGREE (0.77) and MoGAPI (90) metrics. Overall, this proposed workflow represents a reliable and high-throughput tool for monitoring unauthorized statin adulteration.
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BIOMEDICAL CHROMATOGRAPHY
·
2017
·Vol. 31
·期 9
·e3962
·
IF 1.613
Yunsu Ma,Qianru Wang,Hongwen Zhang,Lijun Xie,Juan Chen,Mao Huang,Yun Liu,Yuanyuan Wang,Libin Wang,Luning Sun,Ning Ou
This study presents a high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method for the simultaneous determination of antofloxacinin and its main metabolite – N -demethylated metabolite ( N- DM) – in human urine. Ornidazole was used as the internal standard. This was a clinical urine recovery study, in which 10 healthy Chinese volunteers were intravenously administered a single 200 mg dose of antofloxacin hydrochloride. Compounds were extracted by albumen precipitation, after which samples were isocratically eluted using a Poroshell 120 SB-C 18 column, and were analysed using HPLC–MS/MS under electronic spray ionization positive ion mode. The method was successfully applied in a urine pharmacokinetic study of antofloxacinin, with a detection range of 0.02/0.01 to 200/100 μg/mL (for antofioxacin/ N- DM).The average percentages of antofioxacin/ N- DM measured in urinary excretion frp, 10 volunteers were 54.9 ± 5.7/8.2 ± 2.5% in 120 h duration.
研究领域:
药物分析
·
临床药理学
·
分析化学
·
药代动力学
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Qiao Deng,Jianliang Li,Jingjing Xu,Xiaojing Zhao,Dan Wei,Xu Wang
The accurate quantification of urinary modified nucleosides, promising non-invasive cancer biomarkers, is hindered by their trace concentrations and complex matrix interference. To overcome this challenge, we developed the facile synthesis of a novel ternary magnetic composite (MCS-100GO) by integrating chitosan (CS) and graphene oxide (GO) onto the magnetic core, utilized as adsorbent for magnetic solid-phase extraction (MSPE). The adsorbent leverages the combined effects of hydrogen bonding (from CS and GO) and π-π interactions (from GO) for highly efficient capture, while the magnetic core enables rapid and simple separation. Systematic optimization demonstrated exceptional performance for 3-methylcytidine (m 3 C) and 7-methylguanosine (m 7 G). The MCS-100GO composite achieved rapid adsorption equilibrium (3 min), high maximum adsorption capacities (0.7730 mg/g for m 3 C and 0.7561 mg/g for m 7 G). The developed MCS-100GO based MSPE-HPLC-MS/MS method, validated according to FDA guidelines, exhibited excellent sensitivity (LODs: 0.015–0.030 μg/L), a wide linear range (0.050–50 μg/L; R 2 > 0.9995), and high precision (RSD < 6.4 %). Furthermore, parallelism experiments with a coefficient of variation (CV) of 9.7 % confirmed no significant matrix effects. Compared to existing methods, this approach offers a superior balance of low adsorbent dosage, sensitivity, speed, presenting a promising and efficient strategy for high-throughput analysis of urinary nucleoside biomarkers.
研究领域:
分析化学
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生物材料
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癌症生物标志物
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代谢组学
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环境与生物医学分析
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Xiaoqi Liu,Chenjia Jiang,Haodong Zhou,Yunfeng Yuan,Jinhua Zhu,Xiuhua Liu,Md. Zaved H. Khan,Minghua Lu
Synthetic phenolic antioxidants PG (propyl gallate), TBHQ (tert-butyl hydroquinone), BHA (butyl hydroxyanisole) are commonly used additives in edible oils, but excessive residues may pose health risks. Conventional detection methods suffer from high organic solvent consumption, complex pretreatment procedures, and environmental concerns. To address these limitations, this study developed a rapid, green and efficient analytical method combining deep eutectic solvent (DES)-based liquid-liquid microextraction (LLME) with high-performance liquid chromatography (HPLC) for the rapid determination of phenolic antioxidants in edible oils. Using an optimized hydrophilic DES system composed of choline chloride and 1,3-butanediol, (molar ratio 1:2), along with simplified extraction conditions (780 μL DES, 11 s vortex at room temperature), efficient extraction and enrichment of the target analytes were achieved. The method demonstrated excellent performance specifically for PG and TBHQ, exhibiting a wide linear range (1-400 μg/mL, R² > 0.9970), low limits of detection (0.12-0.28 μg/mL), satisfactory spiked recoveries (90.2 %-113 %), and good intra-day and inter-day precision (RSD < 5.0%). Analysis of real samples demonstrated that the proposed method is highly sensitive, operationally simple, and environmentally friendly for the analysis of PG and TBHQ, offering a promising alternative for rapid monitoring and food safety regulation of these two antioxidants in edible oils. It should be noted that the current hydrophilic DES system did not achieve optimal extraction efficiency for BHA, highlighting the need for further optimization toward a comprehensive multi-analyte approach.
研究领域:
食品化学
·
分析化学
·
食品安全
·
绿色化学
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PubMed
高影响因子