Chinese Journal of Analytical Chemistry最新文献

英文中文

Optimized extraction and antioxidant activity of polysaccharides from Inonotus hispidus using three-phase partitioning 三相分馏法优化了柳条多糖的提取及抗氧化活性

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-12-01 Epub Date: 2025-08-05 DOI: 10.1016/j.cjac.2025.100609

Xiaoshuang ZHOU , Xiaofeng MA , Kai HUANG , Tianyu SHI , Qin TIAN , Tianli ZHANG , Shude YANG , Xianhao CHENG , Rui ZHANG , Yongfei MING

Inonotus hispidus (I. hispidus) is rich in bioactive polysaccharides, making it a valuable dietary supplement and medicinal ingredient. This study employed the three-phase separation method (TPP) to extract and purify polysaccharides from I. hispidus, designated as SH-T. The resulting polysaccharides were then compared with those obtained through the traditional hot water extraction and ethanol precipitation method, designated as SHC, in terms of their physicochemical properties and in vitro antioxidant activity. SH-T extraction achieved maximum efficiency 20 % ammonium sulfate, 1:2 (sample:tert‑butanol) phase ratio, and 25 °C. Under these circumstances, SH-T exhibited a higher protein removal rate, with a yield of 11.10 % and a polysaccharide content of 60.84 %, nearly twice that of SHC obtained through the WEAP method. SH-T and SHC exhibited similar structural characteristics. SH-T displayed superior performance in scavenging DPPH^–, ABTS⁺, and •OH while exhibiting higher reducing power than SHC. In conclusion, TPP demonstrated efficacy in extracting polysaccharides from I. hispidus, yielding products of high purity and enhanced antioxidant properties, thus presenting a promising methodology for the isolation of polysaccharides from I. hispidus.

牛皮草（Inonotus hispidus）富含生物活性多糖，是一种有价值的膳食补充剂和药用成分。本研究采用三相分离法（TPP）对海鞘多糖进行提取纯化，命名为SH-T。然后将所得多糖与传统热水提取和乙醇沉淀法所得的多糖（称为SHC）进行理化性质和体外抗氧化活性比较。SH-T萃取的最大效率为20% %硫酸铵，1:2（样品：叔丁醇）相比，温度为25°C。在此条件下，SH-T的蛋白质去除率更高，产率为11.10 %，多糖含量为60.84 %，几乎是WEAP法的两倍。SH-T和SHC表现出相似的结构特征。SH-T对DPPH -、ABTS+和•OH的清除能力优于SHC，还原能力优于SHC。综上所述，TPP有效地提取了海鞘多糖，所得产物纯度高，抗氧化性能增强，为海鞘多糖的分离提供了一种很有前景的方法。

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引用次数: 0

Key quality attributes of Maren-Zhizhu emulsion molding based on fuzzy mathematical evaluation method and electronic tongue technology: An optimization study 基于模糊数学评价法和电子舌技术的马仁-致珠乳化液成型关键质量属性优化研究

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-12-01 Epub Date: 2025-10-29 DOI: 10.1016/j.cjac.2025.100667

Yuankun CHAI , Xinran HAN , Na Li , Chunyu LI , Zhidong QIU , Junge LI , Ye QIU , Ailing JIA

We developed Maren-Zhizhu emulsion (MZE) according to the principle of “medicine and food come from the same source”. This study aimed to investigate the process factors affecting the stability of MZE using one-way and orthogonal tests, combined with the Box–Behnken response surface method. The molding process was optimized using the particle size, polydispersity index (PDI), potential, surface tension, and static delamination conditions as indicators. Based on human sensory and electronic tongue collection of MZE taste data, the optimal taste-masking process was screened by combining the fuzzy mathematical evaluation method and principal component analysis. The key quality attributes were screened as phospholipid volume percentages, 5 %; xanthan gum volume percentages, 2.4 %; oil-phase ratio volume percentages, 50 %; emulsification temperature 60 °C; homogenization three times; and pressure 400 bar. The flavor-masking agent volume percentages were 5 % crystalline fructose, 3.2 % fructose syrup, and 0.4 % chocolate. In this study, the molding and flavor-masking processes of MZE were investigated to provide research references for the study of the oral emulsion process of Chinese medicine and the development of health products based on homologous Chinese medicine as raw materials.

我们本着“药食同源”的原则，开发了玛仁致珠乳剂（MZE）。本研究采用单因素和正交试验，结合Box-Behnken响应面法，探讨影响MZE稳定性的工艺因素。以粒径、多分散性指数（PDI）、电势、表面张力和静态分层条件为指标，对成型工艺进行了优化。以人感官和电子舌采集的MZE口感数据为基础，采用模糊数学评价法和主成分分析法相结合的方法筛选最佳的掩味工艺。筛选的关键品质属性为磷脂体积百分比，5%；黄原胶体积百分比，2.4%；油相比体积百分比，50%；乳化温度60℃；均质三次；压力400bar。掩蔽剂的体积百分比为5%结晶果糖、3.2%果葡糖浆和0.4%巧克力。本研究通过对MZE的成型和掩味工艺进行研究，为中药口服乳剂工艺研究和以同源中药为原料的保健品开发提供研究参考。

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引用次数: 0

Multi-omics integration of LC-MS/MS, network pharmacology, and molecular docking reveals pleiotropic mechanisms of Millettia speciosa Champ. in NAFLD therapy LC-MS/MS、网络药理学、分子对接等多组学整合研究揭示了密菇的多效机制。NAFLD治疗

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-12-01 Epub Date: 2025-07-22 DOI: 10.1016/j.cjac.2025.100600

Zhuo-Fan XIE, Hao-liang ZHANG, Zao-liang MA, Su-Fang CHEN, Jian-Chun MA

Non-alcoholic fatty liver disease (NAFLD), the most prevalent chronic liver disorder worldwide, is characterized by excessive triglyceride accumulation in the liver. It is strongly associated with metabolic syndrome, type 2 diabetes mellitus, obesity, and cardiovascular diseases. Fueled by the global increase in obesity rates, NAFLD has emerged as the most common liver disease globally. In this study, we utilized liquid chromatography-tandem mass spectrometry (LC-MS/MS) to comprehensively characterize the chemical constituents of Millettia speciosa Champ. By combining network pharmacology and molecular docking techniques, we constructed a “component-target-pathway” network to elucidate the therapeutic targets and mechanisms underlying the anti-NAFLD effects of Millettia speciosa Champ. This integrated approach offers novel insights into its pharmacological activity and identifies potential clinical applications for NAFLD management.

非酒精性脂肪性肝病（NAFLD）是世界范围内最常见的慢性肝病，其特征是肝脏中甘油三酯积累过多。它与代谢综合征、2型糖尿病、肥胖和心血管疾病密切相关。在全球肥胖率上升的推动下，NAFLD已成为全球最常见的肝脏疾病。本研究采用液相色谱-串联质谱（LC-MS/MS）技术对密菇的化学成分进行了全面表征。通过网络药理学和分子对接技术相结合，构建了“组分-靶点-通路”网络，阐明了粟特抗nafld的治疗靶点和作用机制。这种综合方法为其药理活性提供了新的见解，并确定了NAFLD治疗的潜在临床应用。

引用次数: 0

Recent advances in antioxidant cerium-based nanozymes: Catalytic mechanisms and bioanalysis/biomedical applications 抗氧化铈基纳米酶的最新进展：催化机制和生物分析/生物医学应用

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-12-01 Epub Date: 2025-09-28 DOI: 10.1016/j.cjac.2025.100640

Mingxi XIA , Litao GE , Alexandr ROGACHEV , Zijian WANG , Huilin WANG

Antioxidant enzymes serve as crucial reactive oxygen species (ROS) scavenging systems in living organisms, capable of efficiently catalyzing the decomposition of excess ROS and playing pivotal roles in anti-aging processes and tumor therapy. However, natural enzymes face significant limitations in practical applications, including limited sources, poor stability, and high production costs. The catalytic mechanisms and precisely organized three-dimensional structures of natural antioxidant enzymes provide important biomimetic insights for designing and developing artificial nanozymes. Among these, cerium-based nanozymes exhibit superior antioxidant-like activity and reaction kinetics due to their unique Ce³⁺/Ce⁴⁺ redox pairs and surface oxygen vacancy structures, demonstrating promising application in biomedical fields. This review systematically summarizes the catalytic mechanisms and biomedical applications of cerium-based antioxidant nanozymes. Building upon the biomimetic catalytic principles of natural catalase, we analyze the structure-activity relationships and performance enhancement strategies of cerium-based antioxidant nanozymes. Furthermore, we highlight recent advances in biomedical applications of cerium-based antioxidant nanozymes and discuss current challenges and future opportunities for their future use.

抗氧化酶是生物体内重要的活性氧（ROS）清除系统，能够有效催化多余ROS的分解，在抗衰老和肿瘤治疗中发挥关键作用。然而，天然酶在实际应用中面临着很大的限制，包括来源有限、稳定性差、生产成本高。天然抗氧化酶的催化机制和精确组织的三维结构为设计和开发人工纳米酶提供了重要的仿生见解。其中，铈基纳米酶由于其独特的Ce3+/Ce4+氧化还原对和表面氧空位结构，表现出优异的抗氧化活性和反应动力学，在生物医学领域具有广阔的应用前景。本文系统地综述了铈基抗氧化纳米酶的催化机理及其在生物医学上的应用。基于天然过氧化氢酶的仿生催化原理，分析了铈基抗氧化纳米酶的构效关系和性能增强策略。此外，我们重点介绍了铈基抗氧化纳米酶在生物医学应用方面的最新进展，并讨论了其未来应用的当前挑战和未来机遇。

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引用次数: 0

Health risk assessments of worker exposure to heavy metals in informal e-waste recycling communities in Chattogram City, Bangladesh 孟加拉国Chattogram市非正式电子废物回收社区工人接触重金属的健康风险评估

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-12-01 Epub Date: 2025-10-10 DOI: 10.1016/j.cjac.2025.100654

Md. Jainal ABEDIN , Supat WANGWONGWATANA , Md. Nurul Huda BHUIYAN , Mohammad MONIRUZZAMAN , Quanyin TAN , Li LIANG

This study aimed to determine the potential contamination of nine heavy metals and their associated health risks in eight locations near informal e-waste recycling facilities in Chattogram City, Bangladesh. The heavy metals detected in indoor air particulate matter were found to contribute the least to the development of carcinogenic and non-carcinogenic risks to workers working in informal e-waste recycling facilities because the residues of the heavy metals detected were all below the maximum permissible levels established by the U.S. OSHA. In assessing the non-carcinogenic risks, it was found that all the heavy metals detected in different environmental media of surface soil, groundwater, and drinking water posed no probability for causing the risks of concern to the e-waste exposed workers as the target hazard quotient (THQ_i) and the total target hazard quotient (TTHQ) for ingestion and dermal contact of the heavy metals were below the USEPA recommended value of 1. The calculated carcinogenic risks showed that the sum of total target risk (TTR_sum) for dermal contact of Cr, Pb, and Ni in groundwater were higher than the USEPA recommended value of 1 × 10^–4. Also, Cr detected in groundwater was considered the major contributor of the carcinogenic risks to potentially exposed workers through dermal contact based on its calculated target risk (TR_der = 1.09E-4). Proper disposal and management of e-waste should be practiced or enforced to mitigate adverse health risks caused by heavy metal exposure to workers, focusing on groundwater contamination by Cr as the most urgent concern in the informal e-waste recycling facilities.

本研究旨在确定孟加拉国Chattogram市非正式电子废物回收设施附近8个地点的9种重金属的潜在污染及其相关健康风险。在室内空气颗粒物中检测到的重金属被发现对在非正式电子废物回收设施工作的工人致癌和非致癌风险的贡献最小，因为检测到的重金属残留量都低于美国OSHA规定的最大允许水平。在非致癌性风险评估中发现，在表层土壤、地下水和饮用水等不同环境介质中检测到的重金属均不可能对接触电子垃圾的工人造成关注风险，重金属的目标危害商（THQi）和摄入和皮肤接触的总目标危害商（TTHQ）均低于USEPA推荐值1。计算结果表明，地下水中Cr、Pb、Ni皮肤接触的总目标风险之和（TTRsum）均高于USEPA推荐值1 × 10-4。此外，根据计算出的目标风险（TRder = 1.09E-4），地下水中检测到的Cr被认为是通过皮肤接触潜在暴露的工人致癌风险的主要因素。应实行或加强对电子废物的适当处置和管理，以减轻重金属接触对工人造成的不利健康风险，重点关注铬对地下水的污染，这是非正式电子废物回收设施中最紧迫的问题。

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引用次数: 0

Fe2O3-functionalized graphite carbon nitride microtube-based electrochemical sensor for sensitive quantification of lead in tobacco and environmental samples 基于fe2o3功能化石墨氮化碳微管的电化学传感器用于烟草和环境样品中铅的敏感定量

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-11-01 Epub Date: 2025-07-09 DOI: 10.1016/j.cjac.2025.100595

Mengxia YANG , Shengbao HE , Fei YANG , Huimin DENG , Yanbo ZENG , Chunqiong WANG , Fengqin CHANG , Guangzhi HU

Lead (Pb) in the environment are a source of environmental pollution and also presents serious risks to public health. Accordingly, developing rapid and effective Pb(II) detection techniques is essential for environmental protection and biosafety. For Pb(II) detection, tubular Fe₂O₃-graphitic carbon nitride (GCN) composites were successfully prepared herein, and the morphology, structure, and chemical composition were characterized by utilizing various characterization techniques. Fe₂O₃-GCN was prepared by modifying GCN with Fe₂O_3, and an Fe₂O₃-GCNNafion/GCE electrochemical sensor was successfully developed. Under the optimal conditions, the electrochemical signals showed linear correlation with the Pb(II) concentration across two ranges, 3‒15 μg/L and 15‒80 μg/L, and achieving a low detection limit (0.084 μg/L). The Fe₂O₃-GCNNafion/GCE electrochemical sensor exhibited excellent stability, resistance to interference, and good applicability in detecting Pb(II) in both surface water and tobacco digestion solution. This study provides a new strategy for heavy-metal sensing in environmental and tobacco samples, while simultaneously expanding the application of GCN composites in sensing platforms.

环境中的铅是环境污染源之一，也对公众健康构成严重威胁。因此，开发快速有效的铅（II）检测技术对环境保护和生物安全至关重要。为了检测Pb(II)，本文成功制备了管状fe2o3 -石墨氮化碳（GCN）复合材料，并利用各种表征技术对其形貌、结构和化学成分进行了表征。用Fe2O3对GCN进行改性制备Fe2O3-GCN，并成功研制了Fe2O3- gcnnafion /GCE电化学传感器。在最佳条件下，电化学信号与Pb（II）浓度在3 ~ 15 μg/L和15 ~ 80 μg/L范围内呈线性相关，且检出限较低（0.084 μg/L）。Fe2O3-GCNNafion/GCE电化学传感器对地表水和烟草消解液中Pb（II）的检测具有良好的稳定性和抗干扰性。本研究为环境和烟草样品中的重金属传感提供了新的策略，同时拓展了GCN复合材料在传感平台中的应用。

{"title":"Fe2O3-functionalized graphite carbon nitride microtube-based electrochemical sensor for sensitive quantification of lead in tobacco and environmental samples","authors":"Mengxia YANG , Shengbao HE , Fei YANG , Huimin DENG , Yanbo ZENG , Chunqiong WANG , Fengqin CHANG , Guangzhi HU","doi":"10.1016/j.cjac.2025.100595","DOIUrl":"10.1016/j.cjac.2025.100595","url":null,"abstract":"<div><div>Lead (Pb) in the environment are a source of environmental pollution and also presents serious risks to public health. Accordingly, developing rapid and effective Pb(II) detection techniques is essential for environmental protection and biosafety. For Pb(II) detection, tubular Fe<sub>2</sub>O<sub>3</sub>-graphitic carbon nitride (GCN) composites were successfully prepared herein, and the morphology, structure, and chemical composition were characterized by utilizing various characterization techniques. Fe<sub>2</sub>O<sub>3</sub>-GCN was prepared by modifying GCN with Fe<sub>2</sub>O<sub>3,</sub> and an Fe<sub>2</sub>O<sub>3</sub>-GCN<img>Nafion/GCE electrochemical sensor was successfully developed. Under the optimal conditions, the electrochemical signals showed linear correlation with the Pb(II) concentration across two ranges, 3‒15 μg/L and 15‒80 μg/L, and achieving a low detection limit (0.084 μg/L). The Fe<sub>2</sub>O<sub>3</sub>-GCN<img>Nafion/GCE electrochemical sensor exhibited excellent stability, resistance to interference, and good applicability in detecting Pb(II) in both surface water and tobacco digestion solution. This study provides a new strategy for heavy-metal sensing in environmental and tobacco samples, while simultaneously expanding the application of GCN composites in sensing platforms.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 11","pages":"Article 100595"},"PeriodicalIF":1.3,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145334700","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Mineralogical-based analysis of the toxicity reduction mechanism in haematitum processing 基于矿物学的赤铁矿处理毒性还原机理分析

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-11-01 Epub Date: 2025-07-05 DOI: 10.1016/j.cjac.2025.100588

Min LU , Cheng-Cheng WANG , Juan LI , Jing MING , Guo-Hua ZHENG , Bi-Sheng HUANG , Yan CAO

Objective

Haematitum is a mineral medicine with a wide range of clinical uses and has been in use for > 2000 years. It has a certain degree of toxicity, so it is usually processed by calcination and quenching methods to reduce its toxic side effects. It is important to clarify the processing mechanism for the further development of haematitum.

Methods

Haematitum and processed haematitum (calcined and vinegar-quenched haematitum) were analyzed by scanning electron microscope, zeta potential analyzer, specific surface and porosity analyzer, X-ray photoelectron spectrometer, inductively coupled plasma mass spectrometer, and advanced mineral identification and characterization system. Moreover, evaluation of haematitum toxicity and procoagulant capacity using a mice model.

Results

The specific surface area of haematitum decreased from 17.04 to 1.42 m²/g and the zeta potential increased from −24.00 to −16.60 mV after processing. Processed haematitum and its major constituents (except quartz) are all larger in particle size than haematitum. The toxic heavy metal elements arsenic and lead in haematitum were reduced by 16.67 % and 30.77 % after processing, respectively. Some of the arsenic (III) elements are oxidized to the much less toxic arsenic (V) elements after processing. The iron (II) elements in haematitum are also partially oxidized to iron (III) elements. High doses of haematitum were toxic to the lungs, liver, and colon of mice, and the toxicity of processed haematitum was significantly reduced. Both before and after haematitum processing had procoagulant effects, and there was no significant difference.

Conclusion

The mineral material properties of haematitum are altered by processing, such as surface properties, mineral composition, elemental composition, and elemental valence. These findings provide evidence that processing reduces the toxicity of haematitum without affecting the efficacy.

目的血血是一种具有广泛临床用途的矿物药物，已有2000多年的历史。它具有一定的毒性，因此通常采用煅烧和淬火的方法进行加工，以减少其毒副作用。阐明赤铁矿的加工机理对赤铁矿的进一步开发具有重要意义。方法采用扫描电镜、zeta电位分析仪、比表面和孔隙度分析仪、x射线光电子能谱仪、电感耦合等离子体质谱仪和先进的矿物鉴定和表征系统对赤铁矿和加工赤铁矿（煅烧和醋淬）进行分析。此外，用小鼠模型评价了赤铁矿的毒性和促凝能力。结果处理后的赤铁矿比表面积由17.04减小到1.42 m2/g， zeta电位由- 24.00增加到- 16.60 mV。加工过的赤铁矿及其主要成分（石英除外）在粒度上都比赤铁矿大。处理后的赤铁矿中有毒重金属元素砷和铅分别降低了16.67 %和30.77 %。一些砷（III）元素在加工后被氧化成毒性小得多的砷(V)元素。赤铁矿中的铁（II）元素也部分氧化为铁（III）元素。高剂量的赤铁矿对小鼠的肺、肝和结肠都有毒性，处理过的赤铁矿的毒性显著降低。赤铁矿处理前后均有促凝作用，差异无统计学意义。结论加工过程改变了赤铁矿的矿物材料性质，如表面性质、矿物组成、元素组成和元素价态。这些发现提供了证据，证明加工可以在不影响功效的情况下减少赤铁矿的毒性。

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引用次数: 0

A novel electrochemical sensor based on Pickering-droplet-derived Cu-MOF microcapsules for simultaneous determination of dopamine and paracetamol 基于皮克林微滴衍生Cu-MOF微胶囊的新型电化学传感器用于同时测定多巴胺和扑热息痛

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-11-01 Epub Date: 2025-09-10 DOI: 10.1016/j.cjac.2025.100623

Danping TIAN , Ruipeng HAO , Yanzi ZHANG , Wanyu XIE , Pei ZHANG , Wenbo LU

A novel electrochemical sensing platform was developed based on copper-based metal-organic framework (Cu-MOF) microcapsules synthesized via a Pickering emulsion templating approach, where carbon nanoparticles used as solid emulsifiers to enhance electrode interfacial interactions and material conductivity. This design synergistically combines the superior catalytic activity of Cu-MOF with the conductive carbon matrix. The Cu-MOF microcapsules were applied in the modification of a glassy carbon electrode to obtain an electrochemical sensor for simultaneous detection of dopamine and paracetamol. This sensor showed the good sensing performance with a broad linearity range (2–1600 μM for dopamine and 2–6500 μM for paracetamol) and low detection limits (1.69 μM for dopamine and 1.81 μM for paracetamol at S/N = 3). This platform also demonstrated excellent reproducibility (RSD < 3 %) and selectivity against common interferents, highlighting its potential for practical applications in real sample detection.

基于Pickering乳液模板法合成的铜基金属有机骨架（Cu-MOF）微胶囊，开发了一种新型电化学传感平台，其中碳纳米颗粒作为固体乳化剂增强电极界面相互作用和材料导电性。该设计将Cu-MOF优异的催化活性与导电碳基体协同结合。利用Cu-MOF微胶囊对玻碳电极进行修饰，得到了一种同时检测多巴胺和扑热息痛的电化学传感器。该传感器具有较宽的线性范围（多巴胺为2 ~ 1600 μM，扑热息痛为2 ~ 6500 μM）和较低的检出限（S/N = 3时，多巴胺为1.69 μM，扑热息痛为1.81 μM）。该平台还显示出出色的再现性（RSD < 3%）和对常见干扰的选择性，突出了其在实际样品检测中的实际应用潜力。

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引用次数: 0

Self-sufficient Fenton-Like Degradation by Cu-TA Encapsulated Melamine Sponge Cu-TA包封三聚氰胺海绵自给式fenton类降解研究

4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-11-01 DOI: 10.1016/j.cjac.2025.100680

Y. Y. Chen, Peng Zhou, Jiwei Wang, Bei Jiang

Water contamination is a severe and urgent issue, and advanced oxidation processes (AOPs) offer promising solutions for water purification. Among these, copper-based Fenton-like reaction demonstrate advantages such as rapid reaction kinetics and low reduction potential. However, a major limitation of most Fenton-like reactions is their reliance on externally added H 2 O 2 , which poses risks in transportation, storage, and management. To address this, developing self-sufficient Fenton-like systems with in-situ H 2 O 2 generation is critical. In this study, we conjugated copper ions (Cu 2+ ) and tannic acid (TA) on a melamine sponge (MS) substrate to fabricate a self-sufficient Fenton-like catalyst (MS-Cu-TA). MS exhibits high porosity and absorbency, which facilitate efficient liquid absorption for the degradation process. The H 2 O 2 content generated by a single MS-Cu-TA sponge was determined as ∼0.19 mmol, which was sufficient to sustain the Fenton-like reaction. Methylene Blue (MB) degradation results showed that MS-Cu-TA achieved comparable degradation efficiency (∼60% within 0.5 h) without exogenous H 2 O 2 . Notably, in this specific dye degradation process, adsorption and degradation occurred simultaneously. Results from reactive oxygen species (ROS) quenching tests and electron paramagnetic resonance (EPR) spectroscopic analysis revealed that the dominant ROS generated is •OH, which originates from in-situ formed H 2 O 2 . The in-situ H 2 O 2 generation is likely attributed to the auto-oxidation of TA, which acts as both reducing agent and H 2 O 2 precursor. Concurrently, TA reduces Cu 2+ to Cu + , which catalyzes H 2 O 2 to generate hydroxyl radicals (•OH) via a Fenton-like reaction. This work provides valuable insights for developing self-sufficient Fenton-like systems in wastewater treatment. In this study, we conjugated copper ions (Cu 2+ ) and tannic acid (TA) on a melamine sponge (MS) substrate to fabricate a self-sufficient Fenton-like catalyst (MS-Cu-TA). The in-situ H 2 O 2 generation is likely attributed to the auto-oxidation of TA, which acts as both a reducing agent and H 2 O 2 precursor. Concurrently, TA reduces Cu 2+ to Cu + , which catalyzes H 2 O 2 to generate hydroxyl radicals (•OH) via a Fenton-like reaction.

水污染是一个严重而紧迫的问题，高级氧化工艺（AOPs）为水净化提供了有前途的解决方案。其中，铜基类芬顿反应表现出反应动力学快、还原电位低等优点。然而，大多数芬顿类反应的一个主要限制是它们依赖于外部添加的h2o2，这在运输、储存和管理方面存在风险。为了解决这个问题，开发自给自足的类芬顿系统，就地生成h2o2是至关重要的。在这项研究中，我们在三聚氰胺海绵（MS）底物上共轭铜离子（cu2 +）和单宁酸（TA），制备了自给自足的类芬顿催化剂（MS-Cu-TA）。质谱具有较高的孔隙率和吸光度，有利于降解过程中有效的液体吸收。测定单个MS-Cu-TA海绵产生的h2o2含量为~ 0.19 mmol，足以维持芬顿样反应。降解亚甲基蓝（MB）的结果表明，MS-Cu-TA在没有外源h2o2的情况下达到了相当的降解效率（0.5 h内约60%）。值得注意的是，在这个特定的染料降解过程中，吸附和降解同时发生。活性氧（ROS）猝灭实验和电子顺磁共振（EPR）光谱分析结果表明，生成的活性氧主要是•OH，其来源于原位形成的h2o2。原位生成h2o2可能是由于TA的自氧化作用，TA既是还原剂又是h2o2前体。同时，TA将cu2 +还原为Cu +，通过Fenton-like反应催化h2o2生成羟基自由基（•OH）。这项工作为开发自给自足的废水处理类芬顿系统提供了有价值的见解。在这项研究中，我们在三聚氰胺海绵（MS）底物上共轭铜离子（cu2 +）和单宁酸（TA），制备了自给自足的类芬顿催化剂（MS-Cu-TA）。原位生成h2o2可能是由于TA的自氧化作用，TA既是还原剂又是h2o2前体。同时，TA将cu2 +还原为Cu +，通过Fenton-like反应催化h2o2生成羟基自由基（•OH）。

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引用次数: 0

Online-coupled electromembrane extraction and HPLC as a highly efficient, selective and clean microextraction technique for determination of ultra-trace levels of tramadol in biological fluids 在线耦合电膜萃取-高效液相色谱微萃取技术测定生物体液中超痕量曲马多

IF 1.3 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-11-01 Epub Date: 2025-07-19 DOI: 10.1016/j.cjac.2025.100602

Somayeh ARGHAVANI-BEYDOKHTI , Nematollah NOORI , Alireza ASGHARI , Hamidreza HAGHGOO QEZELJE , Fatemeh MEMARIAN , Mahesh Kumar SAH , Ahmad HOSSEINI-BANDEGHARAEI , Maryam RAJABI

A highly efficient microextraction method namely electromembrane extraction coupled online with high performance liquid chromatography (HPLC) apparatus is proposed for extremely selective and accurate measurement of tramadol drug in the human bio-fluid matrix. The method established utilizes a polypropylene sheet as a support for the liquid membrane (1-octanol, 15 µL), which is situated within a poly(methyl methacrylate) cell. 10 mL of donor solution (pH 13.0) is continuously circulated within the extraction cell; it is delineated from the acceptor medium (pH=1.0, 100 µL) through supported liquid membrane (SLM), facilitating selective extraction of target analyte from donor solution to acceptor solution through the membrane interface. This methodology is notably convenient and eco-friendly. It can easily be completely automated, and concurrently addressing all the sample pretreatment goals. This method utilizes an aqueous-phase extractant and enhances sample clean-up by blocking macromolecule extraction through the membrane. To attain the best optimal conditions, the factors influencing extraction efficiency of proposed method were investigated and optimized. Underneath ideal conditions, the proposed method provided an appropriate linearity in a span of 10–1000 ng mL^–¹ (R² = 0.998), good limit of detection (3.0 ng mL^–¹), and remarkable extraction repeatability (RSD, 3.9 %). The applicability of the method was assessed through analyses of human urine and plasma fluids, and the results attained revealed the exceptional ability of method in the complicated matrices’ analysis.

提出了一种高效的微萃取方法，即电膜萃取与高效液相色谱（HPLC）在线耦合，用于人体生物液基质中曲马多药物的极选择性和精确测定。所建立的方法利用聚丙烯片作为液体膜（1-辛醇，15µL）的支撑，液体膜位于聚（甲基丙烯酸甲酯）细胞内。10 mL供体溶液（pH 13.0）在萃取池内连续循环；它从受体介质（pH=1.0, 100µL）通过支撑液膜（SLM）划定，便于通过膜界面从供体溶液选择性地提取目标分析物到受体溶液。这种方法非常方便和环保。它可以很容易地完全自动化，并同时处理所有样品预处理目标。该方法利用水相萃取剂，并通过阻断大分子通过膜的萃取来提高样品的清洁度。为获得最佳提取条件，对影响该方法提取效率的因素进行了研究和优化。在理想条件下，该方法在10 ~ 1000 ng mL-1范围内具有良好的线性关系（R2 = 0.998），良好的检出限（3.0 ng mL-1），具有良好的提取重复性（RSD为3.9 %）。通过对人体尿液和血浆的分析，对该方法的适用性进行了评估，结果显示了该方法在复杂基质分析中的卓越能力。

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