【特约专题】

磷手性二氢苯并氧杂膦烷配体在催化与合成中的应用

曹振¹，徐广庆¹，罗林¹，汤文军^*1,2,3

(1. 绍兴赜军生物医药科技有限公司 研发部，浙江绍兴  312369；2. 中科院上海有机化学研究所 生命过程小分子调控国家重点实验室，上海  200032；3. 国科大杭州高等研究院 化学和材料科学学院，浙江杭州  310024)

摘要：直到Knowles开发的磷手性配体CAMP和DIPAMP在不对称氢化反应中的成功应用，磷手性配体才受到广泛关注。尽管后来开发出了众多活性优异的磷手性配体，但大多都对空气敏感且结构难以修饰，阻碍了其在学术研究和工业中的应用。磷手性二氢苯并氧杂膦烷配体是一类大位阻、富电子、结构可调且性质稳定的膦配体，在过去的10年中，百余个基于该骨架的膦配体已被开发报道并成功应用多种有机化学转化。总结了该类配体在催化和合成中的应用，主要包括大位阻偶联反应、加成反应、环化反应及氢化反应，并着重强调其在不对称催化和合成包括不对称偶联、不对称碳氢键活化及不对称去芳构环化反应中的诸多独特催化特性。磷手性二氢苯并氧杂膦烷配体有望在不对称催化、药物绿色工艺开发及工业化生产中发挥着更加突出的作用。

关键词：磷手性；二氢苯并氧杂膦烷；结构可调；不对称；催化与合成

中图分类号：O62                   文献标识码：A               文章编号：0258-3283（2025）--

DOI：10.13822/j.cnki.hxsj.2025.0251

Application of P-Chiral Dihydrobenzooxaphosphole Ligands in Catalysis and Synthesis CAO Zhen¹, XU Guang-qing¹, LUO Lin¹, TANG Wen-jun^*1,2,3 (1. R&D Center, Shaoxing Zejun Pharmaceuticals Co., Ltd, Shaoxing 312369, China; 2.State Key Laboratory of Chemical Biology, Center for Excellence in Molecular Synthesis, Shanghai Institute of Organic Chemistry, University of Chinese Academy of Sciences, Shanghai 200032, China; 3.School of Chemistry and Materials Science, Hangzhou Institute for Advanced Study, University of Chinese Academy of Sciences, Hangzhou 310024, China )

Abstract：P-Chiral phosphorus ligands did not receive widespread attention in organic chemistry until Knowles made his landmark contribution in asymmetric hydrogenation by developing P-chiral ligands CAMP and DIPAMP. Although numerous P-chiral ligands with high catalytic activity have been subsequently developed, most of them are air-sensitive or lack of structural modularity, impeding their practical application in chemical industry. P-Chiral dihydrobenzooxaphosphole ligands represent a class of sterically bulky, electron-rich, structurally tunable, and chemically stable phosphorus ligands. Over the past decade, more than one hundred variants based on this scaffold have been reported and successfully applied in diverse organic transformations. This review comprehensively summarized the applications of these ligands in catalysis and synthesis, encompassing sterically hindered coupling reactions, addition reactions, cyclization reactions, and hydrogenation reactions. Special emphasis was placed on their unique catalytic properties in asymmetric catalysis and synthesis, such as asymmetric couplings, asymmetric C?H activation, and asymmetric dearomative cyclization. These P-chiral dihydrobenzooxaphosphole ligands are expected to play an increasingly prominent role in asymmetric catalysis, green process development for pharmaceuticals and industrial-scale production.

Key words：P-chiral; dihydrobenzooxaphosphole; structurally tunable; asymmetric; catalysis and synthesis

阴离子交换膜用于电催化CO₂还原的研究进展

王佑庭¹，曹媛媛^*2，魏荣耀¹，范茹¹，吕晶晶¹，吴芬^*1，王正军^1,3

(1. 温州大学化学与材料工程学院新材料与产业技术研究院，浙江温州  325035；

2. 杭州中一检测研究院有限公司，浙江杭州  311258；

3. 温州市生物功能材料与化学重点实验室，浙江温州  325035)

摘要：随着化石燃料的大量使用，温室气体的排放，尤其是二氧化碳等温室气体的大量排放，引起了一系列的环境问题，通过电催化二氧化碳还原（eCO₂RR）可以将其转化为高价值的燃料/商品化学品，为上述问题提供了技术支撑，而近年来随着反应器的设计改进进一步提高了该技术的经济可行性。在CO₂RR反应器中离子交换膜（IEM）对于二氧化碳转化为有用产品的能量效率方面起着关键作用，每种离子交换膜都有着不同的优缺点，而其中阴离子交换膜（AEM）往往表现出更高的效率和产物选择性等优点，在CO₂RR中具备巨大的应用潜力。综述了近年来国内外研究者对于AEM在eCO₂RR中的研究进展，介绍了AEM的作用机制、合成方法、性能评价标准以及近期报道的新型AEM，随后重点关注了这些AEM的设计思路、优化策略，特别是对于其化学稳定性、转化效率、机械强度等方面，最后对于未来AEM设计的挑战和机遇进行了展望。

关键词：温室气体；电催化二氧化碳还原；阴离子交换膜；制备方法；应用

中图分类号：O64    文献标识码：A            文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0171

Research Progress on Anion Exchange Membranes for Electrocatalytic CO₂ Reduction WANG You-ting¹, CAO Yuan-yuan^*2, WEI Rong-yao¹, FAN Ru¹, LV Jing-jing¹, WU Fen^*1, WANG Zheng-jun^1,3 (1. Institute of New Materials and Industrial Technologies, College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China; 2. Zhejiang Zhongyi Testing and Research Institute Co., Ltd., Hangzhou 311258, China; 3. Wenzhou Key Laboratory of Biomaterials and Chemical Functional Materials, Wenzhou 325035, China)

Abstract: With the large use of fossil fuels, the emission of greenhouse gases, especially greenhouse gases such as carbon dioxide, has caused a series of environmental problems. It can be converted into high-value fuel/commodity chemicals through electrocatalytic carbon dioxide reduction (eCO₂RR), providing technical support for the above problems. In recent years, the economic feasibility of the technology has been further improved with the improvement of reactor design. Ion exchange membrane (IEM) plays a key role in the energy efficiency of converting carbon dioxide into useful products in CO₂RR reactors. Each ion exchange membrane has different advantages and disadvantages, and anion exchange membrane (AEM) often exhibits higher efficiency and product selectivity, and has huge application potential in CO₂RR. The research progress of AEM in eCO₂RR in recent years was reviewed, and the mechanism of action, synthesis method, performance evaluation standards and the new AEM reported recently were introduced. Then we focused on the design ideas and optimization strategies of these AEMs, especially in terms of their chemical stability, conversion efficiency and mechanical strength. Finally, the challenges and opportunities of AEM design in the future were prospected.

Key words: greenhouse gas; electrocatalytic carbon dioxide reduction; anion exchange membrane; preparation method; application

【综述与专论】

肉桂精油研究与应用进展

朱紫琪，何静金，余昆莹，钟海艺^*

（广西中医药大学药学院，广西南宁  530000）

摘要：肉桂精油作为一种天然活性物质，其化学组成复杂，包含肉桂醛、δ-杜松烯、苯甲醇等化合物；这些成分相互协同，赋予了肉桂精油广泛的药理作用，包括抗菌、抗氧化、驱虫、抗真菌和抗肿瘤等多种活性功效，被广泛应用于食品保鲜防腐、医药等领域。归纳总结了肉桂精油的常用的提取方法，包括水蒸气蒸馏、超临界二氧化碳萃取法和低共熔溶剂提取法，并概述了各法的萃取原理及其优缺点，为肉桂精油的提取提供参考。同时总结归纳了不同品种、部位所提取的肉桂精油的活性成分和含量，可以得知肉桂的产地和品种也是造成肉桂精油成分和含量差异的重要因素。除此之外，还分别阐述了抗菌、抗氧化、驱虫、抗真菌和抗肿瘤5种生物活性的作用机制和特点。最后通过对国内外研究进行展望，系统简述了肉桂精油在食品保鲜和医疗卫生事业的应用和作用机制，肉桂精油通过抗氧化、抑菌等特性在延长食品保质期方面展现出显著潜力；在医疗卫生领域，其抗炎、抗肿瘤及调节血糖等作用机制为治疗炎症性疾病、癌症及糖尿病提供了新思路。以期为肉桂精油的开发和应用提供理论参考，推动其在更多领域发挥更大的作用。

关键词：肉桂；精油；提取方法；活性成分；实际应用

中图分类号：O631.1         文献识别码：A         文章编号：0258-3283（2025）--

DOI：10.13822/j.cnki.hxsj.2025.0125

Research and Application Progress of Cinnamon Essential Oil ZHU Zi-qi, HE Jing-jin, YU Kun-ying, ZHONG Hai-yi^*（College of Pharmacy, Guangxi University of Chinese Medicine, Nanning 530000, China）

Abstract：Cinnamon essential oil (CEO), as a natural bioactive substance, possesses a complex chemical composition encompassing compounds such as cinnamaldehyde, δ-cadinene, and benzyl alcohol. These constituents act synergistically, endowing CEO with a broad spectrum of pharmacological activities, including antibacterial, antioxidant, insecticidal, antifungal, and antitumor properties. As a result, CEO finds extensive applications in food preservation, pharmaceuticals, and other fields. This paper summarized the commonly used extraction methods for CEO, including steam distillation, supercritical carbon dioxide extraction, and deep eutectic solvent extraction. The extraction principles, advantages, and disadvantages of each method were outlined to provide a reference for efficient CEO extraction. Additionally, the active components and their concentrations in CEO extracted from different cinnamon varieties and plant parts were summarized, revealing that the geographic origin and species of cinnamon significantly influence the chemical profile and content of CEO. The mechanisms and characteristics of five major biological activities, antibacterial, antioxidant, insecticidal, antifungal, and antitumor, were also elucidated. Finally, by reviewing both domestic and international research, the applications and action mechanisms of CEO in food preservation and healthcare were systematically discussed. CEO demonstrated significant potential in extending food shelf life through its antioxidant and antibacterial properties. In the medical field, its anti-inflammatory, antitumor, and blood glucose-regulating effects offered new insights for the treatment of inflammatory diseases, cancer, and diabetes. This review aimed to provide a theoretical foundation for the development and application of CEO, promoting its broader utilization in various fields.

Key words：cinnamon; essential oils; extraction method; active ingredients; practical application

光催化和电化学在连续流合成中的研究进展

杨宏勋¹，凌芳^*2，智俊峰³，查晓明³

国药集团化学试剂有限公司，上海  200002；2. 上海沃凯生物技术有限公司，上海  201507；3. 中国药科大学 工学院，江苏南京  211198）

摘要：近年来，连续流合成技术取得了重要进展，基于微观尺度与连续流动过程的协同作用，能够实现反应过程的精准控制，解决了传统釜式反应的诸多不足，已广泛应用于医药化工行业的生产。光催化和电化学反应作为过程强化的手段，应用于连续流合成中，增强反应过程的同时还可以减少污染。连续流技术与光电催化的融合代表了绿色化学的发展方向，这一创新体系通过将能量耦合，催化协同及反应路径优化，实现了高效、精准、可持续的化学转化。连续流反应器的微通道设计强化了传质与传热效率，使反应时间从数小时缩短至分钟级甚至秒级；光电催化过程无需添加有害催化剂，减少了废弃物的排放，原子经济性高，符合绿色化学理念。连续流技术在原料药、医药中间体等的合成中展现出独特的优势。对近年来光电催化技术应用于连续流合成中的研究进展进行了总结和展望。

关键词：连续流合成；光催化；电化学；过程强化；研究进展

中图分类号：O69           文献标识码：A          文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0261

Recent Progress of Photocatalysis and Electrochemistry in Continuous Flow Synthesis  YANG Hong-xun¹, LING Fang*², ZHI Jun-feng³, ZHA Xiao-ming³ (1.Sinopharm Chemical Reagent Co., Ltd., Shanghai 200002, China; 2.Shanghai Our Chem Bio-Technology Co., Ltd., Shanghai 201507, China; 3. School of Engineering, China Pharmaceutical University, Nanjing 211198, China)

Abstract:In recent years, significant advancements have been achieved in continuous flow synthesis technology. Leveraging the synergistic effect between microscale dimensions and continuous flow processes, this technology enables the enhancement of mass and heat transfer during reactions as well as the precise control of process parameters. It addresses numerous limitations of traditional batch reactor systems and has been widely applied in the production processes of the pharmaceutical and chemical industries. As effective means of process intensification, photocatalytic and electrochemical reactions are integrated into continuous flow synthesis. This not only enhances the reaction process but also reduces pollution. The integration of continuous flow technology with photoelectrocatalysis represents a developmental direction of green chemistry. Through energy coupling, catalytic synergy, and reaction pathway optimization, this innovative system achieves efficient, precise, and sustainable chemical transformations.The microchannel design of continuous flow reactors enhances mass and heat transfer efficiency, shortening reaction times from the traditional several hours to the minute or even second scale. The photoelectrocatalytic and electrochemical process eliminates the need for harmful catalysts, reducing waste generation with high atom economy, which is in line with the concept of green chemistry. Continuous flow technology has demonstrated unique advantages in the synthesis of key intermediates and compounds requiring multi-step reactions. This paper summarized the recent research progress in the application of photoelectrocatalytic technology in continuous flow synthesis and provided an outlook for future development.

Key words:continuous flow synthesis; photocatalysis; electrochemistry; process intensification;research progress

【生化与药用试剂】

药物共晶缓释制剂研究进展

张顺，吴海丽，陈玲，林宁，陈清^*

（广西中医药大学中医药壮瑶医药研究院广西壮瑶药技术创新中心，广西南宁  530200）

摘要：缓释制剂通过理性设计实现药物的缓慢释放，维持平稳的血药浓度、避免峰谷现象，有利于降低药物的毒副作用。对于半衰期短的药物，缓释技术可降低给药频率，提高患者依从性和治疗效果。药物的溶解度及溶出行为与其晶格稳定性及分子间相互作用等固体性质密切相关。研究表明，对于治疗窗窄、半衰期短或局部刺激性大的药物，可通过固体性质的调控实现缓释制剂的优化设计。近年来，引入共形成物制备成为药物共晶，已成为改善药物性能的创新策略。该技术通过分子间超分子作用显著提升药物的晶格稳定性，进而调控其溶出动力学。对近年来具有缓释潜力的药物共晶研究进展进行综述，探讨了共晶技术通过分子间相互作用调控药物理化性质和释放行为的机制原理，基于不同种类药物的临床治疗需求系统分析了现有药物在溶解度、释放特性和生物利用度等方面面临的问题，总结了药物共晶技术在改善这些药物性能方面的独特优势。为基于共晶技术的新型缓释制剂的研发和临床应用提供了重要的理论依据和实践指导。

关键词：药物共晶；缓释制剂；晶格稳定性；溶出度；生物利用度；治疗效果

中图分类号：O64；R943      文献标识码：A       文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0130 

Research Progress on Pharmaceutical Cocrystal Sustained-Release Formulations ZHANG Shun, WU Hai-li, CHEN Ling, LIN Ning, CHEN Qing^*(Guangxi Scientific Research Center of Traditional Chinese Medicine, Guangxi University of Chinese Medicine, Nanning 530200, China) 

Abstract：Sustained release formulations achieve slow drugs release through rational design, maintain stable blood drug concentrations and reducing peak-trough phenomena, and significantly reduce drug toxicity and side effects. For drugs with short half-lives, sustained-release technology can reduce the frequency of administration, improve patient compliance, and enhance treatment efficacy. The solubility and dissolution behavior of drugs are closely related to their solid properties, such as crystal lattice stability and intermolecular interactions. Research indicates that for drugs with narrow therapeutic windows, short half-lives, or high local irritations, the optimization design of sustained-release formulations can be achieved through the regulation of solid properties. In recent years, the introduction of suitable coformants to prepare drug cocrystals, thereby enhancing drug crystal lattice stability and intermolecular interactions, has become an important means of improving drug performance. This technology significantly enhances the lattice stability of drugs through intermolecular supramolecular interactions, thereby regulating their dissolution kinetics. This paper reviewed recent research progress on pharmaceutical cocrystals with sustained-release potential, explored the mechanisms and principles by which cocrystal technology regulates the physicochemical properties and release behavior of drugs through intermolecular interactions, and then systematically analyzed the issues faced by existing drugs in terms of solubility, release characteristics, and bioavailability based on the clinical treatment needs of different types of drugs. It summarized the unique advantages of drug cocrystal technology in improving these drug properties. The review provided critical theoretical and practical guidance for developing cocrystal-based sustained-release formulations.

Key words：pharmaceutical cocrystal; sustained-release formulation;lattice stability; dissolution; biovailability; therapeutic effect

【功能材料】

镉配合物荧光传感检测抗生素的研究进展

朱浩如¹，马新晶¹，白成洁¹，孙赞^*1,2

（1.青海民族大学 化学与材料科学学院，青海 西宁  810007；2.青藏高原资源化学与生态环境保护国家民委重点实验室，青海 西宁  810007）

摘要：近年来，抗生素（包括青霉素类、四环素类、头孢菌类、喹诺酮类、大环内酯类等）的滥用导致其成为水环境中的首要有机污染物，其引发的后果是一个贯穿生态环境、公众健康与医疗体系的连锁反应，且危害程度随时间推移不断加剧。在生态方面，抗生素的残留会破坏水体菌群平衡，催生耐药菌，污染水产品。在健康方面，抗生素的残留会扰乱肠道菌群、削弱免疫力，耐药菌感染还使常规治疗失效，延长病程且增加费用。在医疗方面，耐药性会导致抗生素的保护作用减弱，甚至可能面临“无药可用”风险。传统的抗生素检测方法包括酶免疫分析法、色谱-串联质谱法、离子迁移谱法和表面增强拉曼光谱法等，具有诸多缺点，例如需要复杂的样品预处理过程、较高的时间成本和昂贵的检测设备等，而基于镉配合物的荧光传感器由于具有良好的配位多样性、结构可调性、优异的光物理和光化学性质，因而具有低成本、实时观测、高灵敏度和操作简单等优势，已成为检测抗生素的首选技术之一。总结了镉配合物检测抗生素的最新进展、探讨了配合物的结构设计策略以及作用机理，此外还总结了镉配合物检测抗生素的不足之处、展望了未来的发展趋势。

关键词：镉配合物；抗生素；荧光检测；机理；结构设计

中图分类号：O641.4                文献标识码：A             文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0219

Research Progress on Fluorescence Sensing of Antibiotics Using Cadmium Coordination Polymers Zhu Hao-ru¹, Ma Xin-jing¹, Bai Cheng-jie¹, Sun Zan^*1,2 (1. School of Chemistry and Materials Science, Qinghai Minzu University, Xining 810007, China; 2 Key Laboratory of Resource Chemistry and Eco-environmental Protection in Tibetan Plateau, State Ethnic Affairs Commission, Xining 810007, China)  

Abstract：In recent years, the abuse of antibiotics (including penicillins, tetracyclines, cephalosporins, quinolones, macrolides antibiotics and so on) has led to them becoming the primary organic pollutants in the aquatic environment. The consequences caused by the abuse of antibiotics constitute a chain reaction that spans the ecological environment, public health, and medical system, with the degree of harm escalating as the abuse persists over time. Ecologically, residual antibiotics disrupt the balance of microbial communities in water bodies, promote the emergence of drug-resistant bacteria, and contaminate aquatic products. From the health perspectives, residual antibiotics can disrupt the intestinal flora, weaken the immune system when humans are exposed to them through contaminated water and food. Additionally, infections caused by drug-resistant bacteria render conventional treatments ineffective, prolonging the course of illness and increasing medical costs. In the medical field, drug resistance can lead to a weakened protective effect of antibiotics, and may even face the risk of "no drug available". Traditional antibiotic detection methods include enzyme immunoassay, chromatography tandem mass spectrometry, ion mobility spectrometry, and surface enhanced Raman spectroscopy, which have many disadvantages such as requiring complicated sample pretreatment processes, high time costs, and expensive detection equipment. However, fluorescence sensors based on cadmium coordination polymers have the advantages of low cost, real-time observation, high sensitivity, and simple operation due to their good coordination diversity, structural tunability, excellent photophysical and photochemical properties, and have become one of the preferred technologies for detecting antibiotics. This review summarized the latest advances in the detection of antibiotics using cadmium coordination polymers, explored the structural design strategies and action mechanisms, and additionally concluded the shortcomings of cadmium coordination polymers in antibiotic detection as well as looks ahead to the future development trends.

Key words：cadmium coordination polymers; antibiotics; fluorescence detection; mechanism; structure design

Zn/U异核铀酰MOF的构筑及其荧光传感性能研究

吕艳羽¹，许莹莹¹，司贞秀^*1，戴晓侠¹，姜凌云¹，许伟²

（1. 山东药品食品职业学院 制药工程系，山东 威海  264200；2. 宁波大学 材料科学与化学工程学院，浙江 宁波  315211）  

摘要：谷氨酸（Glu）在生物代谢、食品风味及疾病诊断中具有关键作用，建立快速、灵敏的Glu检测方法对神经科学研究、食品安全监控及临床诊断具有重要意义。基于异核构筑策略开发一种高性能荧光传感材料，以实现对Glu的高选择性识别。通过溶剂热法成功合成了一例新型异核铀酰有机骨架材料［Zn(UO₂)(ntp)₂(5,5'-dm-2,2'-bpy)₂(H₂O)］（H₂ntp = 2-硝基对苯二甲酸，5,5'-dm-2,2'-bpy = 5,5'-二甲基-2,2'-联吡啶），并通过单晶X-射线衍射、荧光光谱和紫外-可见吸收光谱等手段对其结构和光学性能进行了系统表征。荧光传感研究表明，该材料对Glu表现出优异的选择性与灵敏性，呈现显著荧光猝灭效应，检出限（LOD）为0.953 μmol/L。此外，该传感器具备良好的抗干扰能力和循环稳定性。机理研究证实，荧光猝灭源于光诱导电子转移（PET）过程。为锕系异金属MOFs在氨基酸荧光传感领域的应用提供了新思路，展现出潜在的实际应用价值。

关键词：异核；铀酰金属有机骨架；晶体结构；荧光传感；谷氨酸

中图分类号：O65                 文献标识码：A            文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0197

Zn/U Heterobimetallic Uranyl Metal-Organic Framework: Synthesis and Fluorescent Sensing Performance LV Yan-yu ¹, XU Ying-ying¹, SI Zhen-xiu ^*1, DAI Xiao-xia ¹, JIANG Ling-yun ¹, XU Wei ²（1. Department of Pharmaceutical Engineering, Shandong Drug And Food Vocational College, Weihai 264200, China ; 2. School of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China）

Abstract: Glutamic acid (Glu) plays a critical role in biological metabolism, food flavor formation, and disease diagnosis. Therefore, establishing a rapid and sensitive method for detecting Glu is of great significance for neuroscience research, food safety monitoring, and clinical diagnosis. A high-performance fluorescent sensing material was developed based on a heteronuclear construction strategy to achieve highly selective recognition of Glu. A novel heteronuclear uranyl organic framework material, [Zn(UO₂)(ntp)₂(5,5'-dm-2,2'-bpy)₂(H₂O)] (where H₂ntp = 2-nitroterephthalic acid, 5,5'-dm-2,2'-bpy = 5,5'-dimethyl-2,2'-bipyridine), was successfully synthesized via a solvothermal method. Its structure and optical properties were systematically characterized using single-crystal X-ray diffraction, fluorescence spectroscopy, and UV-Vis absorption spectroscopy. Fluorescence sensing studies demonstrated that the material exhibits excellent selectivity and sensitivity toward Glu, showing a significant fluorescence quenching effect with a limit of detection (LOD) of 0.953 μmol/L. Furthermore, the sensor possesses good anti-interference ability and cycling stability. Mechanistic studies confirmed that the fluorescence quenching originates from a photoinduced electron transfer (PET) process. This research provided new insights into the application of actinide-based heterometallic MOFs in amino acid fluorescence sensing and demonstrates potential for practical applications.

Keywords: heteronuclear; uranyl metal-organic framework; crystal structure; fluorescence sensing; glutamic acid

一种苯并吡喃酮荧光探针对Zn²⁺的检测研究

覃姣兰，梁武华，袁涛^*，范歆晨，黄如川，何厚贤

（百色学院广西城市水环境重点实验室，广西百色 533000）

摘要：为设计合成香豆素衍生物荧光探针以实现对金属离子的高选择性、高灵敏识别，并为实际水样中Zn²⁺检测提供理论与应用参考，以香豆素衍生物3-（1H-苯并[d]咪唑-2-基）-7-（二乙氨基）-2H-苯并吡喃-2-酮（BDC）为荧光探针，在乙醇-水混合体系（V（乙醇）:V（水）=1:1）中，通过荧光光谱法研究其对多种金属离子的识别性能，同时采用Job's Plot实验与X-单晶衍射实验解析探针与目标离子的配合机制，并考察探针的线性响应范围、检出限、响应时间及实际水样适用性。研究结果表明，BDC探针对Zn²⁺表现出特异性识别能力，与Zn²⁺作用后荧光显著增强，且不受其他共存金属离子干扰；探针荧光强度与Zn²⁺浓度在特定范围内呈良好线性关系（R²=0.9921），检出限低至0.117 μmol/L，响应时间短（≤0.5 min）。Job's Plot 实验与X-单晶衍射实验进一步证实BDC可与Zn²⁺形成稳定配合物，其荧光增强效应源于配合作用引发的螯合荧光增强（CHEF）效应。综上，BDC 荧光探针具备对Zn²⁺的高选择性、高灵敏性及快速响应特性，可成功应用于实际水样中Zn²⁺的检测，为香豆素类金属离子识别探针的设计与应用提供了有效借鉴。

关键词：香豆素；荧光探针；锌离子检测；光谱研究；荧光增强

中图分类号：O657.3          文献标识码：A         文章编号： 0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0220

Study on Detection of Zn²⁺ by a Benzopyrone Fluorescent Probe QIN Jiao-lan, LIANG Wu-hua, YUAN Tao^*, FAN Xin-chen, HUANG Ru-chuan, He Hou-xian（Guangxi Key Laboratory of Urban Water Environment, Baise University, Baise 533000, China）

Abstract: To design and synthesize coumarin-derived fluorescent probes with highly selectivity and sensitivity for metal ion recognition, as well as to provide theoretical and application references for Zn²⁺ detection in real water samples, this study employed the coumarin derivative 3-(1H-benzo[d]imidazol-2-yl)-7 -(diethylamino)-2H-chromen-2-one (BDC) as a fluorescent probe. In V（ethanol）:V（water）=1:1, the recognition performance of BDC towards various metal ions was investigated via fluorescence spectroscopy. Meanwhile, Job's Plot analysis and X-ray single-crystal diffraction were used to analyze the complexation mechanism between the probe and the target ion. The linear response range, limit of detection (LOD), response time, and applicability of the probe in real water samples were also evaluated. The results showed that BDC exhibited specific recognition ability towards Zn²⁺, with a significant fluorescence enhancement upon interaction with Zn²⁺, with negligible interference from other coexisting metal ions. The fluorescence intensity of BDC showed a good linear relationship with Zn²⁺ concentration within a certain range (R²= 0.9921), with a low LOD of 0.117 μmol/L and a rapid response time (≤0.5 min). Furthermore, Job's Plot analysis and X-ray single-crystal diffraction confirmed that BDC form a stable complex with Zn²⁺, and the fluorescence enhancement effect was attributed to the chelation-enhanced fluorescence (CHEF) effect induced by the complexation.In conclusion, the BDC fluorescent probe possesses high selectivity, high sensitivity, and rapid response characteristics for Zn²⁺, and can be successfully applied to the Zn²⁺ detection in real water samples. This study provided valuable insights for the design and application of coumarin-based fluorescent probes for metal ion recognition.

Key words: coumarin；fluorescent probe；Zn²⁺ detection；spectroscopic study; fluorescence enhancement

吩噻嗪席夫碱荧光探针的合成及在ClO⁻生物成像中的应用

高超颖^*1，邵雨昕¹，包晓英¹，李鹏²，杨杨^*1

(1.内蒙古民族大学 化学与材料学院，内蒙古 通辽 028000；2. 北华大学 理学院，吉林 吉林  132013)

摘要：基于吩噻嗪和二氨基马来腈的缩合反应，合成了一种席夫碱类荧光探针分子PTZCN，用于高选择性检测次氯酸根（ClO^-）。该探针利用吩噻嗪作为电子供体，二氨基马来腈衍生的席夫碱基团作为电子受体，构建了典型的分子内电荷转移（ICT）体系。在40%乙醇-水溶液中，PTZCN与ClO⁻反应后，吸收峰从445 nm显著红移至627 nm，并伴随从黄色到紫色的可见颜色变化；此外，在365 nm紫外激发下，PTZCN在470 nm处发出强烈的蓝色荧光。该探针对ClO⁻表现出高度选择性，可有效区分其他常见干扰物，其检测限达到7.5 × 10⁻⁶ mol/L，且在pH 3~9的范围内保持稳定响应。高分辨质谱与密度泛函理论（DFT）计算的结果表明，ClO⁻选择性断裂探针分子中的C=N键，并发生水解反应，生成吩噻嗪-3-甲醛，进而抑制ICT过程并增强荧光强度。细胞实验表明，PTZCN具有低生物毒性，能够成功用于HeLa细胞中外源性ClO⁻的成像检测，并表现出特定的核区定位。在斑马鱼实验中，PTZCN显示出良好的组织穿透性，早期主要分布于卵黄囊，发育至72 h后，在幼鱼的头部和体部观察到特异性荧光。这些结果突出了PTZCN作为体内ClO⁻检测工具的潜力，并为开发ClO⁻特异性荧光探针提供了新思路。

关键词：吩噻嗪；席夫碱；次氯酸根；荧光探针；生物成像

中图分类号：O626；O641            文献标识码：A             文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0216

Phenothiazine Schiff-base Fluorescent Probes: Synthesis and Application in ClO⁻ Bioimaging GAO Chao-ying^*1, SHAO Yu-xin¹, BAO Xiao-ying¹, LI Peng², YANG Yang^*1(1. College of Chemistry and Materials Science, Inner Mongolia Minzu University, Tongliao 028000, China; 2. School of Sciences, Beihua University, Jilin 132013, China) 

Abstract：A novel Schiff-base fluorescent probe, PTZCN, was designed and synthesized via a condensation reaction between phenothiazine and diaminomaleonitrile for the highly selective detection of hypochlorite (ClO⁻). This molecular system features phenothiazine as the electron donor and a Schiff-base moiety derived from diaminomaleonitrile as the electron acceptor, forming a typical intramolecular charge transfer (ICT) architecture. Upon reaction with ClO⁻ in a 40% ethanol-water solution, the probe exhibited a distinct red shift in its UV-vis absorption spectrum, with the maximum absorption peak shifting from 445 to 627 nm, accompanied by a visible color change from yellow to purple. Additionally, under 365 nm excitation, a remarkable blue fluorescence emission was observed at 470 nm. PTZCN demonstrated high selectivity toward ClO⁻ over other common interfering species, with a detection limit as low as 7.5×10⁻⁶ mol/L and a stable response within the pH range of 3?9. High-resolution mass spectrometry and density functional theory (DFT) calculations indicated that ClO⁻ selectively cleaved and hydrolyzed the C=N bond, yielding highly fluorescent phenothiazine-3-aldehyde. This reaction suppressed the ICT process and restores localized excited-state emission. Cytotoxicity assays indicated low biological toxicity of PTZCN, and it was successfully applied for imaging exogenous ClO⁻ in HeLa cells with notable nuclear localization. In zebrafish models, the probe exhibited good tissue permeability, primarily localizing in the yolk sac of embryos. Specific fluorescence was observed in the head and body regions of larvae after 72 hours of development, demonstrating its potential for ClO⁻ detection in vivo. These findings highlighted PTZCN’s potential as a powerful tool for in vivo ClO⁻ detection and open new avenues for the development of ClO⁻-specific fluorescent probes.

Key words：phenothiazine; Schiff-base; hypochlorite; fluorescent probe; biological imaging

氢氧化钴在盐酸土霉素吸附中的研究

乔敏^a,b，闪冰冰^a，孙琪琪^a，孙漪轩^a，刘淼淼^a，高雅婷^a，赖新鑫^a,b 

(郑州工业应用技术学院 a. 药学与化学工程学院，b. 河南省水环境与健康工程技术研究中心，河南 郑州  451100) 

摘要：以氢氧化钴材料作为吸附剂，吸附水体中盐酸土霉素（OTC·HCl）。探讨该材料对盐酸土霉素的吸附性能，为水体中四环素类抗生素的去除提供数据支撑。采用水热法制备氢氧化钴材料，并采用FT-IR和SEM进行表征，考察不同吸附时间、材料投加量、盐酸土霉素的初始浓度、pH、温度等条件下，吸附剂对盐酸土霉素的吸附情况，设计模拟实际水样实验，考察氢氧化钴材料对盐酸土霉素的实际应用潜力。在吸附时间为60 min、氢氧化钴材料量为10 mg条件下，氢氧化钴材料对盐酸土霉素的最大吸附容量可达59.72 mg/g；吸附过程符合准二级动力学模型，热力学实验表明该吸附过程是一个自发的吸热过程，升温有利于材料对盐酸土霉素的吸附。材料对盐酸土霉素的吸附可在较宽pH范围（3.20 ~ 10.85）和共存离子存在条件下进行，在复杂水体中，材料仍对盐酸土霉素保持较好的吸附能力。氢氧化钴是一种去除盐酸土霉素的高效吸附材料，在抗生素类有机污染物治理领域具有广阔的应用前景。

关键词：氢氧化钴；盐酸土霉素；吸附；抗生素；废水处理

中图分类号：O63；X703         文献标识码：A             文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0156

Adsorption of Oxytetracycline Hydrochloride by Cobalt Hydroxide QIAO Min^{a, b}, SHAN Bing-bing^a, SUN Qi-qi^a, SUN Yi-xuan^a, LIU Miao-miao^a, GAO Ya-ting^a, LAI Xin-xin^{*a, b} (a.School of Pharmacy and Chemical Engineering, b. Henan Province Engineering Technology Research Center of Water Environment and Health, Zhengzhou University of Industrial Technology, Zhengzhou 451100, China) 

Abstract：Cobalt hydroxide was employed as an adsorbent to remove oxytetracycline hydrochloride (OTC·HCl) from aqueous solutions. The adsorption performance of cobalt hydroxide toward OTC·HCl was systematically investigated, providing data support for the removal of tetracycline antibiotics from water. Cobalt hydroxide was prepared by hydrothermal method and characterized by FT-IR and SEM. The adsorption behavior was examined under different conditions, including contact time, adsorbent dosage, initial OTC·HCl concentration, pH, and temperature. Simulated water samples were also carried out to investigate the practical application potential of cobalt hydroxide. The material demonstrated excellent adsorption performance, with a maximum adsorption capacity of 59.72 mg/g is achieved at an absorbent dosage of 10 mg of and a contact time of 60 min. The adsorption process was followed the pseudo-second-order model. Thermodynamic analysis showed that the process was endothermic and spontaneous, with higher temperature favoring adsorption. Effective adsorption occurred over a wide pH range (3.20~10.85) and in the presence of coexisting ions. Even in complex water matrices, cobalt hydroxide maintained excellent adsorption performance toward OTC·HCl. The results indicated that cobalt hydroxide is an efficient adsorption for the removal of oxytetracycline hydrochloride and it shows great application prospects in the field of antibiotic organic pollutant treatment.

Key words：cobalt hydroxide; oxytetracycline hydrochloride; adsorption; antibiotics; wastewater treatment

基于分子模拟筛选的手性药物氟比洛芬表面印迹膜制备研究

谢佳琦，易容^*，姜玉梅，王斌，赖申枝，李容

(湖南化工职业技术学院 制药与生物工程学院，湖南 株洲  412000)

摘要：分子印迹技术具有特异识别性强、稳定性好和实用性高的特点，在药物分离、环境污染与监测以及生物模拟抗体等领域广泛使用。以手性药物R-氟比洛芬(R-flurbiprofen，R-flu)为模板分子，运用分子印迹技术在聚偏氟乙烯（PVDF）中空纤维膜上制备了改性的分子印迹膜。采用Materials Studio分子模拟(Molecular simulation，MS)软件及紫外光谱法分析不同功能单体与模板分子间相互作用，并通过实验验证最优功能单体为4-乙烯基苯甲酸(4-Vinylbenzoic acid，4-VBA)。考察了不同条件下分子印迹膜的制备，运用扫描电子显微镜（Scanning electron microscopy，SEM）、傅里叶变换红外光谱 (Fourier transform infrared spectroscopy，FT-IR)、接触角测量仪等对其形貌及结构进行表征与验证，并对分子印迹膜性能进行分析评价，结果表明：制备的印迹膜(MIM)材料对R-氟比洛芬有高效的特异性识别能力，对R-flu的饱和吸附值为0.64 μmol /g，而非印迹膜（NIM）材料则为0.20 μmol /g。MIM对氟比洛芬外消旋体的结合容量QR/Qs值为1.60，且印迹膜材料稳定性好能重复使用。试验结果为分子模拟筛选用于手性拆分外消旋体药物提供了支持。为后续进一步实现规模化拆分提供了新思路。

关键词：氟比洛芬；分子印迹技术；表面印迹膜；分子模拟；手性药物

中图分类号：O643         文献标识码：A             文章编号：0258-3283（2025）--

DOI：10.13822/j.cnki.hxsj.2025.0245

Preparation of Surface-Imprinted Membranes for Chiral Drug Flurbiprofen Based on Molecular Simulation Screening XIE Jia-qi, YI Rong^*, JIANG Yu-mei, WANG Bin, LAI Shen-zhi, LI Rong (College of Pharmaceutical and bioengineering, Hunan Chemical Vocational Technology College, Zhuzhou 412000, China)

Abstract: Molecular imprinting technology (MIT) is characterized by strong specific recognition ability, good stability, and high practicability. It is widely applied in fields such as drug separation, environmental pollution monitoring and assessment, as well as biomimetic antibody development. Taking chiral drug R-flurbiprofen (R-flu) as the template molecule, a modified molecularly imprinted membrane was prepared on PVDF hollow fiber membranes by molecular imprinting technology. The interaction between different functional monomers and the template molecule was analyzed by Materials Studio molecular simulation (MS) software and ultraviolet spectroscopy, and the optimal functional monomer was verified experimentally to be 4-vinylbenzoic acid (4-VBA). The preparation of molecularly imprinted membranes (MIM) under different conditions was investigated. Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and the contact angle goniometer were employed to characterize and validate the morphology and structure of these membranes. Additionally, the performance of the molecularly imprinted membranes was analyzed and evaluated. The prepared imprinted membrane material has a highly efficient and specific recognition ability for R-flu, with a saturation adsorption capacity of 0.64 μmol/g for R-flu, whereas the non-imprinted membrane (NIM) material showed a value of only 0.20 μmol/g. The binding capacity ratio (Q_R/Qs) of MIM for flurbiprofen racemate was 1.60. Furthermore, the imprinted membrane material demonstrated good stability and could be reused. The experimental results provide support for the molecular simulation screening of functional monomers used in the chiral resolution of racemic drugs, and offer new ideas for the subsequent realization of modeling resolution.

Key words: flurbiprofen; molecular imprinting technology; surface imprinted membranes; molecular simulation; chiral drug

【电化学和新能源】

改性泡沫镍生长NiV-LDH纳米阵列电极材料的超级电容器性能研究

许雪棠^*，徐晴，何衍峰，覃志源，邓家华

（广西大学化学化工学院，广西南宁  530004）

摘要：创新性地采用泡沫镍基底改性（刻蚀）与二次水热法相结合的策略，成功制备了自支撑镍钒双金属层状氢氧化物（NiV-LDH）纳米阵列电极材料，显著提升了其电化学性能。通过系统对比无刻蚀生长（NiV-LDH）、同步刻蚀生长（S-NiV-LDH）及分步刻蚀生长（R-NiV-LDH）3种方式，发现分步刻蚀法（R-NiV-LDH）能有效诱导基底预先形成高度有序的“山脊状”纳米条纹。这一独特的微结构为后续垂直排列的次级纳米墙结构提供了理想的生长模板，不仅显著增加了电极的比表面积，还优化了活性位点的分布，并构建了高效的三维离子扩散通道。性能测试结果表明，R-NiV-LDH电极展现出卓越的综合性能。在2 A/g电流密度下，其质量比电容高达660.6 C/g。在50 mA/cm²的高电流密度下循环5600次后，容量保持率达91.67%，证明其优异的倍率性能和循环稳定性。以其为正极组装的全固态R-NiV-LDH//AC超级电容器，在1.8V宽电压窗口下，实现了0.4455 mWh/cm²的高能量密度和63 mW/cm²的功率密度，并成功驱动了多颗LED灯，验证了其实际应用潜力。此外，深入探讨了泡沫镍基底改性对调控材料微结构及电化学性能的作用机制，为开发高性能超级电容器电极材料提供了新的设计思路和实验依据。

关键词：改性泡沫镍；NiV-LDH；刻蚀；纳米阵列；超级电容器

中图分类号：O646            文献标识码：A        文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0174

Study on the Supercapacitor Performance of NiV-LDH Nanosheet Arrays Grown on Modified Nickel Foam Electrode Materials XU Xue-tang*, XU Qing, HE Yan-feng, QIN Zhi-yuan, DENG Jia-hua (School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China)

Abstract：This study employed an innovative strategy combining nickel foam (NF) substrate modification (etching) with a secondary hydrothermal method to successfully prepare self-supporting nickel-vanadium layered double hydroxide (NiV-LDH) nanoarray electrode materials with greatly enhanced electrochemical performance. By systematically comparing three approaches―direct growth without etching (NiV-LDH), simultaneous etching and growth (S-NiV-LDH), and stepwise etching and growth (R-NiV-LDH)―it was found that the stepwise etching method (R-NiV-LDH) effectively induced the pre-formation of highly ordered "ridge-like" nanostructures on the substrate. This unique microstructure served as an ideal template for the subsequent growth of vertically aligned secondary nanowall structures, significantly increasing the electrode's specific surface area, optimizing the distribution of active sites, and constructing efficient 3D ion diffusion pathways. Electrochemical testing revealed that the R-NiV-LDH electrode exhibited outstanding comprehensive performance, achieving a high specific capacitance of 660.6 C/g at 2 A/g and maintaining 91.67% capacity retention after 5600 cycles at a high current density of 50 mA/cm², demonstrating excellent rate capability and cycling stability. The assembled all-solid-state R-NiV-LDH//AC supercapacitor, using this material as the positive electrode, achieved an energy density of 0.4455 mWh/cm and a power density of 63 mW/cm at a wide voltage window of 1.8 V. It successfully powered multiple LED lights, demonstrating its practical applicability. Furthermore, this study provided an in-depth exploration of the mechanism by which NF substrate modification regulates the material's microstructure and electrochemical performance, offering valuable design concepts and experimental evidences for developing high-performance supercapacitor electrode materials.

Keywords：modified nickel foam; nickel-vanadium layered double hydroxide (NiV-LDH); etching; nanoarray; supercapacitor

【分析与测试】

高效液相色谱法测定运动营养食品中谷氨酰胺的含量

郑秋萍，蔡小明，何孟杭，吴少明，戴明，黄何何^*

（福建省产品质量检验研究院，福建福州  350002）

摘要：针对现行国家食品安全国家标准GB24154-2015《运动营养食品通则》中明确谷氨酰胺可作为运动营养食品添加剂，但必须严格控制每日摄入量问题，旨在优化仪器及前处理条件，建立一套运动营养食品中谷氨酰胺含量的分析方法，为运动营养食品中谷氨酰胺的监测及相关标准制定提供参考依据。采用50%乙腈溶液在超声条件下提取样品中的谷氨酰胺，再以Oasis PRiME HLB小柱通过式净化后，采用AQ-C₁₈色谱柱（4.6 mm×250 mm，5 μm）分离，5.0 mmol/L庚烷磺酸钠溶液（pH 2.5）为水相、V（水）：V（乙腈）=98:2为流动相，以紫外检测器在210 nm波长下进行测定，外标法定量，并在最优条件下进行方法验证。结果显示：谷氨酰胺在10.0～1000 μg/mL范围内呈良好的线性关系，R²=0.999，检出限为0.05~0.2 g/kg，定量限为0.15~0.6 g/kg；在蛋白粉、电解质饮料和能量胶条中进行低、中、高3个浓度水平的加标回收实验，平均回收率为91.1%～100.1%，平行实验（n=6）的相对标准偏差（RSD）为0.32%～2.87%。该方法简单易操作，专属性强、准确度高、重现性好，适用于运动营养食品中谷氨酰胺含量的分析。

关键词：高效液相色谱法；固相萃取；运动营养食品；谷氨酰胺；食品添加剂

中图分类号：O65         文献标识码：A             文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0202

Determination of Glutamine Content in Sports Nutrition Supplements by High Performance Liquid Chromatography ZHENG Qiu-ping, CAI Xiao-ming, HE Meng-hang, WU Shao-ming, DAI Ming, HUANG He-he*(Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China)

Abstract：According to the current national standard GB24154-2015 National Food Safety Standard for General Requirements for Sports Nutrition Foods, glutamine can be used as an additive in sports nutrition products, but its daily intake must be strictly controlled. This study aimed to optimize the instrument and pretreatment conditions and establish an analytical method for determining glutamine content in sports nutrition foods, providing a reference for monitoring and standard development. Glutamine was extracted from samples using 50% acetonitrile under ultrasonic conditions and purified with an Oasis PRiME HLB column. Separation was performed on an AQ-C₁₈ column (4.6 mm × 250 mm, 5 μm), with 5.0 mmol/L sodium heptane sulfonate solution (pH 2.5) and V (water) : V (acetonitrile) = 98:2 as the mobile phase. Detection was performed at 210 nm using a UV detector, and quantification was achieved by the external standard method. Under optimal conditions, glutamine exhibited good linearity in the range of 10.0～1000 μg/mL (R² = 0.999), with a detection limit of 0.05～0.2 g/kg and a quantification limit of 0.15～0.6 g/kg. Recovery experiments at low, medium, and high spiking levels in protein powder, electrolyte beverages, and energy gels gave average recoveries of 91.1% to 100.1%, with relative standard deviations (n = 6) of 0.32% ～ 2.87%. This method is simple, specific, accurate, and reproducible, and is suitable for the determination of glutamine in sports nutrition foods.

Key words: high performance liquid chromatography; solid-phase extraction; sports nutrition supplements; glutamine; food additives

涡旋浸提-电感耦合等离子体发射光谱法测定土壤中有效铁、锰、铜、锌含量

牛倩^*，张军伟

(洛阳生态环境监测中心，河南 洛阳  471000)

摘要：针对土壤有效态的DTPA振荡浸提法存在的浸提时间长、操作繁琐等效率瓶颈，创新性地将涡旋浸提（Vortex-Assisted Extraction, VAE）技术引入土壤有效态微量元素分析，建立了涡旋浸提结合电感耦合等离子体发射光谱法（ICP-OES）测定土壤有效态Fe、Mn、Cu、Zn的新方法。系统优化了涡旋浸提条件和参数，确定最佳参数为：料液比1:4（g/mL）、涡旋速度2000 r/min、浸提时间40 min、温度（25±2）℃。在优化条件下，Fe、Mn、Cu、Zn的方法检出限分别为0.06、0.02、0.012和0.024 mg/kg，标准曲线相关系数均大于0.9996。采用土壤有效态成分分析标准物质验证，方法精密度RSD<6%，准确度RE为95.7%~106.8%，加标回收率在94.8%~103.0%之间。与国家标准HJ 804-2016规定的振荡浸提法对比，两种方法测定结果无显著差异，但涡旋浸提将前处理时间从120 min大幅缩短至40 min，提取效率提高67%。该方法操作简便、分析速度快、结果准确可靠，显著提升了分析效率，为土壤肥力评价和环境监测中大批量样品的快速检测提供了新的技术手段。

关键词：涡旋浸提；电感耦合等离子体发射光谱法；土壤有效态元素；DTPA浸提；快速测定

中图分类号: O657.31                  文献标识码: A                  文章编号：0258-3283（2025）

DOI：10.13822/j.cnki.hxsj.2025.0164

Determination of Available Iron, Manganese, Copper, and Zinc in Soil by Vortex Extraction-Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) Niu Qian^*, Zhang Jun-wei (Luoyang Ecological & Environmental Monitoring Center, Luoyang 471000, China)

Abstract: To address the efficiency bottlenecks of the DTPA oscillating extraction method for soil available nutrients, such as prelonged extraction time and cumbersome operation, this study introduced Vortex-Assisted Extraction (VAE) technology into soil available trace element analysis. A novel method combining vortex extraction and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) was established for the determination of available Fe, Mn, Cu, and Zn in soil. The vortex extraction conditions and parameters were systematically optimized, with optimal parameters determined as follows: soil-to-solution ratio of 1:4 (g/mL), vortex speed of 2000 r/min, extraction time of 40 min, and temperature of (25±2)°C. Under optimized conditions, the method detection limits for Fe, Mn, Cu, and Zn were 0.06, 0.02, 0.012, and 0.024 mg/kg, respectively, with correlation coefficients for standard curves all exceeding 0.9996. Validation using certified reference materials for soil available components showed that the method precision (RSD) was less than 6%, with relative errors (RE) ranging from 95.7% to 106.8%, and spike recovery rates ranging between 94.8% and 103.0%. Compared with the oscillating extraction method specified in national standard HJ 804-2016, no significant differences were observed in the results between the two methods. However, vortex extraction dramatically reduced the pretreatment time from 120 to 40 min, improving extraction efficiency by 67%. This method features simple operation, rapid analysis, and reliable results, significantly enhancing analytical efficiency and providing a new technical approach for the rapid detection of large-batch samples in soil fertility evaluation and environmental monitoring.

Keywords: vortex-assisted extraction; inductively coupled plasma optical emission spectrometry; available soil elements; DTPA extraction; rapid determination