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2025年47(12)中英文摘要
時間:2025-12-17      來源:

【特約專題】

磷手性二氫苯并氧雜膦烷配體在催化與合成中的應用

 

曹振1,徐廣慶1,羅林1,湯文軍*1,2,3

(1. 紹興賾軍生物醫藥科技有限公司 研發部,浙江紹興  3123692. 中科院上海有機化學研究所 生命過程小分子調控國家重點實驗室,上海  2000323. 國科大杭州高等研究院 化學和材料科學學院,浙江杭州  310024)

 

摘要:直到Knowles開發的磷手性配體CAMPDIPAMP在不對稱氫化反應中的成功應用,磷手性配體才受到廣泛關注。盡管后來開發出了眾多活性優異的磷手性配體,但大多都對空氣敏感且結構難以修飾,阻礙了其在學術研究和工業中的應用。磷手性二氫苯并氧雜膦烷配體是一類大位阻、富電子、結構可調且性質穩定的膦配體,在過去的10年中,百余個基于該骨架的膦配體已被開發報道并成功應用多種有機化學轉化。總結了該類配體在催化和合成中的應用,主要包括大位阻偶聯反應、加成反應、環化反應及氫化反應,并著重強調其在不對稱催化和合成包括不對稱偶聯、不對稱碳氫鍵活化及不對稱去芳構環化反應中的諸多獨特催化特性。磷手性二氫苯并氧雜膦烷配體有望在不對稱催化、藥物綠色工藝開發及工業化生產中發揮著更加突出的作用。

關鍵詞:磷手性;二氫苯并氧雜膦烷;結構可調;不對稱;催化與合成

中圖分類號O62                   文獻標識碼A               文章編號:0258-32832025--

DOI10.13822/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 )

AbstractP-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 wordsP-chiral; dihydrobenzooxaphosphole; structurally tunable; asymmetric; catalysis and synthesis

 

陰離子交換膜用于電催化CO2還原的研究進展

 

王佑庭1,曹媛媛*2,魏榮耀1,范茹1,呂晶晶1,吳芬*1,王正軍1,3

(1. 溫州大學化學與材料工程學院新材料與產業技術研究院,浙江溫州  325035

2. 杭州中一檢測研究院有限公司,浙江杭州  311258

3. 溫州市生物功能材料與化學重點實驗室,浙江溫州  325035)

 

摘要:隨著化石燃料的大量使用,溫室氣體的排放,尤其是二氧化碳等溫室氣體的大量排放,引起了一系列的環境問題,通過電催化二氧化碳還原(eCO2RR)可以將其轉化為高價值的燃料/商品化學品,為上述問題提供了技術支撐,而近年來隨著反應器的設計改進進一步提高了該技術的經濟可行性。在CO2RR反應器中離子交換膜(IEM)對于二氧化碳轉化為有用產品的能量效率方面起著關鍵作用,每種離子交換膜都有著不同的優缺點,而其中陰離子交換膜(AEM)往往表現出更高的效率和產物選擇性等優點,在CO2RR中具備巨大的應用潛力。綜述了近年來國內外研究者對于AEMeCO2RR中的研究進展,介紹了AEM的作用機制、合成方法、性能評價標準以及近期報道的新型AEM,隨后重點關注了這些AEM的設計思路、優化策略,特別是對于其化學穩定性、轉化效率、機械強度等方面,最后對于未來AEM設計的挑戰和機遇進行了展望。

關鍵詞:溫室氣體電催化二氧化碳還原陰離子交換膜制備方法應用

中圖分類號O64    文獻標識碼A            文章編號0258-32832025

DOI10.13822/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-jun1,3 (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

 

綜述與專論

肉桂精油研究與應用進展

 

朱紫琪,何靜金,余昆瑩,鐘海藝*

(廣西中醫藥大學藥學院,廣西南寧  530000

 

摘要:肉桂精油作為一種天然活性物質,其化學組成復雜,包含肉桂醛、δ-杜松烯、苯甲醇等化合物;這些成分相互協同,賦予了肉桂精油廣泛的藥理作用,包括抗菌、抗氧化、驅蟲、抗真菌和抗腫瘤等多種活性功效,被廣泛應用于食品保鮮防腐、醫藥等領域。歸納總結了肉桂精油的常用的提取方法,包括水蒸氣蒸餾、超臨界二氧化碳萃取法和低共熔溶劑提取法,并概述了各法的萃取原理及其優缺點,為肉桂精油的提取提供參考。同時總結歸納了不同品種、部位所提取的肉桂精油的活性成分和含量,可以得知肉桂的產地和品種也是造成肉桂精油成分和含量差異的重要因素。除此之外,還分別闡述了抗菌、抗氧化、驅蟲、抗真菌和抗腫瘤5種生物活性的作用機制和特點。最后通過對國內外研究進行展望,系統簡述了肉桂精油在食品保鮮和醫療衛生事業的應用和作用機制,肉桂精油通過抗氧化、抑菌等特性在延長食品保質期方面展現出顯著潛力;在醫療衛生領域,其抗炎、抗腫瘤及調節血糖等作用機制為治療炎癥性疾病、癌癥及糖尿病提供了新思路。以期為肉桂精油的開發和應用提供理論參考,推動其在更多領域發揮更大的作用。

關鍵詞:肉桂;精油;提取方法;活性成分;實際應用

中圖分類號:O631.1         文獻識別碼:A         文章編號:0258-32832025--

DOI10.13822/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

AbstractCinnamon 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 wordscinnamon; essential oils; extraction method; active ingredients; practical application

 

光催化和電化學在連續流合成中的研究進展

 

楊宏勛1,凌芳*2,智俊峰3,查曉明3

國藥集團化學試劑有限公司上海  2000022. 上海沃凱生物技術有限公司上海  2015073. 中國藥科大學 工學院江蘇南京  211198

 

摘要:近年來,連續流合成技術取得了重要進展,基于微觀尺度與連續流動過程的協同作用,能夠實現反應過程的精準控制,解決了傳統釜式反應的諸多不足,已廣泛應用于醫藥化工行業的生產。光催化和電化學反應作為過程強化的手段,應用于連續流合成中,增強反應過程的同時還可以減少污染。連續流技術與光電催化的融合代表了綠色化學的發展方向,這一創新體系通過將能量耦合,催化協同及反應路徑優化,實現了高效、精準、可持續的化學轉化。連續流反應器的微通道設計強化了傳質與傳熱效率,使反應時間從數小時縮短至分鐘級甚至秒級;光電催化過程無需添加有害催化劑,減少了廢棄物的排放,原子經濟性高,符合綠色化學理念。連續流技術在原料藥、醫藥中間體等的合成中展現出獨特的優勢。對近年來光電催化技術應用于連續流合成中的研究進展進行了總結和展望。

關鍵詞:連續流合成;光催化;電化學;過程強化;研究進展

中圖分類號:O69           文獻標識碼:A          文章編號:0258-32832025

DOI10.13822/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

 

 

 

 

【生化與藥用試劑】

 

藥物共晶緩釋制劑研究進展

張順,吳海麗,陳玲,林寧,陳清*

(廣西中醫藥大學中醫藥壯瑤醫藥研究院廣西壯瑤藥技術創新中心,廣西南寧  530200

 

摘要:緩釋制劑通過理性設計實現藥物的緩慢釋放,維持平穩的血藥濃度、避免峰谷現象,有利于降低藥物的毒副作用。對于半衰期短的藥物,緩釋技術可降低給藥頻率,提高患者依從性和治療效果。藥物的溶解度及溶出行為與其晶格穩定性及分子間相互作用等固體性質密切相關。研究表明,對于治療窗窄、半衰期短或局部刺激性大的藥物,可通過固體性質的調控實現緩釋制劑的優化設計。近年來,引入共形成物制備成為藥物共晶,已成為改善藥物性能的創新策略。該技術通過分子間超分子作用顯著提升藥物的晶格穩定性,進而調控其溶出動力學。對近年來具有緩釋潛力的藥物共晶研究進展進行綜述,探討了共晶技術通過分子間相互作用調控藥物理化性質和釋放行為的機制原理,基于不同種類藥物的臨床治療需求系統分析了現有藥物在溶解度、釋放特性和生物利用度等方面面臨的問題,總結了藥物共晶技術在改善這些藥物性能方面的獨特優勢。為基于共晶技術的新型緩釋制劑的研發和臨床應用提供了重要的理論依據和實踐指導。

關鍵詞:藥物共晶;緩釋制劑;晶格穩定性;溶出度;生物利用度;治療效果

中圖分類號O64R943      文獻標識碼A       文章編號:0258-32832025

DOI10.13822/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) 

AbstractSustained 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 wordspharmaceutical cocrystal; sustained-release formulation;lattice stability; dissolution; biovailability; therapeutic effect

功能材料

鎘配合物熒光傳感檢測抗生素的研究進展

 

朱浩如1馬新晶1,白成潔1,孫贊*1,2

1.青海民族大學 化學與材料科學學院,青海 西寧  8100072.青藏高原資源化學與生態環境保護國家民委重點實驗室,青海 西寧  810007

 

摘要:近年來,抗生素(包括青霉素類、四環素類、頭孢菌類、喹諾酮類、大環內酯類等)的濫用導致其成為水環境中的首要有機污染物,其引發的后果是一個貫穿生態環境、公眾健康與醫療體系的連鎖反應,且危害程度隨時間推移不斷加劇。在生態方面,抗生素的殘留會破壞水體菌群平衡,催生耐藥菌,污染水產品。在健康方面,抗生素的殘留會擾亂腸道菌群、削弱免疫力,耐藥菌感染還使常規治療失效,延長病程且增加費用。在醫療方面,耐藥性會導致抗生素的保護作用減弱,甚至可能面臨無藥可用風險。傳統的抗生素檢測方法包括酶免疫分析法、色譜-串聯質譜法、離子遷移譜法和表面增強拉曼光譜法等,具有諸多缺點,例如需要復雜的樣品預處理過程、較高的時間成本和昂貴的檢測設備等,而基于鎘配合物的熒光傳感器由于具有良好的配位多樣性、結構可調性、優異的光物理和光化學性質,因而具有低成本、實時觀測、高靈敏度和操作簡單等優勢,已成為檢測抗生素的首選技術之一。總結了鎘配合物檢測抗生素的最新進展、探討了配合物的結構設計策略以及作用機理,此外還總結了鎘配合物檢測抗生素的不足之處、展望了未來的發展趨勢。

關鍵詞:鎘配合物;抗生素;熒光檢測;機理;結構設計

中圖分類號O641.4                文獻標識碼A             文章編號:0258-32832025

DOI10.13822/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)  

AbstractIn 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 wordscadmium coordination polymers; antibiotics; fluorescence detection; mechanism; structure design

 

Zn/U異核鈾酰MOF的構筑及其熒光傳感性能研究

呂艷羽1,許瑩瑩1,司貞秀*1,戴曉俠1,姜凌云1,許偉2

1. 山東藥品食品職業學院 制藥工程系,山東 威海  2642002. 寧波大學 材料科學與化學工程學院,浙江 寧波  315211)  

摘要:谷氨酸(Glu)在生物代謝、食品風味及疾病診斷中具有關鍵作用,建立快速、靈敏的Glu檢測方法對神經科學研究、食品安全監控及臨床診斷具有重要意義。基于異核構筑策略開發一種高性能熒光傳感材料,以實現對Glu的高選擇性識別。通過溶劑熱法成功合成了一例新型異核鈾酰有機骨架材料[Zn(UO2)(ntp)2(5,5'-dm-2,2'-bpy)2(H2O)](H2ntp = 2-硝基對苯二甲酸,5,5'-dm-2,2'-bpy = 5,5'-二甲基-2,2'-聯吡啶),并通過單晶X-射線衍射、熒光光譜和紫外-可見吸收光譜等手段對其結構和光學性能進行了系統表征。熒光傳感研究表明,該材料對Glu表現出優異的選擇性與靈敏性,呈現顯著熒光猝滅效應,檢出限(LOD)為0.953 μmol/L此外,該傳感器具備良好的抗干擾能力和循環穩定性。機理研究證實,熒光猝滅源于光誘導電子轉移(PET)過程。為錒系異金屬MOFs在氨基酸熒光傳感領域的應用提供了新思路,展現出潛在的實際應用價值。

關鍵詞異核;鈾酰金屬有機骨架;晶體結構;熒光傳感;谷氨酸

中圖分類號:O65                 文獻標識碼:A            文章編號:0258-32832025

DOI10.13822/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 21. 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

一種苯并吡喃酮熒光探針對Zn2+的檢測研究

 

覃姣蘭,梁武華,袁濤*,范歆晨,黃如川,何厚賢

(百色學院廣西城市水環境重點實驗室,廣西百色 533000

 

摘要:為設計合成香豆素衍生物熒光探針以實現對金屬離子的高選擇性、高靈敏識別,并為實際水樣中Zn2+檢測提供理論與應用參考,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)為熒光探針,在乙醇-水混合體系(V(乙醇):V(水)=1:1)中,通過熒光光譜法研究其對多種金屬離子的識別性能,同時采用Job's Plot實驗與X-單晶衍射實驗解析探針與目標離子的合機制,并考察探針的線性響應范圍、檢出限、響應時間及實際水樣適用性。研究結果表明,BDC探針對Zn2+表現出特異性識別能力,與Zn2+作用后熒光顯著增強,且不受其他共存金屬離子干擾;探針熒光強度與Zn2+濃度在特定范圍內呈良好線性關系(R2=0.9921),檢出限低至0.117 μmol/L,響應時間短(≤0.5 min)。Job's Plot 實驗與X-單晶衍射實驗進一步證實BDC可與Zn2+形成穩定合物,其熒光增強效應源于合作用引發的螯合熒光增強(CHEF)效應。綜上,BDC 熒光探針具備對Zn2+的高選擇性、高靈敏性及快速響應特性,可成功應用于實際水樣中Zn2+的檢測,為香豆素類金屬離子識別探針的設計與應用提供了有效借鑒。

關鍵詞:香豆素;熒光探針;鋅離子檢測;光譜研究;熒光增強

中圖分類號O657.3          文獻標識碼:A         文章編號: 0258-32832025

DOI10.13822/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-xianGuangxi 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 Vethanol:Vwater=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: coumarinfluorescent probeZn2+ detectionspectroscopic study; fluorescence enhancement

 

 

 

吩噻嗪席夫堿熒光探針的合成及在ClO?生物成像中的應用

 

高超穎*1邵雨昕1,包曉英1,李鵬2,楊楊*1

(1.內蒙古民族大學 化學與材料學院,內蒙古 通遼 0280002. 北華大學 理學院,吉林 吉林  132013)

 

摘要:基于吩噻嗪和二氨基馬來腈的縮合反應,合成了一種席夫堿類熒光探針分子PTZCN,用于高選擇性檢測次氯酸根(ClO-)。該探針利用吩噻嗪作為電子供體,二氨基馬來腈衍生的席夫堿基團作為電子受體,構建了典型的分子內電荷轉移(ICT)體系。在40%乙醇-水溶液中,PTZCNClO?反應后,吸收峰從445 nm顯著紅移至627 nm,并伴隨從黃色到紫色的可見顏色變化;此外,在365 nm紫外激發下,PTZCN470 nm處發出強烈的藍色熒光。該探針對ClO?表現出高度選擇性,可有效區分其他常見干擾物,其檢測限達到7.5 × 10?6 mol/L,且在pH 3~9的范圍內保持穩定響應。高分辨質譜與密度泛函理論(DFT)計算的結果表明,ClO?選擇性斷裂探針分子中的C=N鍵,并發生水解反應,生成吩噻嗪-3-甲醛,進而抑制ICT過程并增強熒光強度。細胞實驗表明,PTZCN具有低生物毒性,能夠成功用于HeLa細胞中外源性ClO?的成像檢測,并表現出特定的核區定位。在斑馬魚實驗中,PTZCN顯示出良好的組織穿透性,早期主要分布于卵黃囊,發育至72 h后,在幼魚的頭部和體部觀察到特異性熒光。這些結果突出了PTZCN作為體內ClO?檢測工具的潛力,并為開發ClO?特異性熒光探針提供了新思路。

關鍵詞:吩噻嗪;席夫堿;次氯酸根;熒光探針;生物成像

中圖分類號O626O641            文獻標識碼A             文章編號:0258-32832025

DOI10.13822/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) 

AbstractA 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 wordsphenothiazine; Schiff-base; hypochlorite; fluorescent probe; biological imaging

氫氧化鈷在鹽酸土霉素吸附中的研究

 

喬敏a,b,閃冰冰a,孫琪琪a,孫漪軒a,劉淼淼a,高雅婷a,賴新鑫a,b 

(鄭州工業應用技術學院 a. 藥學與化學工程學院b. 河南省水環境與健康工程技術研究中心,河南 鄭州  451100) 

 

摘要:以氫氧化鈷材料作為吸附劑,吸附水體中鹽酸土霉素(OTC·HCl)。探討該材料對鹽酸土霉素的吸附性能,為水體中四環素類抗生素的去除提供數據支撐。采用水熱法制備氫氧化鈷材料,并采用FT-IRSEM進行表征,考察不同吸附時間、材料投加量、鹽酸土霉素的初始濃度、pH、溫度等條件下,吸附劑對鹽酸土霉素的吸附情況,設計模擬實際水樣實驗,考察氫氧化鈷材料對鹽酸土霉素的實際應用潛力。在吸附時間為60 min、氫氧化鈷材料量為10 mg條件下,氫氧化鈷材料對鹽酸土霉素的最大吸附容量可達59.72 mg/g;吸附過程符合準二級動力學模型,熱力學實驗表明該吸附過程是一個自發的吸熱過程,升溫有利于材料對鹽酸土霉素的吸附。材料對鹽酸土霉素的吸附可在較寬pH范圍(3.20 ~ 10.85)和共存離子存在條件下進行,在復雜水體中,材料仍對鹽酸土霉素保持較好的吸附能力。氫氧化鈷是一種去除鹽酸土霉素的高效吸附材料,在抗生素類有機污染物治理領域具有廣闊的應用前景。

關鍵詞:氫氧化鈷;鹽酸土霉素;吸附;抗生素;廢水處理

中圖分類號O63X703         文獻標識碼A             文章編號:0258-32832025

DOI10.13822/j.cnki.hxsj.2025.0156

 

Adsorption of Oxytetracycline Hydrochloride by Cobalt Hydroxide QIAO Mina, b, SHAN Bing-binga, SUN Qi-qia, SUN Yi-xuana, LIU Miao-miaoa, GAO Ya-tinga, 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) 

AbstractCobalt 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 wordscobalt hydroxide; oxytetracycline hydrochloride; adsorption; antibiotics; wastewater treatment

 

 

 

 

基于分子模擬篩選的手性藥物氟比洛芬表面印跡膜制備研究

 

謝佳琦,易容*,姜玉梅,王斌,賴申枝,李容

(湖南化工職業技術學院 制藥與生物工程學院,湖南 株洲  412000)

 

摘要:分子印跡技術具有特異識別性強、穩定性好和實用性高的特點,在藥物分離、環境污染與監測以及生物模擬抗體等領域廣泛使用。以手性藥物R-氟比洛芬(R-flurbiprofenR-flu)為模板分子,運用分子印跡技術在聚偏氟乙烯(PVDF)中空纖維膜上制備了改性的分子印跡膜。采用Materials Studio分子模擬(Molecular simulationMS)軟件及紫外光譜法分析不同功能單體與模板分子間相互作用,并通過實驗驗證最優功能單體為4-乙烯基苯甲酸(4-Vinylbenzoic acid4-VBA)。考察了不同條件下分子印跡膜的制備,運用掃描電子顯微鏡(Scanning electron microscopySEM)、傅里葉變換紅外光譜 (Fourier transform infrared spectroscopyFT-IR)、接觸角測量儀等對其形貌及結構進行表征與驗證,并對分子印跡膜性能進行分析評價,結果表明:制備的印跡膜(MIM)材料對R-氟比洛芬有高效的特異性識別能力,對R-flu的飽和吸附值為0.64 μmol /g,而非印跡膜(NIM)材料則為0.20 μmol /gMIM對氟比洛芬外消旋體的結合容量QR/Qs值為1.60,且印跡膜材料穩定性好能重復使用。試驗結果為分子模擬篩選用于手性拆分外消旋體藥物提供了支持。為后續進一步實現模化拆分提供了新思路。

關鍵詞:氟比洛芬分子印跡技術表面印跡膜分子模擬手性藥物

中圖分類號O643         文獻標識碼A             文章編號:0258-32832025--

DOI10.13822/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 (QR/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

 

【電化學和新能源】

改性泡沫鎳生長NiV-LDH納米陣列電極材料超級電容器性能研究

許雪棠*,徐晴,何衍峰,覃志源,鄧家華

(廣西大學化學化工學院,廣西南寧  530004

 

摘要創新性地采用泡沫鎳基底改性(刻蝕)與二次水熱法相結合的策略,成功制備了自支撐鎳釩雙金屬層狀氫氧化物(NiV-LDH)納米陣列電極材料,顯著提升了其電化學性能。通過系統對比無刻蝕生長(NiV-LDH)、同步刻蝕生長(S-NiV-LDH)及分步刻蝕生長(R-NiV-LDH3種方式,發現分步刻蝕法(R-NiV-LDH)能有效誘導基底預先形成高度有序的山脊狀納米條紋。這一獨特的微結構為后續垂直排列的次級納米墻結構提供了理想的生長模板,不僅顯著增加了電極的比表面積,還優化了活性位點的分布,并構建了高效的三維離子擴散通道。性能測試結果表明,R-NiV-LDH電極展現出卓越的綜合性能。在2 A/g電流密度下,其質量比電容高達660.6 C/g。在50 mA/cm2的高電流密度下循環5600次后,容量保持率達91.67%,證明其優異的倍率性能和循環穩定性。以其為正極組裝的全固態R-NiV-LDH//AC超級電容器,在1.8V寬電壓窗口下,實現了0.4455 mWh/cm2的高能量密度和63 mW/cm2的功率密度,并成功驅動了多顆LED燈,驗證了其實際應用潛力。此外,深入探討了泡沫鎳基底改性對調控材料微結構及電化學性能的作用機制,為開發高性能超級電容器電極材料提供了新的設計思路和實驗依據。

關鍵詞:改性泡沫鎳;NiV-LDH;刻蝕;納米陣列;超級電容器

中圖分類號:O646            文獻標識碼:A        文章編號:0258-32832025

DOI10.13822/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)

AbstractThis 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.

Keywordsmodified nickel foam; nickel-vanadium layered double hydroxide (NiV-LDH); etching; nanoarray; supercapacitor

 

分析與測試

 

高效液相色譜法測定運動營養食品中谷氨酰胺的含量

 

鄭秋萍,蔡小明,何孟杭,吳少明,戴明,黃何何*

(福建省產品質量檢驗研究院,福建福州  350002

摘要:針對現行國家食品安全國家標準GB24154-2015《運動營養食品通則》中明確谷氨酰胺可作為運動營養食品添加劑,但必須嚴格控制每日攝入量問題,旨在優化儀器及前處理條件,建立一套運動營養食品中谷氨酰胺含量的分析方法,為運動營養食品中谷氨酰胺的監測及相關標準制定提供參考依據。采用50%乙腈溶液在超聲條件下提取樣品中的谷氨酰胺,再以Oasis PRiME HLB小柱通過式凈化后,采用AQ-C18色譜柱(4.6 mm×250 mm5 μm)分離,5.0 mmol/L庚烷磺酸鈉溶液(pH 2.5)為水相、V(水):V(乙腈)=98:2為流動相,以紫外檢測器在210 nm波長下進行測定,外標法定量,并在最優條件下進行方法驗證。結果顯示:谷氨酰胺在10.01000 μg/mL范圍內呈良好的線性關系,R2=0.999,檢出限為0.05~0.2 g/kg,定量限為0.15~0.6 g/kg;在蛋白粉、電解質飲料和能量膠條中進行低、中、高3個濃度水平的加標回收實驗,平均回收率為91.1%100.1%,平行實驗(n=6)的相對標準偏差(RSD)為0.32%2.87%。該方法簡單易操作,專屬性強、準確度高、重現性好,適用于運動營養食品中谷氨酰胺含量的分析。

關鍵詞:高效液相色譜法;固相萃取;運動營養食品;谷氨酰胺;食品添加劑

中圖分類號O65         文獻標識碼A             文章編號:0258-32832025

DOI10.13822/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)

AbstractAccording 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 10.01000 μg/mL (R2 = 0.999), with a detection limit of 0.050.2 g/kg and a quantification limit of 0.150.6 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

 

渦旋浸提-電感耦合等離子體發射光譜法測定土壤中有效鐵、錳、銅、鋅含量

牛倩*,張軍偉

(洛陽生態環境監測中心,河南 洛陽  471000)

摘要:針對土壤有效態的DTPA振蕩浸提法存在的浸提時間長、操作繁瑣等效率瓶頸,創新性地將渦旋浸提(Vortex-Assisted Extraction, VAE)技術引入土壤有效態微量元素分析,建立了渦旋浸提結合電感耦合等離子體發射光譜法(ICP-OES)測定土壤有效態FeMnCuZn的新方法。系統優化了渦旋浸提條件和參數,確定最佳參數為:料液比1:4g/mL、渦旋速度2000 r/min、浸提時間40 min、溫度(25±2。在優化條件下,FeMnCuZn的方法檢出限分別為0.060.020.0120.024 mg/kg,標準曲線相關系數均大于0.9996。采用土壤有效態成分分析標準物質驗證,方法精密度RSD<6%,準確度RE95.7%~106.8%,加標回收率在94.8%~103.0%之間。與國家標準HJ 804-2016規定的振蕩浸提法對比,兩種方法測定結果無顯著差異,但渦旋浸提將前處理時間從120 min大幅縮短至40 min,提取效率提高67%。該方法操作簡便、分析速度快、結果準確可靠,顯著提升了分析效率,為土壤肥力評價和環境監測中大批量樣品的快速檢測提供了新的技術手段。

關鍵詞:渦旋浸提;電感耦合等離子體發射光譜法;土壤有效態元素;DTPA浸提;快速測定

中圖分類號: O657.31                  文獻標識碼: A                  文章編號0258-32832025

DOI10.13822/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

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