【特约专稿】

改性生物炭吸附水体中微塑料的研究：改性方法和去除机理

罗堂，李锦雅，纪鹏宇，范世锁^*

（安徽农业大学 资源与环境学院，安徽 合肥  230036）

摘要: 微塑料作为一种新兴的全球性环境污染物，在水体中广泛分布，对生态系统和人类健康构成严重威胁。生物炭因其独特的孔隙结构和表面性质，在环境污染治理中展现出广阔前景。然而，原状生物炭对微塑料的吸附存在效率低、容量有限等问题，而功能化改性可显著提升其吸附性能。系统综述了改性生物炭去除水体中微塑料的研究进展。重点阐述了化学改性（如金属负载、酸碱处理）与物理改性（如蒸气活化）等方法，通过调控生物炭的孔隙结构、表面电荷和官能团，增强其与微塑料的作用。同时，深入剖析了物理截留、静电吸引、氢键及表面络合等多种吸附机制。进一步探讨了生物炭自身特性、微塑料性质（如类型、粒径）以及环境因素（如pH值、溶解性有机质）对吸附过程的综合影响。此外，简要评述了改性生物炭的再生技术与实际应用所面临的挑战，包括制备成本、长期生态安全性及在复杂水体环境中的稳定性问题。旨在为改性生物炭材料的优化设计及其在微塑料污染治理中的工程应用提供理论参考。

关键词: 生物炭；微塑料；改性方法；吸附机制；影响因素；实际挑战

中图分类号：O647      文献标识码：A      文章编号：0258-3283（2026）--

DOI：10.13822/j.cnki.hxsj.2025.0298

Engineered Biochar for Microplastic Removal from Water: Modification Strategies and Mechanisms LUO Tang, LI Jin-ya, JI Peng-yu, FAN Shi-suo^* (School of Resources and Environment, Anhui Agricultural University, Hefei 230036, China)

Abstract: Microplastics are an emerging global environmental pollutant that are widely distributed in aquatic environments and have attracted increasing attention due to their potential ecological and health impacts.. Biochar shows great promise in environmental pollution remediation due to its unique pore structure and surface properties. However, the adsorption of microplastics by raw biochar was often limited by low efficiency and low capacity, and various modification strategies have been developed to improve its effectiveness. This review systematically summarized recent advances in the removal of microplastics from aqueous environments using modified biochar. Chemical modification methods, including metal impregnation and acid or alkali treatment, as well as physical modification approaches such as steam activation, were discussed with respect to their effects on the pore structure, surface charge, and functional groups of biochar. The main adsorption mechanisms, such as physical interception, electrostatic attraction, hydrogen bonding, and surface complexation, are also discussed in detail. Furthermore, the influences of biochar properties, microplastic characteristics (e.g., type, size), and environmental factors (e.g., pH, dissolved organic matter) on the adsorption process are examined. Additionally, this review briefly addressed regeneration techniques for modified biochar and the challenges of practical application, including preparation cost, long-term environmental safety, and stability in complex aqueous environments. This review provided a reference for the design and application of modified biochar material for microplastic removal in aquatic environments.

Key words：biochar; microplastics; modification methods; adsorption mechanisms; influencing factors; practical challenges

碱促进下2,3-二取代苯并呋喃的高效合成

张金坤^,2，李芷乐³，邱小权³，黄年玉^*3，王能中^*3

(1. 三峡大学 第一临床医学院，湖北宜昌  443002；2. 宜昌市中心人民医院，湖北 宜昌  443003；3. 三峡大学 生物与制药学院 天然产物研究与利用湖北省重点实验室，湖北宜昌  443002)

摘要：苯并呋喃作为一种重要的杂环结构单元，广泛存在于天然产物、药物分子、农药以及功能材料中。同时，其本身作为一种潜力的合成子，用于制备多种多样的生物活性分子。迄今为止，尽管苯并呋喃母核的合成方法已较为成熟，但针对2,3-二取代苯并呋喃的高效、通用的合成方法仍相对有限。现有的一些方法往往面临反应条件苛刻、步骤繁琐或底物普适性不佳等挑战。因此，开发一种条件温和、高效、操作简便的合成方法是非常有必要的。基于此，设计以易于制备的邻羟基查尔酮与商业可得的γ-溴代巴豆酸酯为原料，在温和的碱性条件下，经过一锅多步串联反应生成一系列2,3-二取代苯并呋喃类化合物。该策略避免了使用昂贵金属催化剂或苛刻反应条件，展现出良好的官能团兼容性与操作简便性。该合成策略不仅为2,3-二取代苯并呋喃类化合物的高效合成提供了一条新颖途径，也为后续深入研究这类化合物的生物活性及材料性能奠定了坚实的物质基础，在药物化学和有机合成领域具有潜在的应用价值。

关键词：苯并呋喃；合成；碱促进；邻羟基查尔酮；γ-溴代巴豆酸酯

中图分类号：O62           文献标识码：A         文章编号：

DOI：10.13822/j.cnki.hxsj.2025.0318

Base-Promoted Efficient Synthesis of 2,3-Disubstituted Benzofurans  ZHANG Jin-kun^1,2, LI Zhi-yue³, QIU Xiao-quan³, HUANG Nian-yu^*3, WANG Neng-zhong^*3（1. The First College of Clinical Medical Science, China Three Gorges University, Yichang 443002, China; 2. Yichang Central People's Hospital, Yichang 443003, China; 3. Hubei Key Laboratory of Natural Products Research and Development, College of Biological and Pharmaceutical Sciences, China Three Gorges University, Yichang 443002, China）

Abstract: Benzofuran is a heterocyclic structural unit that occurs widely in natural products, drugs, pesticides, and functional materials, and it is used as a potential synthetic building block in preparing various biologically active molecules. The synthesis of benzofuran cores is well-established, but efficient general methods of synthesizing 2,3-disubstituted benzofurans remain relatively limited. Several reported methods often suffer from challenges, such as harsh reaction conditions, cumbersome steps, and poor substrate generalities, and thus, developing a facile, mild, efficient, operationally simple synthetic method is necessary. This study designed a method of synthesizing 2,3-disubstituted benzofuran derivatives using easily prepared o-hydroxychalcones and commercially available γ-bromocrotonates as starting materials. The reaction proceeded via a one-pot multistep tandem process under mildly basic conditions. This strategy avoided the use of expensive metal catalysts and harsh reaction conditions, demonstrating a good functional-group compatibility and operational simplicity. This synthetic strategy provided a novel approach for use in efficiently synthesizing 2,3-disubstituted benzofuran derivatives. It also laid a solid foundation for further in-depth research into their biological activities and material properties, displaying potential for application in the fields of medicinal chemistry and organic synthesis.

Key words：benzofuran; synthesis; base promotion; o-hydroxychalcone; γ-bromocrotonate

双亲性去磷脂填料的制备及其在兽残检测中的应用

徐晨，王明，陈武炼^*

(上海安谱实验科技股份有限公司，上海 200000)

摘要：针对复杂食品基质中兽残检测困难、磷脂去除难的问题，通过在硅胶表面修饰十八烷基三氯硅烷（Octadecyltrichlorosilane,OTS），制备了一种双亲性的去磷脂材料（Phospholipid removal material,PPR）。通过FTIR、SEM、N₂吸附-脱附仪等对材料进行表征，证明PPR填料的成功制备。基于PPR填料的固相萃取与液相色谱-质谱/质谱（HPLC-MS/MS）联用技术，建立了一种能快速净化食品基质磷脂并检测食品中19种兽残的分析方法。结果表明，制备的PPR填料对鸡蛋、全脂牛奶、鸡肉、猪肉这4种食品基质的磷脂净化率为98.58%~99.91%,相对标准偏差3.9%~5.6%，PRiME HLB的磷脂去除率为94.09%~99.64%，相对标准偏差2.8%~5.9%；在19种β-受体激动剂和喹诺酮类兽残加标实验中，PPR填料对鸡蛋的兽残加标回收率为81.0%~102.3%，相对标准偏差1.4%~8.2%，PRiME HLB的兽残加标回收率为80.5%~104.3%，相对标准偏差在3.1%~9.4%。PPR填料的磷脂净化率及兽残加标回收率与市售进口产品性能相当，且具有制备简便、成本低、磷脂净化效率高等特点，在食品安全检测领域具有广泛应用前景。

关键词：兽残；磷脂；固相萃取；喹诺酮；受体激动剂

中图分类号：O657.63     文献标志码：A     文章编号：

DOI：10.13822/j.cnki.hxsj.2025.0293

Preparation of Amphiphilic Phospholipid Removal Fillers and the Application in Animal Residue Detection  XU Chen, WANG Ming, CHEN Wu-lian^*  (ANPEL Laboratory Technologies(Shanghai) Inc., Shanghai 200000, China )

Abstract: To address the analytical challenges in veterinary drug residue detection in complex food matrices, particularly the interference from phospholipid that can affect detection accuracy and instrument performance, a novel amphiphilic phospholipid removal material (PPR) was developed. The PPR material was prepared by surface modification of octadecyltrichlorosilane (OTS) on silica gel, providing both hydrophobic and hydrophilic properties. The successful fabrication of the PPR material was confrimed using Fourier-transform infrared spectroscopy (FTIR) for functional group identification, scanning electron microscopy (SEM) for morphological analysis, and nitrogen adsorption-desorption measurements for surface area and pore structure evaluation. A reliable analytical methodology was subsequently established by integrating the PPR filler based solid-phase extraction (SPE) with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), enabling rapid purification of phospholipids from food matrices and simultaneous detection of 19 veterinary drug residues. The results showed that the prepared PPR filler had a phospholipid purification rate of 98.58%~99.91%, with a relative standard deviation of 3.9%~5.6% for four food matrices: eggs, whole milk, chicken, and pork. The phospholipid removal rate of PRiME HLB was 94.09%~99.64%, with a relative standard deviation of 2.8%~5.9%; In the animal residue spiked experiments of 19 types of β-receptor agonists and quinolones, the recovery rate of PPR fillers for animal residues in eggs was 81.0%~102.3%, with a relative standard deviation of 1.4%~8.2%. The recovery rate of PRiME HLB for animal residues was 80.5%~104.3%, with a relative standard deviation of 3.1%~9.4%. The phospholipid removal efficiency and residue recovery of PPR fillers are comparable to the performance of commercially available imported products. PPR fillers have the characteristics of simple preparation, good stability, low cost, high phospholipid purification efficiency, indicating potential for widespread application in food safety testing.

Key words: beast remnants; phospholipids; solid phase extraction; quinolone; receptor agonist

【综述与专论】

共价有机笼在药物递送、生物成像和生物传感中的研究进展

王满江，于江，魏会强，侯文彬，李?亮^*

(中国医学科学院北京协和医学院 放射医学研究所，天津  300192)

摘要：共价有机笼（COCs）是一类由有机小分子通过共价键构筑的离散笼状功能材料，具有空腔尺寸可调、结构明确、化学稳定性高及溶液可加工性优良等核心特征。近年来，COCs 在生物医学领域展现出巨大应用潜力，尤其在药物递送、生物成像和生物传感3大方向取得显著进展。在药物递送方面，通过精准结构设计与功能化修饰，COCs 可实现对芳香族、疏水性等不同类型药物的高选择性包载，结合 pH、氧化还原、酶响应等刺激机制，实现药物的靶向可控释放，显著提升治疗效果并降低毒副作用。在生物成像领域，COCs 可通过嵌入荧光模块、配合顺磁金属离子或负载放射性核素，构建荧光、磁共振、PET 等单模态及多模态成像探针，兼具高灵敏度、低生物蓄积风险及良好生物相容性。在生物传感领域，依托其精确定义的分子空腔与可控表面化学，COCs 可实现对 ATP、活性氧、金属离子及生物标志物的高特异性识别与信号转导，展现出优异的传感性能。系统综述了 COCs 的结构设计、合成策略及生物功能化修饰方法，重点探讨其在上述3大领域的作用机制与代表性应用，并分析了 COCs 在生物稳定性、体内代谢、规模化制备等方面面临的关键挑战，最后对其在精准医学、疾病早筛等领域的未来发展方向进行展望，为相关研究提供参考。 

关键词：共价有机笼；动态共价化学：药物递送；生物成像；生物传感

中图分类号：O657      文献标识码：A      文章编号：0258-3283（2026）--

DOI：10.13822/j.cnki.hxsj.2026.0001

Research Progress of Covalent Organic Cages in Drug Delivery, Bioimaging, and Biosensing WANG Man-jiang, YU Jiang, WEI Hui-qiang, HOU Wen-bin, LI Yi-liang^* (Institute of Radiation Medicine, Chinese Academy of Medical Sciences & Peking Union Medical College, Tianjin 300192, China)

Abstract: Covalent organic cages (COCs) are a class of discrete cage-like functional materials constructed from small organic molecules via covalent bonding and feature tunable cavity sizes, well-defined structures, high chemical stability, and excellent solution processability. In recent years, COCs have demonstrated enormous application potential in the biomedical field, achieving remarkable progress in three key areas in particular: drug delivery, bioimaging, and biosensing. For drug delivery, COCs that achieve the highly selective encapsulation of various drugs, such as aromatic and hydrophobic agents, have been developed through precise structural design and functional modification. Combined with stimulus-responsive mechanisms, including pH, redox, and enzyme responsiveness, these COCs enable targeted and controlled drug release, significantly enhancing therapeutic efficacy while reducing side effects. For bioimaging, COCs can be engineered into single-modal and multimodal imaging probes (e.g., fluorescence, magnetic resonance, and PET) that exhibit high sensitivity, low bioaccumulation risk, and favorable biocompatibility by incorporating fluorescent modules, chelating paramagnetic metal ions, or loading radionuclides. Further, owing to their precisely defined molecular cavities and controllable surface chemistry, COCs can realize the highly specific recognition and signal transduction of ATP, reactive oxygen species, metal ions, and biomarkers, thereby exhibiting outstanding performance in biosensing. This review systematically summarizes the structural design, synthetic strategies, and biological functionalization methods of COCs, focusing on their mechanisms of action and representative applications in the above three areas. It also analyzes the key challenges faced by COCs in terms of their biological stability, in vivo metabolism, and large-scale production. Finally, the future development directions of COCs in precision medicine, early disease screening, and other fields are discussed, providing references for related research.

Key words: covalent organic cages; dynamic covalent chemistry; drug delivery; bioimaging; biosensing

肝缺血再灌注损伤可视化荧光探针的研究进展

张文轩^a，徐黎^a，冯书敏^a，李玉桃^*b

（湖北中医药大学 a. 药学院, b. 检验学院，湖北武汉  430065）

摘要：肝缺血再灌注损伤（HIRI）是肝切除、肝移植等手术中常见的严重并发症，其机制涉及缺血期能量代谢障碍与再灌注期氧化应激爆发、钙超载及多种细胞死亡途径的复杂级联过程。传统诊断方法如血清学检测、影像学检查存在灵敏度低、时空分辨率差、有创性强等局限性，难以实现 HIRI 关键生物标志物的早期、动态监测。近年来，荧光探针技术凭借其高灵敏度、实时可视化能力，成为解析 HIRI 分子机制的重要工具。首先系统阐述了HIRI的病理进展，并梳理了与其密切相关的核心生物标志物，包括活性氧物种（ROS）、微环境参数（如粘度）、能量代谢物（如ATP、线粒体DNA）及气体信号分子（如H₂S）等。在此基础上，重点综述了针对这些标志物设计开发的各类荧光探针的研究进展，依据其检测目标与设计策略，分为活性氧与能量代谢探针、微环境参数探针、气体信号分子探针以及近红外与多响应探针等类别进行详细评述，总结了探针的设计原理、响应机制、成像性能及应用实例。最后探讨当前荧光探针技术面临的挑战，并展望其在未来的发展方向。

关键词：缺血再灌注损伤；荧光探针；生物标志物；靶向性；近红外

中图分类号：O657      文献标识码：A      文章编号：0258-3283（2026）--

DOI：10.13822/j.cnki.hxsj.2026.0022

Advances in Fluorescent Probes for Visualizing Hepatic Ischemia-Reperfusion Injury Zhang Wen-xuan^a, Xu Li^a, Feng Shu-min^a, Li Yu-tao^*b (a. College of Pharmacy, b. College of Laboratory Medicine, Hubei University of Chinese Medicine, Wuhan 430065, China)

Abstract: Hepatic ischemia-reperfusion injury (HIRI) is a severe complication in surgeries, such as hepatectomy and liver transplantation, and involves a complex cascade of ischemia-induced energy failure, oxidative stress, calcium overload, and cell death upon reperfusion. Conventional diagnostic approaches, including serologic assays and imaging techniques, are limited by low sensitivity, poor spatiotemporal resolution, and invasiveness, thereby restricting early and in situ detection of critical biomarkers. Fluorescent probe technology has emerged as a powerful tool for studying HIRI owing to its high sensitivity, spatiotemporal resolution, and real-time imaging capabilities. This review first outlines the pathological progression of HIRI and the key biomarkers implicated in this process, including reactive oxygen species (ROS), microenvironmental parameters (e.g., viscosity), energy metabolites (e.g., ATP and mitochondrial DNA), and gas signaling molecules (e.g., H₂S). Subsequently, we systematically summarize recent advances in the design and application of fluorescent probes that target these biomarkers. These probes are categorized and discussed based on their detection targets and design strategies, including probes for ROS, energy metabolism, microenvironmental parameters, gas signaling molecules, and near-infrared and multi-responsive probes, with a focus on their design principles, response mechanisms, imaging performance, and representative applications. Finally, we address the current challenges in reversible detection, multi-analyte imaging, and clinical translation while highlighting future applications of fluorescent probes in the early diagnosis, mechanistic research, drug evaluation, and surgical guidance of HIRI.

Key words: ischemia-reperfusion injury; fluorescent probes; biomarkers; targeting; near-infrared imaging

辅助结晶研究进展及其在天然产物结构鉴定中的应用

连子娇0F^,2，李正³，赵玉培⁴，郭晶²，臧新钰^3,5，章见亮^*3，扈靖^*1,2,3,5

（1. 天津中医药大学 中药学院，天津  301617；2. 盈科瑞（天津）创新医药研究有限公司，天津300382；3. 北京盈科瑞创新药物研究有限公司，天津  300382；4. 北京盈科瑞药物安全有效性研究有限公司，北京  102200；5. 北京盈科瑞创新医药股份有限公司，北京  102200）

摘要: 单晶X射线衍射在天然产物结构鉴定中的应用已十分广泛，但是许多天然产物在成功培养高质量单晶的过程中还面临挑战。为克服传统单晶培养方法的局限性，目前已经发展出多种利用分子间特异性相互作用的超分子创新辅助结晶策略，包括晶体海绵（在预先形成的多孔晶体中对有机分子进行有序排列）和结晶伴侣（基于非固有多孔通道材料的结晶伴侣与有机分子共结晶）。深入总结了辅助结晶策略的前沿进展，并将晶体海绵与结晶伴侣进行了系统的分类，详细阐述了各类方法的基本原理及其在天然产物结构鉴定中的应用，旨在促进研究人员更高效地借助辅助结晶策略来鉴定天然产物的结构。另外，可通过晶体结构预测来计算模拟最佳结晶条件，探索人工智能、机器学习相结合调控结晶的新方法。

关键词：晶体海绵；结晶伴侣；天然产物；单晶X射线衍射；结构鉴定

中图分类号：O65  文献标识码：A    文章编号： 

DOI: 10.13822/j.cnki.hxsj.2025.0309

Recent Advances in Assisted Crystallization and Their Applications in the Structural Identification of Natural Products  LIAN Zi-jiao^1,2，LI Zheng³，ZHAO Yu-pei⁴，GUO Jing²，ZANG Xin-yu^3,5，ZHANG Jian-liang^*3，HU Jing^*1,2,3,5  (1. School of Chinese Materia Medica, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China;2. Increasepharm (Tianjin) Innovative Medicine Institute Limited, Tianjin 300382, China;3. Beijing Increasepharm Innovative Medicine Institute Limited, Tianjin 300382, China;4. Beijing Increasepharm Safety and Efficacy Co., Ltd, Beijing 102200, China;5. Beijing Increasepharm Pharmaceutical Research Co., Ltd, Beijing 102200, China)

Abstract: Single-crystal X-ray diffraction is widely used to elucidate the structure of natural products. However, the cultivation of high-quality single crystals from natural products remains challenging. To overcome the limitations of traditional cultivation methods, new supramolecular-assisted crystallization strategies that utilize specific intermolecular interactions have been developed. These methodologies include the crystalline sponge method (which involves an orderly arrangement of organic molecules within preformed porous crystals) and the crystallization chaperone method (co-crystallization with organic molecules based on a non-intrinsic channel material). This review comprehensively summarizes the recent advances in these assisted crystallization strategies. A systematic classification of crystalline sponges and crystallization chaperones is provided, along with a detailed discussion of their principles and applications in the structural identification of natural products, with the aim of facilitating more efficient utilization of these strategies to determine the structures of natural products. Additionally, crystal structure prediction can be employed to computationally simulate the optimal crystallization conditions and explore new approaches that integrate artificial intelligence and machine learning to regulate crystallization.

Key words：crystalline sponges; crystallization chaperones; natural products; single crystal X-ray diffraction; structural determination

【功能材料】

核壳型铜铁银纳米复合材料的杀菌活性研究

钱晓雨，蔺咏梅，皇甫彤，饶珂萌^*

（陕西三二?一医院 感染性疾病科，陕西汉中  723000）

摘要：由病原微生物引起的感染已成为全球公共卫生、生态环境及经济稳定的重大威胁。尤其随着传统有机抗生素的滥用，多重耐药菌的不断出现使得现有防治手段面临严峻挑战。为此，通过一锅法成功构建了CuFe₂O₄纳米载体，并借助表面修饰策略将超小粒径的纳米Ag均匀负载于其表面，制备出具有核壳结构的CuFe₂O₄@Ag纳米复合材料。该结构不仅有效抑制了银纳米颗粒的团聚，还能够在有氧条件下通过类Fenton反应持续产生·OH与¹O₂等活性氧（ROS）物种，并与释放的Cu²⁺、Fe³⁺及Ag⁺等多种金属离子发挥协同杀菌效应。实验结果表明，CuFe₂O₄@Ag对大肠杆菌（E. coli）、金黄色葡萄球菌（S. aureus）及耐甲氧西林金黄色葡萄球菌（MRSA）均表现出优异的杀菌活性，在15 min内杀菌率均达到99.99%以上。机制研究表明，材料释放的金属离子与ROS共同作用，不可逆地破坏了细菌细胞壁的负电性环境，中和表面电荷，导致细胞膜完整性丧失，引发胞内质粒、核酸及关键离子外泄，最终致使细菌死亡。因此，CuFe₂O₄@Ag纳米复合材料展现出快速、广谱且高效的杀菌性能，在医疗器械表面防护及抗感染材料领域具有重要的应用前景。

关键词：杀菌；杀菌机制；大肠杆菌；金黄色葡萄球菌；耐药

中图分类号：O611.4      文献标识码：A      文章编号：0258-3283（2026）--

DOI：10.13822/j.cnki.hxsj.2025.0294

Antibacterial Activity of Core?Shell Copper?Iron?Silver Nanocomposites QIAN Xian-yu, LIN Yong-mei, HUANG Fu-Tong, RAO Ke-meng^* (Infectious diseases Department of Shaanxi 3201 Hospital , Hanzhong 723000, China)

Abstract: Infections caused by pathogenic microorganisms have emerged as a major threat to global public health, the ecological environment, and economic stability. In particular, owing to the widespread misuse of conventional organic antibiotics, the continuous emergence of multidrug-resistant bacteria poses severe challenges to existing prevention and treatment strategies. To that end, this study constructed a CuFe₂O₄ nanocarrier via a one-pot method and, through surface-modification strategies, uniformly loaded ultrasmall silver nanoparticles onto its surface to prepare a CuFe₂O₄@Ag nanocomposite with a core?shell structure. This architecture not only effectively inhibits the aggregation of silver nanoparticles but also enables the continuous generation of reactive oxygen species (ROS) such as ·OH and ¹O₂ under aerobic conditions via a Fenton-like reaction, which synergizes with released metal ions such as Cu²⁺, Fe³⁺, and Ag⁺ to exert bactericidal effects. Experimental results show that CuFe₂O₄@Ag exhibits excellent antibacterial activity against Escherichia coli, Staphylococcus aureus, and methicillin-resistant Staphylococcus aureus, with a sterilization rate exceeding 99.99% achieved within 15 min. Mechanistic studies reveal that the released metal ions and ROS function synergistically to irreversibly disrupt the negatively charged environment of bacterial cell walls. This neutralizes surface charges, compromises the cell-membrane integrity, and induces the leakage of intracellular plasmids, nucleic acids, and key ions, thus ultimately resulting in bacterial death. The CuFe₂O₄@Ag nanocomposite demonstrates rapid, broad-spectrum, and highly efficient antibacterial performance, thereby showcasing its significant application potential in medical-device surface protection and anti-infective materials.

Key words：bactericidal; bactericidal mechanism; escherichia coli; staphylococcus aureus; drug resistance

一种萘碳酰腙荧光探针对Al³⁺检测和生物成像研究

张继东^*a,b，吴勇^a ，谢冬^a，吕宗菀^a，刘小月^a，姜西蒙^a 

(安康学院a.化学与环境学院 陕西省富硒食品质量监督检验中心，b.界面多孔材料陕西省高等学校重点实验室，陕西安康725000)

摘要：设计合成了两种萘碳酰腙类荧光探针L1和L2，并对其结构通过¹HNMR和ESI-MS进行了表征，其中探针L1（10 µmol/L）在V（乙醇）:V（HEPES buffer）=3:7(pH 7.4)溶液中对Al³⁺在水溶液中表现出高选择性，高灵敏性识别能力，不受其它离子干扰。采用Job，Pot实验、ESI-MS、¹HNMR和DFT理论计算进行了分析，其检测机理为光诱导电子转移（PET）进程和-C=N-异构化行为。DFT理论计算预测了其结合模式为Al(L1)₂，ESI-MS，¹HNMR和Job，Pot实验结果与其保持一致。通过荧光滴定实验表明，探针L1对Al³⁺浓度荧光强度在一定范围内呈良好线性关系，检出限低至47.3 nmol/L。L1在细胞中的表现出良好的细胞透过性，可以用于细胞中外源性Al³⁺离子的荧光成像检测。综上所述，荧光探针L1具备对Al³⁺表现出高选择性、高灵敏性，可成功应用于溶液中Al³⁺的检测，为萘碳酰腙类金属离子识别探针的设计与应用提供借鉴依据。

关键词：萘碳酰腙；荧光探针；铝离子检测；细胞成像；DFT理论计算

中图分类号：O62    文献标识码：A    文章编号： 

DOI：10.13822/j.cnki.hxsj.2026.0005

Naphtho-Carbonyl Hydantoin?Based Fluorescent Probes for Selective Al³⁺ Detection and Cellular Imaging  ZHANG Ji-dong^*a,b, WU Yong^a, XIE dong^a, LV Zong-yu^a, LIU Xiao-yue^a，JIANG Xi-meng^a (a.Shaanxi Province Selenium-rich Food Quality Supervision and Inspection Center College of Chemistry and Environment, b. Shaanxi Provincial Key Laboratory of Porous Materials for Interface Engineering, Ankang University, Ankang 725000) 

Abstract：Two naphtho-carbonyl hydantoin-based fluorescent probes, L1 and L2, were designed and synthesized, and their structures were characterized by proton nuclear magnetic resonance (¹HNMR) spectroscopy and electrospray ionization mass spectrometry (ESI-MS). Among them, L1 (10 µmol/L) exhibited high selectivity and sensitivity toward Al³⁺ in an aqueous medium composed of V（ethanol）:V（HEPES buffer）=3:7(pH 7.4), with negligible interference from other metal ions. The binding mechanism was investigated using Job’s plot analysis, potentiometric titration, ESI-MS, ¹HNMR spectroscopy, and density functional theory (DFT) calculations. The results indicated that the sensing response arose from inhibition of photoinduced electron transfer (PET) and restriction of C=N bond isomerization. DFT calculations suggested an Al(L1)₂ binding stoichiometry, which was consistent with the ESI-MS, ¹HNMR, and Job’s plot/potentiometric titration results. Fluorescence titration revealed a good linear relationship between the fluorescence intensity of L1 and Al³⁺ concentration within a defined range, with a detection limit as low as 47.3 nmol/L. In addition, L1 demonstrated excellent cell membrane permeability and was successfully applied to fluorescence imaging of exogenous Al³⁺ in living cells. Overall, L1 functions as a highly selective and sensitive fluorescent probe for Al³⁺ in both aqueous solutions and cellular environments. These findings provide a useful reference for the rational design and development of naphtho-carbonyl hydantoin-based fluorescent probes for metal-ion detection.

Keywords：naphtho-carbonyl; hydantoin; fluorescent probe; aluminum ion detection; cell image; density functional theory

【分离提取技术】

用工业乙腈制备梯度级色谱乙腈的研究

董艺萌^*，杨长青，刘若峰,于朴凡，王路

（北京化学试剂研究所有限责任公司，北京  102607）

摘要：随着液相色谱在药物分析、生物分离等领域的深入应用，作为常用的液相色谱流动相之一的色谱纯乙腈对紫外透光性、基线稳定性和批次一致性有非常严苛的标准。采用工业级乙腈为原料，使用氧化、吸附、精馏等工艺进行提纯，深入探索了乙腈中微量水分的去除方法，分析和讨论了水分难以去除的原因，讨论和确定了精馏塔的液泛速度和压力降重要的关键参数的设定。该工艺可以中试规模、多批次连续生产出高纯度色谱级乙腈，所得产品在195~280 nm波长范围内的紫外吸光度低至0.002~0.026，基线平稳无杂峰，其中在190 nm处的吸光度稳定控制在0.015以下，产品的各项指标优于默克公司在售产品。经实践表明，该技术路线具有工艺流程合理、操作稳定可靠、产品质量优异等特点，特别适用于高纯度色谱级乙腈的规模化生产，为高端分析检测领域提供了可靠的技术支撑。

关键词：分子筛；色谱乙腈；活性炭；精馏；吸附

中图分类号：O65;TQ421    文献标识码：A    文章编号：   

DOI：10.13822/j.cnki.hxsj.2025.0301

Research on the Preparation of Gradient-Grade Acetonitrile from Industrial Acetonitrile  DONG Yi-meng*, YANG Chang-qing, LIU Ruo-feng, YU Pu-fan, Wang Lu (Beijing Research Institute of Chemical Reagents Co., Ltd., Beijing 102607, China)

Abstract：With the increasing application of liquid chromatography in fields such as pharmaceutical analysis and biological separation, the requirements for key mobile-phase solvents have become increasingly stringent. Chromatographic-grade acetonitrile, which is one of the most commonly used solvents, must meet rigorous standards for ultraviolet (UV) transmittance, baseline stability, and batch-to-batch consistency. Industrial-grade acetonitrile was employed as the raw material. A purification process integrating oxidation, adsorption, and rectification was systematically implemented. A removal method for trace water in acetonitrile, a critical impurity affecting the UV performance, was thoroughly investigated. Challenges associated with water removal, including its strong interactions and potential azeotropic behavior, were analyzed and discussed. Furthermore, key operational parameters for the rectification column, namely, the flooding velocity and pressure drop, were examined and optimized to ensure stable and efficient operation, enabling the continuous, multi-batch production of high-purity chromatographic-grade acetonitrile on a pilot scale. The obtained product exhibited exceptional performance; the UV absorbance was as low as 0.026~0.002 across the 195~280 nm wavelength range, accompanied by a flat and clean baseline free from extraneous peaks. Notably, the absorbance at the highly demanding 190 nm wavelength was consistently controlled below 0.015. A comprehensive evaluation confirmed that all critical performance indicators of the product surpassed those of commercially available Merck products. Practical application demonstrated that this technical route features a rational process design, stable and reliable operation, and excellent product quality. This method is particularly suitable for the large-scale production of high-purity chromatographic-grade acetonitrile. This study provides reliable technical support and a viable material solution for high-end analytical and detection applications, offering a competitive alternative for domestic supply in this specialized sector.

Keywords: molecular sieves; chromatographic-grade acetonitrile; activated carbon; distillation; adsorption

【分析与测试】

复杂基质中新精神活性物质分析方法研究进展

邹秀静¹，贺锦灿^*1，李亚庆²，姚宏忠²，程良红^*2，张毅³

(1. 广东药科大学 公共卫生学院 广东广州 10006，2. 广东省证据材料司法鉴定（南天）工程技术研究中心 广东深圳 18055，3. 深圳市职业技术大学 广东 深圳  18055)  

摘要：新精神活性物质（New Psychoactive Substances，NPS）是一类尚未被国际禁毒公约列管、具有滥用潜力并可对公共健康构成严重威胁的一类物质。该类物质常通过结构修饰规避法律监管，给监管与公共健康防控带来严峻挑战。建立高效可靠的分析检测方法对NPS的监测与管控具有重要意义。本文综述复杂基质中NPS前处理技术与分析检测方法的研究进展。在样品前处理方面，固相萃取、液相微萃取及QuEChERS等方法已被广泛应用于生物体液、污水及毛发等复杂样本中NPS的提取与净化，但仍面临步骤繁琐、回收率不稳定等问题。在分析检测领域，气相色谱-质谱联用、液相色谱-高分辨质谱等技术已成为NPS结构鉴定与定量分析的主要手段，其中高分辨质谱凭借其高灵敏度和准确质量数测定能力，在未知NPS识别中发挥关键作用。然而，现有方法仍存在分析周期长、设备依赖度高、新出现结构响应滞后等局限。发展更简便、高效与自动化的前处理技术，与快速、高通量及现场化分析手段是预期NPS检测的主要方向，以期以提升对NPS的识别效率并减少对化学修饰NPS的监管漏洞。

关键词: 新精神活性物质；样品前处理；分析检测方法；液相色谱-高分辨质谱；高通量分析；药物滥用监测

中图分类号：R123，O65      文献标识码：A      文章编号：0258-3283（2026）--

DOI：10.13822/j.cnki.hxsj.2025.0271

Research Progress into Analytical Methods for New Psychoactive Substances ZOU Xiu-jing¹, HE Jin-can^*1, LI Ya-qing², YAO Hong-zhong², CHENG Liang-hong², ZHANG Yi³ (1. Guangdong Pharmaceutical University, School of Public Health, Guangzhou 510006, China; 2. Guangdong Provincial Forensic Science of Evdience Materials (Nantian) Engineering Technology Reasearch Center, Shenzhen 18055, China; 3. Shenzhen Polytechnic University, Guangdong, Shenzhen 518055, China)

Abstract: New psychoactive substances (NPS) are chemical entities that have not yet been scheduled under international drug control conventions, possess abuse potential, and pose serious threats to public health. These substances often exploit structural modifications to circumvent legal controls, thereby presenting significant regulatory challenges and public-health-protection obstacles. Establishing efficient and reliable analytical detection methods for monitoring and controlling NPS is therefore an important objective. This article reviews recent advances in sample-pretreatment techniques and analytical-detection methods for NPS in complex matrices. Sample-pretreatment methods such as solid-phase extraction, liquid-phase microextraction, and QuEChERS have been widely used to extract and purify NPS from complex samples, including biological fluids, wastewater, and hair. However, some issues, including cumbersome procedures and inconsistent recovery rates, remain. Analytical-detection techniques such as gas chromatography?mass spectrometry and liquid chromatography?high-resolution mass spectrometry have become primary tools for identifying MPS structures and analyzing them quantitatively. Among these, high-resolution mass spectrometry plays a key role in identifying unknown NPS owing to its high sensitivity and accurate mass-measuring capability. Nevertheless, existing methods still face limitations, including long analytical cycles, high dependences on specialized equipment, and delayed responses to newly emerging structural analogs. Future developments are anticipated to focus on simpler, more-efficient, and automated pretreatment techniques, along with rapid, high-throughput, and on-site analytical approaches aimed at making NPS identification more efficient and reducing regulatory gaps for chemically modified analogs.

气相色谱-质谱法测定化妆品中除草醚和吡氟禾草灵残留

蔡翠玲，侯颖烨，钟钰，曾广丰，谢建军，董洁，王璐^*

(广州海关技术中心 国家级进出口食品质量安全风险验证评价实验室（化妆品），广东广州 510623）

摘要：天然健康的化妆品受到越来越多消费者青睐和关注，但在化妆品中添加植物提取液却存在农药残留的风险，因此，亟需建立化妆品中相应农药残留的检测方法。建立了同时测定化妆品中除草醚和吡氟禾草灵残留量的气相色谱-质谱法。样品采用乙腈水溶液超声提取、增强型脂质去除（Enhanced matrix removal-lipid dispersion，EMR-Lipid）固相萃取柱净化、经HP-5MS毛细管柱（30.0 m×0.25 mm×0.25 μm）分离，在多反应监测（MRM）模式下检测，采用基质匹配标准曲线、外标法定量。结果表明，除草醚在0.020~0.500 mg/L范围内线性关系良好，线性相关系数（r²）≥0.9936，检出限0.020 mg/kg，定量限0.050 mg/kg；吡氟禾草灵在0.004~0.100 mg/L范围内线性关系良好，r²≥0.9925，检出限0.004 mg/kg，定量限0.010 mg/kg。在6种化妆品空白基质添加高、中、低3个浓度水平的除草醚和吡氟禾草灵，平均回收率分别为91.08%~109.68%和81.47%~109.87%，相对标准偏差（RSD，n=6）分别为0.50%~10.97%和0.30%~9.41%。采用该方法对30个化妆品实际样品进行检测，结果均未检出除草醚和吡氟禾草灵。该方法适用性广、准确性高、灵敏度高，为化妆品中除草醚和吡氟禾草灵的筛查监测和风险评估提供了方法支撑。

关键词：气相色谱-质谱法；除草醚；吡氟禾草灵；化妆品；农药残留

中图分类号：O65-分析化学    文献标识码：A    文章编号：

DOI：10.13822/j.cnki.hxsj.2025.0290

Determination of Nitrofen and Fluazifop-butyl in Cosmetics by Gas Chromatography?Mass Spectrometry   CAI Cui-ling，HOU Ying-ye，ZHONG Y, ZENG Guang-feng，XIE Jian-jun，DONG Jie，WANG Lu ^*  （National Import and Export Food Quality Safety Risk Verification and Evaluation Laboratory (Cosmetics) ，Guangzhou Customs Technical Center, Guangzhou 510623, China, Guangzhou 510623, China)

Abstract: Cosmetics with natural and healthy characteristics are increasingly favored by consumers. However, adding plant extracts to cosmetics poses risks owing to the potential presence of pesticide residues. Nitrofen and fluazifop-butyl are widely used herbicides that are clearly listed in the Technical Specification for Cosmetics Safety (2015 edition) regulations as potentially detectable in cosmetics. Therefore, there is an urgent need to develop methods for detecting pesticide residues in cosmetics. We established a gas-chromatography?mass-spectrometry-based (GC?MS-based) method for simultaneously determining nitrofen and fluazifop-butyl in cosmetics. The sample is first ultrasonically extracted with aqueous acetonitrile and then centrifuged. The supernatant is then purified using an enhanced matrix-removal?lipid-dispersion (EMR?lipid) solid-phase extraction column. The analytes are then separated using an HP-5MS capillary column (length: 30.0 mm, diameter: 0.25 mm, film thickness: 0.25 μm), and the compounds are analyzed by GC-MS and quantified using the external-standard method and a matrix-matched calibration curve. Nitrofen exhibited a good linear relationship in the 0.020?0.500 mg/L range, with a coefficient of determination (r²) of ≥0.9936, and limits of detection (LOD) and quantification (LOQ) of 0.020 and 0.050 mg/kg, respectively. Additionally, fluazifop-butyl exhibited a good linear relationship in the 0.004~0.100 mg/L range, with r² ≥0.9925, and an LOD and LOQ of 0.004 and 0.010 mg/kg, respectively. Average nitrofen and fluazifop-butyl recoveries of 91.08?109.68% and 81.47%~109.87%, respectively, were determined by adding high, medium, and low concentrations of the pesticides to six different blank matrices, with relative standard deviations (RSDs, n=6) of 0.50~10.97% and 0.30~9.41%, respectively. The developed method was used to analyze 30 cosmetic samples, with neither nitrofen nor fluazifop-butyl detected in any of the samples. The established method is widely applicable, highly accurate, and easy to use, providing methodological support for the screening, monitoring, and risk assessment of nitrofen and fluazifop-butyl in cosmetics.

Key words: gas chromatography?mass spectrometry (GC-MS); nitrofen; fluazifop-butyl; cosmetics;pesticide residue