2026年48(3)中英文摘要
【特約專稿】
改性生物炭吸附水體中微塑料的研究:改性方法和去除機理
羅堂,李錦雅,紀鵬宇,范世鎖*
(安徽農業大學 資源與環境學院,安徽 合肥 230036)
摘要: 微塑料作為一種新興的全球性環境污染物,在水體中廣泛分布,對生態系統和人類健康構成嚴重威脅。生物炭因其獨特的孔隙結構和表面性質,在環境污染治理中展現出廣闊前景。然而,原狀生物炭對微塑料的吸附存在效率低、容量有限等問題,而功能化改性可顯著提升其吸附性能。系統綜述了改性生物炭去除水體中微塑料的研究進展。重點闡述了化學改性(如金屬負載、酸堿處理)與物理改性(如蒸氣活化)等方法,通過調控生物炭的孔隙結構、表面電荷和官能團,增強其與微塑料的作用。同時,深入剖析了物理截留、靜電吸引、氫鍵及表面絡合等多種吸附機制。進一步探討了生物炭自身特性、微塑料性質(如類型、粒徑)以及環境因素(如pH值、溶解性有機質)對吸附過程的綜合影響。此外,簡要評述了改性生物炭的再生技術與實際應用所面臨的挑戰,包括制備成本、長期生態安全性及在復雜水體環境中的穩定性問題。旨在為改性生物炭材料的優化設計及其在微塑料污染治理中的工程應用提供理論參考。
關鍵詞: 生物炭;微塑料;改性方法;吸附機制;影響因素;實際挑戰
中圖分類號:O647 文獻標識碼:A 文章編號: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
堿促進下2,3-二取代苯并呋喃的高效合成
張金坤,2,李芷樂3,邱小權3,黃年玉*3,王能中*3
(1. 三峽大學 第一臨床醫學院,湖北宜昌 443002;2. 宜昌市中心人民醫院,湖北 宜昌 443003;3. 三峽大學 生物與制藥學院 天然產物研究與利用湖北省重點實驗室,湖北宜昌 443002)
摘要:苯并呋喃作為一種重要的雜環結構單元,廣泛存在于天然產物、藥物分子、農藥以及功能材料中。同時,其本身作為一種潛力的合成子,用于制備多種多樣的生物活性分子。迄今為止,盡管苯并呋喃母核的合成方法已較為成熟,但針對2,3-二取代苯并呋喃的高效、通用的合成方法仍相對有限。現有的一些方法往往面臨反應條件苛刻、步驟繁瑣或底物普適性不佳等挑戰。因此,開發一種條件溫和、高效、操作簡便的合成方法是非常有必要的。基于此,設計以易于制備的鄰羥基查爾酮與商業可得的γ-溴代巴豆酸酯為原料,在溫和的堿性條件下,經過一鍋多步串聯反應生成一系列2,3-二取代苯并呋喃類化合物。該策略避免了使用昂貴金屬催化劑或苛刻反應條件,展現出良好的官能團兼容性與操作簡便性。該合成策略不僅為2,3-二取代苯并呋喃類化合物的高效合成提供了一條新穎途徑,也為后續深入研究這類化合物的生物活性及材料性能奠定了堅實的物質基礎,在藥物化學和有機合成領域具有潛在的應用價值。
關鍵詞:苯并呋喃;合成;堿促進;鄰羥基查爾酮;γ-溴代巴豆酸酯
中圖分類號:O62 文獻標識碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2025.0318
Base-Promoted Efficient Synthesis of 2,3-Disubstituted Benzofurans ZHANG Jin-kun1,2, 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
雙親性去磷脂填料的制備及其在獸殘檢測中的應用
徐晨,王明,陳武煉*
(上海安譜實驗科技股份有限公司,上海 200000)
摘要:針對復雜食品基質中獸殘檢測困難、磷脂去除難的問題,通過在硅膠表面修飾十八烷基三氯硅烷(Octadecyltrichlorosilane,OTS),制備了一種雙親性的去磷脂材料(Phospholipid removal material,PPR)。通過FTIR、SEM、N2吸附-脫附儀等對材料進行表征,證明PPR填料的成功制備。基于PPR填料的固相萃取與液相色譜-質譜/質譜(HPLC-MS/MS)聯用技術,建立了一種能快速凈化食品基質磷脂并檢測食品中19種獸殘的分析方法。結果表明,制備的PPR填料對雞蛋、全脂牛奶、雞肉、豬肉這4種食品基質的磷脂凈化率為98.58%~99.91%,相對標準偏差3.9%~5.6%,PRiME HLB的磷脂去除率為94.09%~99.64%,相對標準偏差2.8%~5.9%;在19種β-受體激動劑和喹諾酮類獸殘加標實驗中,PPR填料對雞蛋的獸殘加標回收率為81.0%~102.3%,相對標準偏差1.4%~8.2%,PRiME HLB的獸殘加標回收率為80.5%~104.3%,相對標準偏差在3.1%~9.4%。PPR填料的磷脂凈化率及獸殘加標回收率與市售進口產品性能相當,且具有制備簡便、成本低、磷脂凈化效率高等特點,在食品安全檢測領域具有廣泛應用前景。
關鍵詞:獸殘;磷脂;固相萃取;喹諾酮;受體激動劑
中圖分類號:O657.63 文獻標志碼:A 文章編號:
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
【綜述與專論】
共價有機籠在藥物遞送、生物成像和生物傳感中的研究進展
王滿江,于江,魏會強,侯文彬,李?亮*
(中國醫學科學院北京協和醫學院 放射醫學研究所,天津 300192)
摘要:共價有機籠(COCs)是一類由有機小分子通過共價鍵構筑的離散籠狀功能材料,具有空腔尺寸可調、結構明確、化學穩定性高及溶液可加工性優良等核心特征。近年來,COCs 在生物醫學領域展現出巨大應用潛力,尤其在藥物遞送、生物成像和生物傳感3大方向取得顯著進展。在藥物遞送方面,通過精準結構設計與功能化修飾,COCs 可實現對芳香族、疏水性等不同類型藥物的高選擇性包載,結合 pH、氧化還原、酶響應等刺激機制,實現藥物的靶向可控釋放,顯著提升治療效果并降低毒副作用。在生物成像領域,COCs 可通過嵌入熒光模塊、配合順磁金屬離子或負載放射性核素,構建熒光、磁共振、PET 等單模態及多模態成像探針,兼具高靈敏度、低生物蓄積風險及良好生物相容性。在生物傳感領域,依托其精確定義的分子空腔與可控表面化學,COCs 可實現對 ATP、活性氧、金屬離子及生物標志物的高特異性識別與信號轉導,展現出優異的傳感性能。系統綜述了 COCs 的結構設計、合成策略及生物功能化修飾方法,重點探討其在上述3大領域的作用機制與代表性應用,并分析了 COCs 在生物穩定性、體內代謝、規模化制備等方面面臨的關鍵挑戰,最后對其在精準醫學、疾病早篩等領域的未來發展方向進行展望,為相關研究提供參考。
關鍵詞:共價有機籠;動態共價化學:藥物遞送;生物成像;生物傳感
中圖分類號:O657 文獻標識碼:A 文章編號: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
肝缺血再灌注損傷可視化熒光探針的研究進展
張文軒a,徐黎a,馮書敏a,李玉桃*b
(湖北中醫藥大學 a. 藥學院, b. 檢驗學院,湖北武漢 430065)
摘要:肝缺血再灌注損傷(HIRI)是肝切除、肝移植等手術中常見的嚴重并發癥,其機制涉及缺血期能量代謝障礙與再灌注期氧化應激爆發、鈣超載及多種細胞死亡途徑的復雜級聯過程。傳統診斷方法如血清學檢測、影像學檢查存在靈敏度低、時空分辨率差、有創性強等局限性,難以實現 HIRI 關鍵生物標志物的早期、動態監測。近年來,熒光探針技術憑借其高靈敏度、實時可視化能力,成為解析 HIRI 分子機制的重要工具。首先系統闡述了HIRI的病理進展,并梳理了與其密切相關的核心生物標志物,包括活性氧物種(ROS)、微環境參數(如粘度)、能量代謝物(如ATP、線粒體DNA)及氣體信號分子(如H?S)等。在此基礎上,重點綜述了針對這些標志物設計開發的各類熒光探針的研究進展,依據其檢測目標與設計策略,分為活性氧與能量代謝探針、微環境參數探針、氣體信號分子探針以及近紅外與多響應探針等類別進行詳細評述,總結了探針的設計原理、響應機制、成像性能及應用實例。最后探討當前熒光探針技術面臨的挑戰,并展望其在未來的發展方向。
關鍵詞:缺血再灌注損傷;熒光探針;生物標志物;靶向性;近紅外
中圖分類號:O657 文獻標識碼:A 文章編號:0258-3283(2026)--
DOI:10.13822/j.cnki.hxsj.2026.0022
Advances in Fluorescent Probes for Visualizing Hepatic Ischemia-Reperfusion Injury Zhang Wen-xuana, Xu Lia, Feng Shu-mina, 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., H?S). 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
輔助結晶研究進展及其在天然產物結構鑒定中的應用
連子嬌0F,2,李正3,趙玉培4,郭晶2,臧新鈺3,5,章見亮*3,扈靖*1,2,3,5
(1. 天津中醫藥大學 中藥學院,天津 301617;2. 盈科瑞(天津)創新醫藥研究有限公司,天津300382;3. 北京盈科瑞創新藥物研究有限公司,天津 300382;4. 北京盈科瑞藥物安全有效性研究有限公司,北京 102200;5. 北京盈科瑞創新醫藥股份有限公司,北京 102200)
摘要: 單晶X射線衍射在天然產物結構鑒定中的應用已十分廣泛,但是許多天然產物在成功培養高質量單晶的過程中還面臨挑戰。為克服傳統單晶培養方法的局限性,目前已經發展出多種利用分子間特異性相互作用的超分子創新輔助結晶策略,包括晶體海綿(在預先形成的多孔晶體中對有機分子進行有序排列)和結晶伴侶(基于非固有多孔通道材料的結晶伴侶與有機分子共結晶)。深入總結了輔助結晶策略的前沿進展,并將晶體海綿與結晶伴侶進行了系統的分類,詳細闡述了各類方法的基本原理及其在天然產物結構鑒定中的應用,旨在促進研究人員更高效地借助輔助結晶策略來鑒定天然產物的結構。另外,可通過晶體結構預測來計算模擬最佳結晶條件,探索人工智能、機器學習相結合調控結晶的新方法。
關鍵詞:晶體海綿;結晶伴侶;天然產物;單晶X射線衍射;結構鑒定
中圖分類號:O65 文獻標識碼:A 文章編號:
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-jiao1,2,LI Zheng3,ZHAO Yu-pei4,GUO Jing2,ZANG Xin-yu3,5,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】
核殼型銅鐵銀納米復合材料的殺菌活性研究
錢曉雨,藺詠梅,皇甫彤,饒珂萌*
(陜西三二?一醫院 感染性疾病科,陜西漢中 723000)
摘要:由病原微生物引起的感染已成為全球公共衛生、生態環境及經濟穩定的重大威脅。尤其隨著傳統有機抗生素的濫用,多重耐藥菌的不斷出現使得現有防治手段面臨嚴峻挑戰。為此,通過一鍋法成功構建了CuFe?O?納米載體,并借助表面修飾策略將超小粒徑的納米Ag均勻負載于其表面,制備出具有核殼結構的CuFe?O?@Ag納米復合材料。該結構不僅有效抑制了銀納米顆粒的團聚,還能夠在有氧條件下通過類Fenton反應持續產生·OH與1O?等活性氧(ROS)物種,并與釋放的Cu2?、Fe3?及Ag?等多種金屬離子發揮協同殺菌效應。實驗結果表明,CuFe?O?@Ag對大腸桿菌(E. coli)、金黃色葡萄球菌(S. aureus)及耐甲氧西林金黃色葡萄球菌(MRSA)均表現出優異的殺菌活性,在15 min內殺菌率均達到99.99%以上。機制研究表明,材料釋放的金屬離子與ROS共同作用,不可逆地破壞了細菌細胞壁的負電性環境,中和表面電荷,導致細胞膜完整性喪失,引發胞內質粒、核酸及關鍵離子外泄,最終致使細菌死亡。因此,CuFe?O?@Ag納米復合材料展現出快速、廣譜且高效的殺菌性能,在醫療器械表面防護及抗感染材料領域具有重要的應用前景。
關鍵詞:殺菌;殺菌機制;大腸桿菌;金黃色葡萄球菌;耐藥
中圖分類號:O611.4 文獻標識碼:A 文章編號: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 CuFe?O4 nanocarrier via a one-pot method and, through surface-modification strategies, uniformly loaded ultrasmall silver nanoparticles onto its surface to prepare a CuFe?O4@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 1O? 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 CuFe?O4@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 CuFe?O?@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
一種萘碳酰腙熒光探針對Al3+檢測和生物成像研究
張繼東*a,b,吳勇a ,謝冬a,呂宗菀a,劉小月a,姜西蒙a
(安康學院a.化學與環境學院 陜西省富硒食品質量監督檢驗中心,b.界面多孔材料陜西省高等學校重點實驗室,陜西安康725000)
摘要:設計合成了兩種萘碳酰腙類熒光探針L1和L2,并對其結構通過1HNMR和ESI-MS進行了表征,其中探針L1(10 μmol/L)在V(乙醇):V(HEPES buffer)=3:7(pH 7.4)溶液中對Al3+在水溶液中表現出高選擇性,高靈敏性識別能力,不受其它離子干擾。采用Job,Pot實驗、ESI-MS、1HNMR和DFT理論計算進行了分析,其檢測機理為光誘導電子轉移(PET)進程和-C=N-異構化行為。DFT理論計算預測了其結合模式為Al(L1)2,ESI-MS,1HNMR和Job,Pot實驗結果與其保持一致。通過熒光滴定實驗表明,探針L1對Al3+濃度熒光強度在一定范圍內呈良好線性關系,檢出限低至47.3 nmol/L。L1在細胞中的表現出良好的細胞透過性,可以用于細胞中外源性Al3+離子的熒光成像檢測。綜上所述,熒光探針L1具備對Al3+表現出高選擇性、高靈敏性,可成功應用于溶液中Al3+的檢測,為萘碳酰腙類金屬離子識別探針的設計與應用提供借鑒依據。
關鍵詞:萘碳酰腙;熒光探針;鋁離子檢測;細胞成像;DFT理論計算
中圖分類號:O62 文獻標識碼:A 文章編號:
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 Yonga, XIE donga, LV Zong-yua, LIU Xiao-yuea,JIANG Xi-menga (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
【分離提取技術】
用工業乙腈制備梯度級色譜乙腈的研究
董藝萌*,楊長青,劉若峰,于樸凡,王路
(北京化學試劑研究所有限責任公司,北京 102607)
摘要:隨著液相色譜在藥物分析、生物分離等領域的深入應用,作為常用的液相色譜流動相之一的色譜純乙腈對紫外透光性、基線穩定性和批次一致性有非常嚴苛的標準。采用工業級乙腈為原料,使用氧化、吸附、精餾等工藝進行提純,深入探索了乙腈中微量水分的去除方法,分析和討論了水分難以去除的原因,討論和確定了精餾塔的液泛速度和壓力降重要的關鍵參數的設定。該工藝可以中試規模、多批次連續生產出高純度色譜級乙腈,所得產品在195~280 nm波長范圍內的紫外吸光度低至0.002~0.026,基線平穩無雜峰,其中在190 nm處的吸光度穩定控制在0.015以下,產品的各項指標優于默克公司在售產品。經實踐表明,該技術路線具有工藝流程合理、操作穩定可靠、產品質量優異等特點,特別適用于高純度色譜級乙腈的規模化生產,為高端分析檢測領域提供了可靠的技術支撐。
關鍵詞:分子篩;色譜乙腈;活性炭;精餾;吸附
中圖分類號:O65;TQ421 文獻標識碼:A 文章編號:
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
【分析與測試】
復雜基質中新精神活性物質分析方法研究進展
鄒秀靜1,賀錦燦*1,李亞慶2,姚宏忠2,程良紅*2,張毅3
(1. 廣東藥科大學 公共衛生學院 廣東廣州 10006,2. 廣東省證據材料司法鑒定(南天)工程技術研究中心 廣東深圳 18055,3. 深圳市職業技術大學 廣東 深圳 18055)
摘要:新精神活性物質(New Psychoactive Substances,NPS)是一類尚未被國際禁毒公約列管、具有濫用潛力并可對公共健康構成嚴重威脅的一類物質。該類物質常通過結構修飾規避法律監管,給監管與公共健康防控帶來嚴峻挑戰。建立高效可靠的分析檢測方法對NPS的監測與管控具有重要意義。本文綜述復雜基質中NPS前處理技術與分析檢測方法的研究進展。在樣品前處理方面,固相萃取、液相微萃取及QuEChERS等方法已被廣泛應用于生物體液、污水及毛發等復雜樣本中NPS的提取與凈化,但仍面臨步驟繁瑣、回收率不穩定等問題。在分析檢測領域,氣相色譜-質譜聯用、液相色譜-高分辨質譜等技術已成為NPS結構鑒定與定量分析的主要手段,其中高分辨質譜憑借其高靈敏度和準確質量數測定能力,在未知NPS識別中發揮關鍵作用。然而,現有方法仍存在分析周期長、設備依賴度高、新出現結構響應滯后等局限。發展更簡便、高效與自動化的前處理技術,與快速、高通量及現場化分析手段是預期NPS檢測的主要方向,以期以提升對NPS的識別效率并減少對化學修飾NPS的監管漏洞。
關鍵詞: 新精神活性物質;樣品前處理;分析檢測方法;液相色譜-高分辨質譜;高通量分析;藥物濫用監測
中圖分類號:R123,O65 文獻標識碼:A 文章編號: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.
氣相色譜-質譜法測定化妝品中除草醚和吡氟禾草靈殘留
蔡翠玲,侯穎燁,鐘鈺,曾廣豐,謝建軍,董潔,王璐*
(廣州海關技術中心 國家級進出口食品質量安全風險驗證評價實驗室(化妝品),廣東廣州 510623)
摘要:天然健康的化妝品受到越來越多消費者青睞和關注,但在化妝品中添加植物提取液卻存在農藥殘留的風險,因此,亟需建立化妝品中相應農藥殘留的檢測方法。建立了同時測定化妝品中除草醚和吡氟禾草靈殘留量的氣相色譜-質譜法。樣品采用乙腈水溶液超聲提取、增強型脂質去除(Enhanced matrix removal-lipid dispersion,EMR-Lipid)固相萃取柱凈化、經HP-5MS毛細管柱(30.0 m×0.25 mm×0.25 μm)分離,在多反應監測(MRM)模式下檢測,采用基質匹配標準曲線、外標法定量。結果表明,除草醚在0.020~0.500 mg/L范圍內線性關系良好,線性相關系數(r2)≥0.9936,檢出限0.020 mg/kg,定量限0.050 mg/kg;吡氟禾草靈在0.004~0.100 mg/L范圍內線性關系良好,r2≥0.9925,檢出限0.004 mg/kg,定量限0.010 mg/kg。在6種化妝品空白基質添加高、中、低3個濃度水平的除草醚和吡氟禾草靈,平均回收率分別為91.08%~109.68%和81.47%~109.87%,相對標準偏差(RSD,n=6)分別為0.50%~10.97%和0.30%~9.41%。采用該方法對30個化妝品實際樣品進行檢測,結果均未檢出除草醚和吡氟禾草靈。該方法適用性廣、準確性高、靈敏度高,為化妝品中除草醚和吡氟禾草靈的篩查監測和風險評估提供了方法支撐。
關鍵詞:氣相色譜-質譜法;除草醚;吡氟禾草靈;化妝品;農藥殘留
中圖分類號:O65-分析化學 文獻標識碼:A 文章編號:
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