2026年48(5)中英文摘要
【特約專稿】
海水電解中催化劑抗氯離子腐蝕性能研究進(jìn)展
鄧愷元1,2a,劉柯2a,3,雷蕾2b,黎挺挺*1,汪德高*2c,3
(1. 寧波大學(xué)材料科學(xué)與化學(xué)工程學(xué)院,浙江寧波 315211;2. 中國科學(xué)院寧波材料技術(shù)與工程研究所 a.浙江省數(shù)據(jù)驅(qū)動(dòng)高安全能源材料及應(yīng)用重點(diǎn)實(shí)驗(yàn)室,寧波市特種能源材料與化學(xué)重點(diǎn)實(shí)驗(yàn)室,先進(jìn)核能材料實(shí)驗(yàn)室,b.浙江省生物基高分子材料重點(diǎn)實(shí)驗(yàn)室,高分子與復(fù)合材料實(shí)驗(yàn)室,c.前沿交叉科學(xué)研究中心,浙江 寧波 315201;3. 中國科學(xué)院大學(xué),北京 101408)
摘要:海水電解在不加劇淡水資源壓力的前提下為大規(guī)模綠色制氫提供了一條低成本的清潔能源轉(zhuǎn)換途徑。但海水中高濃度氯離子(~0.5 mol/L)引發(fā)的陽極腐蝕、析氯競爭及催化劑失活等問題,大幅降低電解效率、縮短設(shè)備壽命,嚴(yán)重制約其工業(yè)化應(yīng)用。現(xiàn)有文獻(xiàn)多聚焦催化劑分類或單一抗腐蝕策略的探討,缺乏對氯離子侵蝕動(dòng)態(tài)機(jī)制的系統(tǒng)解析,且忽視催化劑設(shè)計(jì)與電解體系的全鏈條適配性。系統(tǒng)闡述了海水電解核心科學(xué)矛盾及熱力學(xué)競爭本質(zhì),重點(diǎn)分析了氯離子腐蝕與鈣鎂離子沉積兩大挑戰(zhàn),深入揭示了氯離子對活性位點(diǎn)的毒化作用、晶格結(jié)構(gòu)的破壞及金屬腐蝕溶出3種侵蝕路徑。基于氯離子腐蝕的干預(yù)機(jī)制及作用靶點(diǎn),創(chuàng)新性地將抗腐蝕催化劑設(shè)計(jì)范式劃分為主動(dòng)調(diào)控、被動(dòng)防御及全體系適配3大類別,結(jié)合原位表征與理論計(jì)算闡明其抗腐蝕機(jī)理。最后,比較了模擬海水與真實(shí)海水體系性能差異,展望催化劑發(fā)展方向,為其定向設(shè)計(jì)及其工業(yè)化應(yīng)用提供理論基礎(chǔ)與技術(shù)支撐。
關(guān)鍵詞:電解海水;電催化劑;氯離子腐蝕;動(dòng)態(tài)吸附調(diào)控;表面屏蔽
中圖分類號:O64 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0046
Progress in Chloride Corrosion Resistance of Catalysts for Seawater Electrolysis DENG Kai-yuan1,2a, LIU Ke2a,3, LEI Lei2b, LI Ting-ting*1, WANG De-gao*2c,3 (1. School of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China; 2a.Zhejiang Key Laboratory of Data-Driven High-Safety Energy Materials and Applications, Ningbo Key Laboratory of Special Energy Materials and Chemistry, Laboratory of Advanced Nuclear Materials, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China, 2b.Key Laboratory of Biobased Polymeric Materials of Zhejiang Province, Laboratory of Polymers and Composites, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China, 2c.Advanced Interdisciplinary Sciences Research (AIR) Center, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences (CAS), Ningbo, Zhejiang 315201, China; 3. University of Chinese Academy of Sciences, Beijing 101408)
Abstract:Seawater electrolysis is a cost-effective and environmentally sustainable approach for large-scale green hydrogen production that reduces reliance on freshwater resources. However, challenges such as anode corrosion, competitive chlorine evolution, and catalyst deactivation―primarily caused by the high chloride ion concentration (~0.5 mol/L) in seawater―substantially reduce electrolysis efficiency, shorten equipment lifetime, and limit industrial deployment. Existing studies have predominantly focused on classifying catalyst types or exploring isolated anticorrosion strategies, with limited comprehensive analysis of the dynamic mechanisms underlying chloride ion?induced degradation and insufficient attention to the integrative compatibility between catalyst design and the overall electrolysis system. This review examines the fundamental scientific challenges and thermodynamic competition in seawater electrolysis, with particular emphasis on the dual challenges of chloride ion corrosion and calcium?magnesium ion deposition. It further delineates three principal chloride ion?induced degradation pathways: active-site poisoning, lattice structure disruption, and metal corrosion coupled with dissolution. Based on the mechanisms and targets of chloride ion corrosion, an innovative anticorrosion catalyst design framework is proposed, including three categories: active regulation, passive defense, and holistic system adaptation. The anticorrosion mechanisms are systematically elucidated by integrating in situ characterization techniques with theoretical modeling. Finally, this review compares the performance of simulated and real seawater systems, outlines future directions for catalyst development, and provides a theoretical foundation and technical guidance for the targeted design and industrial application of seawater electrolysis catalysts.
Key words:seawater electrolysis; electrocatalyst; chloride ion corrosion; dynamic adsorption regulation; surface shielding
【綜述與專論】
小檗堿及其衍生物抗菌作用研究進(jìn)展
尹靈,劉慶漢,廖向文*,王金濤*
(江西科技師范大學(xué) ,江西 南昌 330013)
摘要:全球多重耐藥菌廣泛傳播,抗生素耐藥危機(jī)加劇,傳統(tǒng)抗菌藥物療效下降與新型藥物研發(fā)不足,推動(dòng)天然抗菌活性物質(zhì)成為研究熱點(diǎn)。小檗堿是黃連等傳統(tǒng)中藥的主要異喹啉類生物堿,具有低毒性、低致突變性、多靶點(diǎn)作用及低耐藥誘導(dǎo)風(fēng)險(xiǎn),在抗感染領(lǐng)域展現(xiàn)出重要應(yīng)用前景。系統(tǒng)闡述小檗堿的理化特性與廣譜藥理活性,重點(diǎn)總結(jié)其六大抗菌機(jī)制。綜述小檗堿對金黃色葡萄球菌、糞腸球菌、艱難梭菌等革蘭氏陽性菌,以及大腸桿菌、銅綠假單胞菌、肺炎克雷伯菌、鮑曼不動(dòng)桿菌、幽門螺桿菌等革蘭氏陰性菌的抑制作用,尤其對多重耐藥菌株仍保持良好活性,結(jié)構(gòu)修飾衍生物可顯著提升抗菌效果。同時(shí),小檗堿作為天然外排泵抑制劑,與多種抗生素聯(lián)用呈現(xiàn)協(xié)同增效作用,可逆轉(zhuǎn)細(xì)菌耐藥;對白色念珠菌、新生隱球菌等真菌亦具有廣譜抑制活性。盡管小檗堿存在水溶性差、生物利用度低等瓶頸,新型制劑遞送策略已有效改善其應(yīng)用局限。為小檗堿及其衍生物在抗多重耐藥菌領(lǐng)域的研究與臨床轉(zhuǎn)化提供參考,為應(yīng)對全球抗菌藥物耐藥危機(jī)提供中醫(yī)藥思路。
關(guān)鍵詞:小檗堿;抗菌;抗菌機(jī)制;協(xié)同作用;多重耐藥菌
中圖分類號:O62 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0052
Research Progress on the Antibacterial Effects of Berberine and Its Derivatives YIN Ling, LIU Qing-han, LIAO Xiang-wen*, WANG Jin-tao* (Jiangxi Science and Technology Normal University, Nanchang 330013, China)
Abstract: The widespread dissemination of multidrug-resistant bacteria worldwide has exacerbated the antibiotic resistance crisis. The diminished efficacy of conventional antibacterial agents and insufficient development of novel drugs have driven intensive research on natural antimicrobial active substances. Berberine, a major isoquinoline alkaloid derived from traditional Chinese medicines such as Coptis chinensis Franch., exhibits low toxicity, low mutagenicity, multi-target effects, and low risk of inducing drug resistance, showing promising application prospects in the field of anti-infective therapy. This study systematically elaborated on the physicochemical properties and broad-spectrum pharmacological activities of berberine, focusing on its six major antibacterial mechanisms. It reviews the inhibitory effects of berberine on gram-positive bacteria, including Staphylococcus aureus, Enterococcus faecalis and Clostridioides difficile, and on gram-negative bacteria, such as Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumoniae, Acinetobacter baumannii, and Helicobacter pylori. Notably, berberine retains favorable activity against multidrug-resistant strains, and its structurally modified derivatives can significantly enhance its antibacterial efficacy. Furthermore, as a natural efflux pump inhibitor, berberine exerts synergistic effects when combined with various antibiotics and can reverse bacterial resistance. It also exhibits broad-spectrum inhibitory activity against fungi, including Candida albicans and Cryptococcus neoformans. Despite limitations, such as poor water solubility and low bioavailability, novel formulation and delivery strategies have effectively improved its application constraints. This review provides a reference for the research and clinical translation of berberine and its derivatives in combating multidrug-resistant bacteria, and offers insights from traditional Chinese medicine to address the global antibiotic resistance crisis.
Key words:berberine; antibacterial; antibacterial mechanism; synergistic effect; multidrug-resistant bacteria
香豆素類藥物藥理活性研究進(jìn)展
劉帝1, 萬明濤2, 路文濤3, 王丹3, 葉文強(qiáng)4, 門靖*5,6
(1. 陜西省漢中市漢臺(tái)區(qū)市場監(jiān)督管理局漢中路所,陜西 漢中 723000;2. 陜西省漢中市漢臺(tái)區(qū)市場監(jiān)督管理局鋪鎮(zhèn)所 陜西 漢中 723007;3. 陜西省藥品和疫苗檢查中心,陜西西安 710077;4. 陜西中醫(yī)藥大學(xué)藥學(xué)院,陜西咸陽 712046;5.陜西共裕康宸醫(yī)藥科技有限公司,陜西西安 710086;6. 陜西科技大學(xué) 化學(xué)與化工學(xué)院,陜西 西安 710021)
摘要:香豆素類化合物是由苯并α-吡喃酮環(huán)稠合成的次級代謝產(chǎn)物,屬于鄰羥基肉桂酸內(nèi)酯類化合物,廣泛存在于自然界中。香豆素類化合物因具有豐富的藥理活性及治療多種疾病的潛力而備受關(guān)注,其藥理活性及應(yīng)用是天然產(chǎn)物、新藥開發(fā)、大健康領(lǐng)域的研究熱點(diǎn)。香豆素類化合物常作為優(yōu)勢結(jié)構(gòu)被應(yīng)用于藥物設(shè)計(jì)和新藥開發(fā)領(lǐng)域。多年來,研究人員進(jìn)行了深入研究,將吡喃基、倍半萜烯基、烷基胺、硝基、芳烴基、哌嗪基、丙烯酸酯基、三氟甲基等多種化學(xué)基團(tuán)引入香豆素母環(huán)結(jié)構(gòu)中,并有多種香豆素類藥物已被成功應(yīng)用于疾病的治療。香豆素類藥物的開發(fā)與應(yīng)用已成為抗菌、抗腫瘤領(lǐng)域新藥開發(fā)和天然產(chǎn)物研究的重要方向,展現(xiàn)出豐富的藥理活性和較高的臨床價(jià)值。基于藥渡數(shù)據(jù)庫和國內(nèi)外文獻(xiàn)的研究成果,對具有抗凝、抗菌、抗腫瘤等治療活性的香豆素類藥物研究進(jìn)展進(jìn)行綜述,并對其發(fā)展前景進(jìn)行展望,以期對香豆素類藥物的進(jìn)一步研發(fā)和應(yīng)用提供參考。
關(guān)鍵詞:香豆素;藥理活性;研究進(jìn)展;抗菌;抗腫瘤
中圖分類號:R284 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:0258-3283(2026)--
DOI:10.13822/j.cnki.hxsj.2026.0044
Research Progress in Molecular Activity of Coumarin-Related Drugs LIU Di1, WAN Ming-tao2, LU Wen-tao3, WANG Dan3, YE Wen-qiang4, MEN Jing5,6 (1. Market Supervision and Administration Bureau of Hantai District of Hanzhong Road, Hanzhong 723000, China; 2. Market Supervision and Administration Bureau of Hantai District of Puzhen, Hanzhong 723007, China; 3. Shaanxi Center for Drug and Vaccine Inspection, Xi’an 710077, China; 4. College of pharmacy, Shaanxi University of Chinese Medicine, Xianyang 712046, China; 5. Shaanxi Gongyu Kangchen Pharmaceutical Technology Co., Ltd, Xi’an 710086, China; 6. College of Chemistry and Chemical Engineering, Shaanxi University of Science and Technology, Xi’an 710021, China)
Abstract: Coumarin compounds are secondary metabolites formed by the fusion of a benzene ring and an α-pyrone ring, belonging to the class of ortho-hydroxycinnamic acid lactones, which are widely distributed in nature. Coumarins have attracted considerable attention owing to their rich pharmacological activity and potential for treating various diseases, with applications in natural products, drug design and development, and overall health. For many years, researchers have studied coumarins in depth, introducing various functional groups, such as pyran, sesquiterpene, alkylamine, nitro, aromatic, piperazine, acrylate, and trifluoromethyl groups, into their parent ring structure. Several coumarin drugs―particularly antibacterial and antitumor drugs―have been successfully used to treat various diseases, demonstrating their rich pharmacological activity and high clinical value. This review summarizes the research progress of coumarin drugs with therapeutic activities, including anticoagulation, antibacterial, and antitumor effects, based on drug databases and domestic and foreign literature. This study provides an outlook on the development prospects of coumarin drugs, aiming to provide a reference for further research, development, and application.
Key words:coumarin; pharmacological activity; research progress; antibacterial; antitumor
【生化與藥用試劑】
基于ST-6-2核酸適配體的顯色探針用于快速檢測新冠病毒S蛋白
王新研,朱鶴2,嘎魯*1,愛軍*2
(1. 內(nèi)蒙古醫(yī)科大學(xué)藥學(xué)院,內(nèi)蒙古呼和浩特 010110;2. 內(nèi)蒙古師范大學(xué) 化學(xué)與環(huán)境科學(xué)學(xué)院,內(nèi)蒙古 呼和浩特 010022)
摘要:基于ST-6-2核酸適配體與金納米顆粒(AuNPs),構(gòu)建了一種用于快速檢測新冠病毒S蛋白的比色生物傳感器。采用檸檬酸鈉還原氯金酸法制備粒徑均勻的AuNPs,通過圓二色光譜驗(yàn)證適配體與S蛋白的結(jié)合構(gòu)象變化。比較了冷凍-解凍法、鹽老化法和低pH法3種DNA與AuNPs的偶聯(lián)策略,以UV-Vis光譜評估偶聯(lián)效果,確定低pH法為最優(yōu)方案。將巰基修飾的cDNA和Poly T共價(jià)偶聯(lián)至AuNPs表面,制備顯色探針(AuNPs@SH-DNA)。基于競爭性側(cè)向流層析原理,組裝試紙條,用于S蛋白的可視化檢測。實(shí)驗(yàn)結(jié)果表明,該傳感器對S蛋白具有良好的信號響應(yīng),可實(shí)現(xiàn)快速、低成本、便攜式檢測。該比色傳感器平臺(tái)為新冠病毒的即時(shí)檢測提供了新方案,在疫情篩查和分散式診斷中具有應(yīng)用潛力。
關(guān)鍵詞:金納米顆粒;核酸適配體;新冠病毒S蛋白;比色傳感器;側(cè)向流層析
中圖分類號: O65 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0074
Colorimetric Probe Based on ST-6-2 Aptamer for Rapid Detection of SARS-CoV-2 Spike Protein WANG Xin-yan 1, ZHU He 2,GA Lu *1, AI Jun *2 (1. School of Pharmacy, Inner Mongolia Medical University, Hohhot 010110; 2. College of Chemistry and Environmental Science, Inner Mongolia Normal University, Hohhot 010022)
Abstract:A colorimetric biosensor based on ST-6-2 aptamer and gold nanoparticles (AuNPs) was developed for the rapid detection of the SARS-CoV-2 spike protein. AuNPs with uniform particle size were synthesized using the sodium-citrate reduction method, and the binding conformational change between the aptamer and the spike protein was verified via circular dichroism spectroscopy. Three conjugation strategies for the DNA functionalization of AuNPs, namely the freeze?thaw, salt-aging, and low-pH methods, were compared. The conjugation efficiency was evaluated based on UV-Vis absorption spectra, and the low-pH method was identified as the optimal strategy. A colorimetric probe (AuNPs@SH-DNA) was constructed by covalently coupling thiol-modified cDNA and Poly T to the surface of AuNPs. Based on the principle of competitive lateral-flow chromatography, a test strip was assembled for the visual detection of the spike protein. Experimental results show that the sensor exhibited favorable signal response toward the spike protein, thus enabling rapid, low-cost, and point-of-care detection. This colorimetric aptasensor platform provides a novel solution for the point-of-care testing of SARS-CoV-2 and demonstrates significant potential for epidemic screening and decentralized diagnostics.
Key words:gold nanoparticles; aptamer; SARS-CoV-2 spike protein; colorimetric sensor; lateral flow chromatography
【分離提取技術(shù)】
金丹附延顆粒揮發(fā)油包合工藝研究
朱良輝1,吳倩穎1,2,陳偉康*1,劉德鴻1,陳希1,繆貴忠3
(1. 江西省藥品檢驗(yàn)檢測研究院江西省藥品與醫(yī)療器械質(zhì)量工程技術(shù)研究中心,江西南昌 330029;2. 江西中醫(yī)藥大學(xué) 藥學(xué)院,江西 南昌 330004;3. 江西華太藥業(yè)有限公司,江西 宜豐 336300)
摘要:優(yōu)選金丹附延顆粒揮發(fā)油的飽和水溶液法環(huán)糊精包合制備工藝。在單因素考察的基礎(chǔ)上,以包合率、得率、載藥量的綜合評分為評價(jià)指標(biāo),采用響應(yīng)面法,對溫度、時(shí)間、轉(zhuǎn)速、β-環(huán)糊精與揮發(fā)油質(zhì)量體積比進(jìn)行考察。通過Design-Expert 13軟件分析各因素的交互作用優(yōu)選最佳工藝參數(shù)。利用4種表征實(shí)驗(yàn)(電子顯微鏡、薄層色譜圖、紅外光譜、紫外光譜)檢驗(yàn)包合物是否已成功形成。最佳的包合工藝參數(shù)為:實(shí)驗(yàn)溫度30 ℃、攪拌時(shí)間2.15 h,轉(zhuǎn)速1400 r/min,β-環(huán)糊精與揮發(fā)油質(zhì)量體積比6:1;響應(yīng)面結(jié)果P值<0.05,R2>0.9,表明該方案可行性高。轉(zhuǎn)速和β-環(huán)糊精與揮發(fā)油質(zhì)量體積比之間存在交互影響。4種表征實(shí)驗(yàn)從多維度驗(yàn)證了包合物與其他材料的區(qū)別,證實(shí)包合物已形成,表明該工藝穩(wěn)定可靠。優(yōu)化了金丹附延顆粒揮發(fā)油β-環(huán)糊精包合物的包合制備工藝,該方法穩(wěn)定可行,可為后續(xù)相關(guān)生產(chǎn)的研究和開發(fā)提供參考。
關(guān)鍵詞:金丹附延顆粒;揮發(fā)油;包合物;響應(yīng)面;飽和水溶液法
中圖分類號:R94 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0036
Research on the Volatile Oil Embedding Process of Jindan Fuyan Granules ZHU Liang-hui1,WU Qian-ying1,2 ,CHEN Wei-kang*1, LIU De-hong1, CHEN Xi1 ,MIAO Gui-zhong3(1. Jiangxi Provincial Institute of Drug Control, Jiangxi Province Engineering Technology Research Center for Drug and Medical Instrument Quality, Jiangxi 30029, China; 2. School of Pharmacy, Jiangxi University of Traditional Chinese Medicine, Nanchang 330004, China;3. Jiangxi Huatai Pharmaceutical Co., Ltd., Yifeng 336300, China)
Abstract: This study aimed to optimize the preparation process of a β-cyclodextrin (β-CD) inclusion complex containing the volatile oil from JinDan FuYan Granules via the saturated aqueous solution method. On the basis of single-factor experiments, response surface methodology (RSM) was employed to investigate the effects of the temperature, stirring time, stirring speed, and mass?volume ratio of β-CD to volatile oil, with the comprehensive score of the inclusion rate, yield, and drug loading capacity set as the evaluation index. Design-Expert 13 software was applied to analyze the interactions of various factors and optimize the process parameters. Four characterization experiments, including scanning electron microscopy, thin-layer chromatography, Fourier transform infrared spectroscopy, and ultraviolet?visible spectroscopy, were performed to verify the successful formation of the inclusion complex. The optimal inclusion process parameters were determined as follows: experimental temperature of 30 ℃, stirring time of 2.15 h, stirring speed of 1400 r/min, and mass?volume ratio of β-CD to volatile oil of 6:1. The P-value of the RSM model was less than 0.05, and the coefficient of determination (R2) was greater than 0.9, indicating favorable fitting performance and high feasibility of the established model. A significant interaction was detected between the stirring speed and the mass?volume ratio of β-CD to volatile oil. The four characterization experiments verified the differences between the inclusion complex and raw materials from multiple dimensions, confirmed the successful formation of the inclusion complex, and proved the stability and reliability of the optimized process. This study optimizes the preparation process of a β-CD inclusion complex containing volatile oil from JinDan FuYan Granules. The established method is stable and feasible, and can provide insights for subsequent research and development of related industrial production.
Key words: Jindan Fuyan granules; volatile oil; inclusion complex; response surface methodology: saturated aqueous solution method
【化學(xué)品與環(huán)境】
基于傅里葉變換紅外氣體分析儀的零氣發(fā)生器檢測方法研究
呂利*,夏春,李劍,程麗萍,王海燕,楊倩,王國娟
(青島市計(jì)量技術(shù)研究院,山東 青島 266101)
摘要:零氣發(fā)生器性能能否滿足標(biāo)準(zhǔn)要求,直接影響后續(xù)分析結(jié)果的準(zhǔn)確性。為了檢測零氣發(fā)生器性能符合國家標(biāo)準(zhǔn)GB18285-2018要求,設(shè)計(jì)了一種使用傅里葉變換紅外氣體分析儀檢測零氣發(fā)生器性能的方法。通過動(dòng)態(tài)稀釋法將不同種類的國家有證標(biāo)準(zhǔn)氣體稀釋到國標(biāo)要求的檢測用特定濃度值,文中稱其為“參考標(biāo)準(zhǔn)氣體”。傅里葉變換紅外氣體分析儀測量參考標(biāo)準(zhǔn)氣體的響應(yīng)值,并考察分析儀對不同參考標(biāo)準(zhǔn)氣體的檢出限。依次將國家有證標(biāo)準(zhǔn)氣體先后輸入A、B、C 3個(gè)廠家零氣發(fā)生器,輸出氣體使用傅里葉變換紅外氣體分析儀測量響應(yīng)值,并與參考標(biāo)準(zhǔn)氣體的響應(yīng)值做除法。結(jié)果表明,3個(gè)廠家零氣發(fā)生器都能滿足國標(biāo)的要求,該方法在零氣發(fā)生器校準(zhǔn)檢測中的良好應(yīng)用表現(xiàn),提高了零氣發(fā)生器檢測效率和可靠性,為零氣質(zhì)量檢測提供重要參考。
關(guān)鍵詞:零氣發(fā)生器;標(biāo)準(zhǔn)物質(zhì);傅里葉變換紅外氣體分析儀;動(dòng)態(tài)稀釋法;檢出限
中圖分類號:O65 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:0258-3283(2026)--
DOI:10.13822/j.cnki.hxsj.2026.0009
Research on the Detection Method for Zero-Gas Generator Based on Fourier-Transform Infrared Gas Analyzer LV Li*, XIA Chun, LI Jian, CHENG Li-ping, WANG Hai-yan, YANG Qian,WANG Guo-juan (Qingdao Institute of Measurement Technology, Qingdao, 266101, China)
Abstract:The performance of a zero-gas generator directly affects the accuracy of the subsequent analysis results. To determine whether the performance meets the requirements of the national standard GB18285-2018, a detection method incorporating a Fourier-transform infrared (FTIR) gas analyzer was designed. Various nationally certified standard gases were dynamically diluted to the specific concentrations required by the national standard for detection, which are referred to as “reference standard gases” in the text. The FTIR gas analyzer measured the responses of the reference standard gases, and the detection limits of the analyzer were determined for various reference standard gases. National certified standard gases were successively input into zero-gas generators from three different manufacturers: A, B, and C. The responses of the output gases were measured using the FTIR gas analyzer and then divided by the responses of the reference standard gases. The results showed that the zero-gas generators from all three manufacturers met the requirements of the national standard. The robust performance of this method for the calibration and assessment of detection capability of zero-gas generators improves their detection efficiency and reliability, providing an important reference for the quality detection of zero gas.
Key words:zero air generator; reference material; FTIR spectroscopy; dynamic dilution method; detection limit
【分析與測試】
磁性復(fù)合材料的制備及其在水中多氯聯(lián)苯測定中的應(yīng)用
王福德,張文舒*2
(1.山東省沂水縣檢驗(yàn)檢測中心,山東臨沂 276400;2.合肥綜合性科學(xué)中心環(huán)境研究院,安徽 合肥 231299)
摘要:通過將聚多巴胺(PDA)包覆在磁性材料表面合成磁性復(fù)合材料NiFe2O4/SiO2@PDA,建立了一種磁固相萃取-氣質(zhì)聯(lián)用快速測定水中18種PCBs的方法。稱取0.05 g NiFe2O4/SiO2@PDA萃取劑,加入裝有15.0 mL樣品中(已調(diào)節(jié)樣品pH 3.0),加入1.0 μL替代物標(biāo)液,渦旋提取1.5 min,磁鐵分離后傾出溶液,加入1.0 mL V(二氯甲烷):V(丙酮) = 1:1混合溶液,渦旋解吸2 min,磁鐵分離后將溶液裝入色譜小瓶中,至氣質(zhì)聯(lián)用儀進(jìn)行測定。方法學(xué)驗(yàn)證結(jié)果:18種PCBs的方法檢出限為0.03~0.1 μg/L,相關(guān)系數(shù) r ≥ 0.9995;對實(shí)際廢水樣品進(jìn)行兩個(gè)質(zhì)量濃度(3.33、13.3μg/L)的加標(biāo)分析,加標(biāo)回收率范圍分別為91.8%~105%和92.8%~105%,相對標(biāo)準(zhǔn)偏差范圍分別為1.7%~4.4%和1.6%~3.9%(n = 6);磁性復(fù)合材料重復(fù)萃取6次后,目標(biāo)物回收率93.1%~103%。該方法操作簡單、快速、準(zhǔn)確、可循環(huán),可應(yīng)用于水中18種PCBs的測定。
關(guān)鍵詞:多氯聯(lián)苯;氣質(zhì)聯(lián)用儀;磁固相萃取;廢水;聚多巴胺
中圖分類號:O657 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0014
Preparation of Magnetic Composite Materials and Its Application in the Determination of PCBs in Water WANG Fu-de1,ZHANG Wen-shu*2 (1.Yishui County Inspection and Testing Center,Linyi 276400, China;2. Institute of Environment Hefei Comprehensive Science Center, Hefei 231299, China)
Abstract:A magnetic composite material, NiFe2O4/SiO2@PDA, was synthesized by coating the surface of a magnetic material with polydopamine (PDA). A method for the rapid determination of 18 PCBs in water using magnetic solid-phase extraction coupled with gas chromatography-mass spectrometry (MSPE-GC-MS) was established. NiFe?O?/SiO?@PDA extractant (0.05 g) was added to water (15 mL; the pH of the sample was adjusted to 3.0), and a surrogate standard solution (1.0 μL) was added. The mixture was extracted by vortexing for 1.5 min, separated with a magnet, and the supernatant was decanted. Subsequently, 1.0 mL of dichloromethane:acetone (1:1 v/v) was added, followed by vortex desorption for 2 min and a second separation with a magnet. The solution was transferred to a chromatographic vial and injected into a gas chromatography?mass spectrometer for determination. The method validation results are as follows: the method detection limits (MDLs) for the 18 PCBs ranged from 0.03 to 0.1 μg/L, with correlation coefficients (r) ≥ 0.9995. Spiked recovery tests were performed on actual wastewater samples at two concentrations (3.33 and 13.3 μg/L). The spiked recoveries ranged from 91.8% to 105% and 92.8% to 105%, respectively, with relative standard deviations (RSDs) of 1.7?4.4% and 1.6?3.9% (n = 6). After six repeated extractions using the magnetic composite material, the recoveries of the target analytes remained in the range of 93.1%~103%. This method is simple, rapid, accurate, recyclable, and can be applied to the determination of 18 PCBs in water.
Keywords:PCBs;GCMS;MSPE;wastewater;PDA
2023-2025年蕪湖市市售果蔬中30種農(nóng)藥殘留污染狀況調(diào)查與分析
陶媛*,胡美紅,張菁,李勇競
(蕪湖市疾病預(yù)防控制中心,安徽蕪湖 241000)
摘要:分析近3年蕪湖市市售水果、蔬菜中30種農(nóng)藥殘留量,評估經(jīng)果蔬途徑攝入農(nóng)藥的健康風(fēng)險(xiǎn)。參照食品安全風(fēng)險(xiǎn)監(jiān)測方案,分別抽取蕪湖市2023、2024和2025年市售蔬果類食品,共111份樣品,參考2023、2024及2025年《國家食品污染物和有害因素風(fēng)險(xiǎn)監(jiān)測工作手冊》的檢測方法。對樣品中噻蟲胺等30種農(nóng)藥含量進(jìn)行檢測,并采用風(fēng)險(xiǎn)商值HQ及累計(jì)暴露危害指數(shù)法HI對檢出的農(nóng)藥殘留進(jìn)行膳食暴露風(fēng)險(xiǎn)評估,評價(jià)因膳食攝入對人體健康的風(fēng)險(xiǎn)。111份果蔬樣品中,檢出有農(nóng)藥殘留的樣品為74份,檢出率為66.7%(74/111),其中2023年樣本數(shù)為41份,檢出率為70.7%(29/41);2024年樣本數(shù)為30份,檢出率為70.0%(21/30);2025年樣本數(shù)為40份,檢出率為60.0%(24/40)。近3年監(jiān)測的樣品中,超標(biāo)7份,超標(biāo)率為6.31%(7/111)。8大類蔬菜和5大類水果樣品農(nóng)藥殘留,檢出率前三的是鮮豆類(100%),柑橘類(100%),葉菜類(88.9%);超標(biāo)率前三的是根莖類(33.3%),鮮豆類(25.0%),鱗莖類和蕓薹類(20.0%)。此外,部分樣品存在多種農(nóng)藥殘留現(xiàn)象。111份果蔬樣品中,有50份檢出兩種或兩種以上農(nóng)藥殘留,多殘留率為45.0%(50/111)。以暴露濃度最大值計(jì)算蔬菜中HQ,范圍為0~2.59,以暴露濃度平均值計(jì)算蔬菜中HQ,范圍為0~0.0378,HI為0.090。以暴露濃度最大值計(jì)算水果中HQ,范圍為0~0.138, 以暴露濃度平均值計(jì)算水果中HQ,范圍為0~0.0073,HI為0.013。2023~2025年蕪湖市市售果蔬農(nóng)藥殘留總體上污染程度較輕,3年檢出率呈下降趨勢,但少數(shù)樣品存在一定健康風(fēng)險(xiǎn)。
關(guān)鍵詞:果蔬;農(nóng)藥殘留;食品安全;健康風(fēng)險(xiǎn);結(jié)果分析
中圖分類號:O65 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:0258-3283(2026)--
DOI: 10.13822/j.cnki.hxsj.2026.0010
Investigation of the Pollution Status of 30 Pesticide Residues in Fruits and Vegetables Sold in Wuhu City from 2023 to 2025 TAO Yuan*, Hu Mei-hong, ZHANG Jing, Li Yong-jing (Wuhu Center for Disease Control and Prevention,Wuhu 241000, China)
Abstract: This study analyzed the levels of 30 pesticide residues in fruits and vegetables sold in Wuhu City over the past three years and assessed the health risks associated with pesticide intake through the consumption of these foods. A total of 111 samples of fruits and vegetables sold in Wuhu City from 2023 to 2025 were collected. The detection method refers to the 2023, 2024, and 2025 National Food Contaminants and Harmful Factors Risk Monitoring Work Manual. The levels of 30 pesticides, including clothianidin, were analyzed in the samples, and the Health Quotient (HQ) and Hazard Index (HI) methods were employed to assess dietary exposure risks and evaluate the risks to human health due to dietary intake. Among the 111 fruit and vegetable samples, 74 contained pesticide residues, with a detection rate of 66.7% (74/111). Specifically, 41 samples from 2023 had a pesticide detection rate of 70.7% (29/41); 30 samples from 2024 had a pesticide detection rate of 70.0% (21/30); and 40 samples from 2025 had a pesticide detection rate of 60.0% (24/40). Among the samples monitored over the past three years, seven exceeded the allowable limits, representing an over-limit rate of 6.31% (7/111). In terms of pesticide residues in the eight major categories of vegetables and five major categories of fruits, the top three categories in terms of detection rate were fresh beans (100%), citrus fruits (100%), and leafy vegetables (88.9%); the top three categories in terms of over-limit rate were root vegetables (33.3%), fresh beans (25.0%), and bulbous and brassica vegetables (20.0%). In addition, some samples contained multiple pesticide residues. Among the 111 fruit and vegetable samples, 50 contained two or more types of pesticide residues, with a multiresidue rate of 45.0% (50/111). When calculated based on the maximum exposure concentration and average exposure concentration in vegetables, the HQ ranged from 0 to 2.59 and from 0 to 0.0378 (with an HI of 0.090), respectively. When the HQ in fruits was calculated based on the maximum exposure concentration and average exposure concentration, the range was 0?0.138 and 0?0.0073 (with an HI of 0.013), respectively. Overall, the pollution levels of pesticide residues in fruits and vegetables sold in Wuhu City from 2023 to 2025 were relatively low. The detection rate showed a downward trend over the three year period, but a few samples indicated health risks.
Keywords: fruits and vegetables; pesticide residues; food safety; health risks; result analysis
基于ATR-FTIR法快速鑒別亳州產(chǎn)菊花品種
榮百玲,范成龍1,朱倩1,陳寅1,卓園園1,崔雪嬌2,張小倩2,徐倩3,胡云飛*2
(1. 江蘇省人民醫(yī)院宿遷醫(yī)院,江蘇宿遷 223800;2.亳州學(xué)院 安徽省現(xiàn)代中藥產(chǎn)業(yè)共性技術(shù)研究中心,安徽 亳州 236800;3.安徽中醫(yī)藥大學(xué)第二附屬醫(yī)院,安徽 合肥 230061)
摘要:為建立一種快速、準(zhǔn)確的亳州菊花品種鑒別方法,本研究采用衰減全反射傅立葉變換紅外光譜(ATR-FTIR)結(jié)合化學(xué)計(jì)量學(xué)方法,對11個(gè)不同品種的亳州菊花樣品進(jìn)行分析。首先采集各樣品的ATR-FTIR光譜信息,并對原始光譜數(shù)據(jù)進(jìn)行多種預(yù)處理和變量篩選,以降低噪聲干擾、增強(qiáng)光譜特征并提高模型的分類能力。在此基礎(chǔ)上,采用正交偏最小二乘判別分析(OPLS-DA)對不同品種菊花樣品進(jìn)行分類識(shí)別,考察其在模式識(shí)別中的應(yīng)用效果。ATR-FTIR光譜能夠較好地反映不同品種亳州菊花樣品的化學(xué)組成差異,結(jié)合化學(xué)計(jì)量學(xué)分析可實(shí)現(xiàn)對不同品種樣品的快速分類與有效鑒別。OPLS-DA結(jié)果顯示,不同品種菊花樣品之間具有較為清晰的聚類趨勢,能夠較直觀地反映各品種間的差異。通過對多種光譜預(yù)處理方法及變量選擇方法的比較與評估,確定MSC結(jié)合2nd D為最優(yōu)預(yù)處理方法。進(jìn)一步采用支持向量機(jī)(SVM)建立分類預(yù)測模型。結(jié)果顯示,SVM模型具有優(yōu)異的分類性能和較高的預(yù)測精度,訓(xùn)練集準(zhǔn)確率達(dá)到100%,測試集準(zhǔn)確率為98.2%,表明所建立模型具有良好的識(shí)別能力和泛化性能。研究結(jié)果說明,ATR-FTIR結(jié)合化學(xué)計(jì)量學(xué)方法能夠有效區(qū)分不同品種的亳州菊花。與傳統(tǒng)鑒別方法相比,該方法具有操作簡便、分析快速、效率高及結(jié)果準(zhǔn)確可靠等優(yōu)點(diǎn),可為亳州菊花品種鑒別及質(zhì)量評價(jià)提供新的技術(shù)手段和理論依據(jù)。
關(guān)鍵詞:菊花;ATR-FTIR;化學(xué)計(jì)量學(xué);品種鑒別;質(zhì)量評價(jià)
中圖分類號:O657.3 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0058
Rapid Identification of Chrysanthemum Varieties Produced in Bozhou Based on ATR-FTIR Method RONG Bai-ling1, FAN Cheng-long1, ZHU Qian1, CHEN Yin1, ZHUO Yuan-yuan1, CUI Xue-jiao2, Zhang Xiao-qian2, XU Qian3, HU Yun-fei *2(1. Suqian Hospital of Jiangsu Provincial People's Hospital, Suqian 223800, China; 2. Anhui Provincial Research Center for Common Technologies of Modern Chinese Medicine Industry, Bozhou University, Bozhou 236800, China; 3. The Second Affiliated Hospital of Anhui University of Chinese Medicine, Hefei 230061, China)
Abstract:To establish a rapid and accurate method for the identification of chrysanthemum varieties in Bozhou, we analyzed 11 varieties of Chrysanthemum morifolium Ramat. from Bozhou by combining attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy with chemometric methods. First, ATR-FTIR spectral information was collected from all the samples, and the raw spectral data were subjected to multiple preprocessing methods and variable selection to reduce noise interference, enhance the spectral features, and improve the classification ability of the model. Orthogonal partial least squares discriminant analysis (OPLS-DA) was used to classify and identify samples of different chrysanthemum varieties, and its application in pattern recognition was evaluated. The ATR-FTIR spectra reflected the differences in the chemical composition among the different varieties of Chrysanthemum morifolium Ramat. from Bozhou. When combined with chemometric analysis, this method enabled the rapid classification and effective discrimination of different varieties. The OPLS-DA results showed a relatively clear clustering trend among samples from different varieties and visually reflected the differences among the varieties. By comparing and evaluating the various spectral preprocessing and variable selection methods, multiplicative scatter correction combined with second derivative (2nd D) was determined to be the optimal preprocessing method. Furthermore, a support vector machine (SVM) model was established for classification and prediction. The results showed that the SVM model exhibited excellent classification performance and high predictive accuracy, with an accuracy of 100% for the training set and 98.2% for the test set, indicating that the established model possessed good recognition ability and generalization performance. These findings demonstrate that ATR-FTIR combined with chemometric methods can effectively distinguish different varieties of Chrysanthemum morifolium Ramat. from Bozhou. Compared with traditional identification methods, this method has the advantages of simple operation, rapid analysis, high efficiency, and accurate and reliable results. Therefore, this study provides a new technical method and theoretical basis for the identification of chrysanthemum varieties and quality evaluation of Chrysanthemum morifolium Ramat. from Bozhou.
Key words:Chrysanthemum morifolium; ATR-FTIR; chemometrics; variety identification; quality evaluation
基于新型SPME/GC×GC-QTOF-MS技術(shù)檢測4種食源性致病菌揮發(fā)性代謝物
黃寶華1,2,方舒婷2,3,黃毅權(quán)2,陳智勇2,劉舒芹*3,周志*1
(1. 廣州醫(yī)科大學(xué) 藥學(xué)院,廣東 廣州 511436;2. 廣東省科學(xué)院測試分析研究所(中國廣州分析測試中心),廣東 廣州 510070;3. 暨南大學(xué) 環(huán)境與氣候?qū)W院,廣東 廣州 511443)
摘要:致病菌誘發(fā)的食源性疾病嚴(yán)重威脅食品安全,因此,亟需開發(fā)便捷且有效的食品病原體識(shí)別方法。近年來,隨著代謝組學(xué)技術(shù)的成熟和微生物揮發(fā)性代謝產(chǎn)物數(shù)據(jù)庫的完善,揮發(fā)性代謝產(chǎn)物分析已成為食品和臨床中致病菌鑒別的重要替代方法。因此,為實(shí)現(xiàn)食源性致病菌的快速、無損識(shí)別,將固相微萃取(Solid-phase microextraction,SPME)技術(shù)與全二維氣相色譜四極桿飛行時(shí)間質(zhì)譜(Comprehensive two-dimensional gas chromatography quadrupole time-of-flight mass spectrometry,GC×GC-QTOF-MS)技術(shù)耦合,構(gòu)建了一種基于細(xì)菌揮發(fā)性代謝物指紋的原位檢測策略。采用新型自制SPME探針,對蠟樣芽孢桿菌、乙型溶血性鏈球菌、痢疾桿菌和阪崎腸桿菌培養(yǎng)體系中釋放的揮發(fā)性代謝物進(jìn)行高覆蓋捕獲與分析,成功鑒定出107種微生物揮發(fā)性有機(jī)化合物。進(jìn)一步的多變量統(tǒng)計(jì)分析表明,不同致病菌的響應(yīng)揮發(fā)性代謝特征明顯分離,并篩選出21種潛在的差異性揮發(fā)性代謝物,其中在蠟樣芽孢桿菌、乙型溶血性鏈球菌、痢疾桿菌和阪崎腸桿菌分別篩選出5、5、7和4種。隨后的食品樣品驗(yàn)證結(jié)果顯示,吲哚可作為阪崎腸桿菌的特征性揮發(fā)性標(biāo)志物,在乳制品基質(zhì)中仍能夠被穩(wěn)定檢出。總體而言,基于微生物揮發(fā)性代謝指紋的分析方法在食源性致病菌快速識(shí)別中具有一定應(yīng)用潛力,可為食品安全檢測和風(fēng)險(xiǎn)防控提供技術(shù)參考。
關(guān)鍵詞:食源性致病菌;微生物揮發(fā)性有機(jī)化合物;代謝組學(xué);固相微萃取;全二維氣相色譜-質(zhì)譜;多變量統(tǒng)計(jì)分析
中圖分類號:O657 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:0258-3283(2026)--
DOI:10.13822/j.cnki.hxsj.2026.0056
Detection of Volatile Metabolites in Four Foodborne Pathogens Using a Novel SPME/GC×GC-QTOF-MS Strategy HUANG Bao-hua1,2, FANG Shu-ting2,3, HUANG Yi-quan2, CHEN Zhi-yong2, LIU Shu-qin*,3, ZHOU Zhi*,1 (1. School of Pharmaceutical Sciences, Guangzhou Medical University, Guangzhou 511436, China; 2. Guangdong Academy of Sciences Institute of Testing and Analysis ( China National Analytical Center), Guangzhou 510070, China; 3. College of Environment and Climate, Jinan University, Guangzhou 511443, China)
Abstract: Foodborne diseases caused by pathogenic bacteria pose a serious threat to food safety, creating an urgent need for convenient and effective pathogen detection methods. With the maturation of metabolomics technology and limitations in existing microbial volatile metabolite databases, the analysis of foodborne pathogen volatile metabolites has emerged as a promising alternative for pathogen identification in both food and clinical settings. To enable rapid, non-destructive identification of foodborne pathogenic bacteria, a volatile metabolite fingerprint?based in situ detection strategy was developed by coupling solid-phase microextraction (SPME) with comprehensive two-dimensional gas chromatography?quadrupole time-of-flight mass spectrometry (GC×GC?QTOF-MS). A novel self-fabricated SPME probe was employed to achieve high-coverage capture and efficient enrichment of microbial volatile metabolites released by Bacillus cereus, Streptococcus pyogenes, Shigella, and Enterobacter sakazakii, resulting in the identification of 107 microbial volatile organic compounds. Multivariate statistical analysis revealed significant separation of volatile metabolic features among the different pathogenic bacteria. A total of 21 potential differential volatile metabolites were identified, comprising 5, 5, 7, and 4 metabolites from B. cereus, S. pyogenes, Shigella, and E. sakazakii, respectively. Subsequent validation in food samples demonstrated that indole could serve as a characteristic volatile marker for E. sakazakii and remained detectable in dairy matrices. These results indicate that volatile metabolite fingerprint analysis has potential for rapid identification of foodborne pathogens and may provide a valuable reference for food safety monitoring.
Key words: foodborne pathogenic bacteria; microbial volatile organic compounds; metabolomics; solid phase microextraction; comprehensive two-dimensional gas chromatography-mass spectrometry; multivariate statistical analysis
【標(biāo)準(zhǔn)物質(zhì)與標(biāo)準(zhǔn)品】
乙二胺四乙酸二鈉標(biāo)準(zhǔn)滴定溶液濃度測量方法的對比研究
鄭琦,曹曉蓉,張永吉*,郁家駿*,白倩
(國藥集團(tuán)化學(xué)試劑有限公司,上海 201506)
摘要:對比研究了光度滴定電極法與化學(xué)滴定法測量乙二胺四乙酸二鈉標(biāo)準(zhǔn)滴定溶液濃度的優(yōu)缺點(diǎn)。實(shí)驗(yàn)表明:光度滴定電極法標(biāo)定0.05010、0.1006 mol/L的乙二胺四乙酸二鈉容量分析用溶液標(biāo)準(zhǔn)物質(zhì)的En值分別為:0.19和0.008,均小于1,光度滴定電極法的測試結(jié)果與乙二胺四乙酸二鈉容量分析用溶液標(biāo)準(zhǔn)物質(zhì)特性值的一致性滿足要求。光度滴定電極法與化學(xué)滴定法測試乙二胺四乙酸二鈉容量分析用溶液標(biāo)準(zhǔn)物質(zhì)濃度的相對標(biāo)準(zhǔn)偏差均小于0.1%,但光度滴定電極法的重復(fù)性表現(xiàn)相比化學(xué)滴定法更加優(yōu)秀。光度滴定電極法測試乙二胺四乙酸二鈉容量分析用溶液標(biāo)準(zhǔn)物質(zhì)濃度的相對擴(kuò)展不確定度(0.17%、0.15%)小于化學(xué)滴定法(0.21%、0.23%),測試結(jié)果的準(zhǔn)確性更高。光度滴定電極法每次滴定所消耗的時(shí)間約為117 s,化學(xué)滴定法每次滴定所消耗的時(shí)間約為271 s,光度滴定電極法的滴定速度明顯快于化學(xué)滴定法的滴定速度。
關(guān)鍵詞:自動(dòng)電位滴定;乙二胺四乙酸二鈉標(biāo)準(zhǔn)滴定溶液;光度滴定電極;化學(xué)滴定;相對標(biāo)準(zhǔn)偏差;相對誤差
中圖分類號:O655 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:
DOI:10.13822/j.cnki.hxsj.2026.0055
Comparative Study of Different Methods of Measuring the Concentration of a Disodium Ethylenediaminetetraacetic Acid Standard Titration Solution ZHENG Qi, CAO Xiao-rong, ZHANG Yong-ji*, YU Jia-jun*, Bai Qian (Sinopharm Chemical Reagent Co., Ltd., Shanghai 201506, China)
Abstract:A comparative study was conducted to evaluate the advantages and disadvantages of photometric titration with an electrode and chemical titration in determining the concentrations of disodium ethylenediaminetetraacetic acid (EDTA) standard titration solutions. The respective En values used for calibrating the 0.05010 and 0.1006 mol/L EDTA standard solutions using photometric titration with an electrode were 0.19 and 0.008, respectively which are <1. The results obtained using photometric titration with an electrode displayed satisfactory consistencies with the characteristic values of the EDTA standard solutions. Both methods exhibited relative standard deviations of <0.1% when evaluating EDTA standard solutions, with photometric titration using an electrode displaying a superior repeatability compared to that of chemical titration. The relative expanded uncertainties of concentration determination using photometric titration with an electrode (0.17% and 0.15%) were lower than those of chemical titration (0.21% and 0.23%), indicating a higher measurement accuracy. Photometric titration with an electrode required approximately 117 s per titration cycle, which was significantly faster than the duration of 271 s required for chemical titration, revealing a markedly improved titration efficiency.
Key words:automatic potentiometric titrator; ethylenediamine tetraacetic acid disodium salt standard titration solution; Photometric titration electrode; chemical titration; relative standard deviation; relative error
【合成與應(yīng)用】
嵌段共聚物與剛性功能粒子的受限共組裝及其微結(jié)構(gòu)調(diào)控機(jī)制研究
童亮1,曾蕓1,羅?h1,劉忠春2,李金輝*1
(1. 江西理工大學(xué) 江西省功能晶態(tài)材料化學(xué)江西省重點(diǎn)實(shí)驗(yàn)室,江西 贛州 341000;2. 江西永通科技股份有限公司,江西 贛州 341000)
摘要:通過構(gòu)建4種嵌段共聚物(P2VP-b-PtBA、P2VP-b-PNIPAAm、PS-b-P4VP、PS-b-PNIPAAm-b-PMMA)與4種剛性功能粒子(天然石墨、包裹石墨、硬碳、普魯士藍(lán)類似物)的系統(tǒng)研究模型,采用溶劑蒸發(fā)誘導(dǎo)的三維受限共組裝方法,并利用透射電子顯微鏡對復(fù)合形貌進(jìn)行系統(tǒng)表征。結(jié)果表明,聚合物鏈段的化學(xué)性質(zhì)通過調(diào)控液滴在剛性粒子表面的潤濕行為,主導(dǎo)了最終復(fù)合形貌的形成。具體而言,含聚苯乙烯嵌段的體系憑借與石墨表面之間的強(qiáng)π-π相互作用,實(shí)現(xiàn)連續(xù)、緊密的包覆結(jié)構(gòu);含聚乙烯基吡啶嵌段的體系則通過其吡啶基團(tuán)與普魯士藍(lán)顆粒表面金屬離子的配位作用,實(shí)現(xiàn)特異性吸附,形成穩(wěn)固的“球-方塊”異質(zhì)鑲嵌結(jié)構(gòu);而在缺乏此類特異性相互作用的體系中,則觀察到明顯的去潤濕現(xiàn)象,導(dǎo)致聚合物微球發(fā)生屈曲、團(tuán)聚或微相分離。建立了聚合物-填料界面相互作用與復(fù)合形貌之間的結(jié)構(gòu)-性能關(guān)聯(lián),為功能化復(fù)合材料的微觀結(jié)構(gòu)預(yù)先設(shè)計(jì)提供了具有一定普適性的方法參考。
關(guān)鍵詞:嵌段共聚物;三維受限組裝;復(fù)合材料;界面潤濕;微結(jié)構(gòu)調(diào)控
中圖分類號:O631 文獻(xiàn)標(biāo)識(shí)碼:A 文章編號:0258-3283(2026)--
DOI:10.13822/j.cnki.hxsj.2026.0038
Restricted Co-Assembly of Block Copolymers and Rigid Functional Particles and Their Microstructural Regulation Mechanisms TONG Liang1, ZENG Yun1, LUO Yue1, LIU Zhong-chun2, LI Jin-hui*1 (1. Jiangxi Provincial Key Laboratory of Functional Crystalline Materials Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China; 2. Jiangxi Yongtong Technology Co., Ltd., Ganzhou 341000, China)
Abstract:A systematic research model comprising four block copolymers (P2VP-b-PtBA, P2VP-b-PNIPAAm, PS-b-P4VP, and PS-b-PNIPAAm-b-PMMA) and four rigid functional particles (natural graphite, encapsulated graphite, hard carbon, and a Prussian blue analogue) was constructed using a solvent-evaporation-induced three-dimensional confined co-assembly method. The resulting composite morphologies were systematically characterized by transmission electron microscopy. The results showed that the final composite morphology was primarily governed by the chemical properties of the polymer segments and involved regulation of the wetting behavior of droplets on the surfaces of the rigid particles. Specifically, systems containing polystyrene blocks formed continuous and dense coating structures via strong π-π interactions with the graphite surface. Systems containing polyvinylpyridine blocks exhibited specific adsorption through coordination between pyridine groups and metal ions on the surfaces of Prussian blue particles, forming stable heteromeric “ball-square” structures. Systems lacking such specific interactions exhibited significant dewetting phenomena, resulting in buckling, agglomeration, or microphase separation of polymer microspheres. A structure-property correlation between interfacial polymer-filler interactions and composite morphology was established, providing a general reference for the predesign of functionalized composite microstructures.
Key words:block copolymers; 3D restricted assembly; composite materials; interfacial wetting; microstructural regulation