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    《化學試劑》2022年第3期中英文摘要

    發布時間: 2022-03-10 14:11:19   試劑信息網

    可見光催化構建碳氮鍵的研究進展

     

    范玉蘭,蔡劉歡,郭維*

    (贛南師范大學 化學化工學院,江西贛州341000

     

    摘要:可見光是一種清潔的可再生能源,利用可見光能代替傳統的熱能進行化學轉化具有綠色、高效優點。碳氮鍵是廣泛存在于多種生物活性分子和藥物分子中的重要化學鍵,光催化構筑碳氮鍵在有機和藥物化學領域中具有重要研究意義。近年來光催化形成碳氮鍵研究得到了快速發展,許多新穎的合成方法不斷涌現。綜述了可見光催化構建C(sp2)N鍵和C(sp3)N的研究新進展,并對部分反應機理進行了評述。

    關鍵詞:光催化反應;碳氮鍵形成;機理;研究進展

    中圖分類號:O621.3      文獻標識碼:A      文章編號:0258-32832022--

     

    Recent Advances in Visible-Light Catalyzed Formation of Carbon-Nitrogen Bonds FAN Yu-lan, CAI Liu-huan, GUO Wei* (School of Chemistry and Chemical Engineering, Gannan Normal University, Ganzhou 341000, China), Huaxue Shiji, 2022, 44(3),

    Abstract: Visible light is an efficient, clean, and renewable energy. Compared with traditional thermal conditions, visible light catalyzed chemical transformation shave huge advantages of green and high efficiency. Carbon-nitrogen bonds are important chemical bonds that exist in bioactive and medicinal molecules. Construction of carbon-nitrogen bonds is significant in organic and pharmaceuticalchemistry. Recently, various novel visible-light catalyzed synthetic carbon-nitrogen bonds formation methods have been developed rapidly. In this review, we have focused on the recent research on visible light catalyzed C(sp2)N and C(sp3)N bonds formation. Some possible reaction mechanisms are also reviewed.

    Keywords: visible-light catalyzed reaction; carbon-nitrogen bond formation; mechanism; research progress

    引用本文:范玉蘭,蔡劉歡,郭維. 可見光催化構建碳氮鍵的研究進展[J]. 化學試劑,2022, 44(3):317-327.

     

    pH和溫度響應型介孔SiO2雜化材料的藥物控釋研究進展

    徐小歡,孫繼紅*

    (北京工業大學 環境化工系 綠色催化與分離北京市重點實驗室,北京  100124

     

    摘要:基于介孔SiO2所制備的智能響應型有機-無機雜化納米復合材料由于其優異的物化性能、可控的結構特征及其良好的生物相容性,近年來在藥物緩控釋領域中備受關注。針對丙烯酰胺共聚丙烯酸聚合物P(NIPAM-co-AA)和介孔SiO2納米球,分析和歸納了具有pH和溫度雙重響應性能的介孔SiO2雜化材料的合成策略、物化性能及其構-效關系,重點闡述了刺激響應機制研究進展及其對藥物裝載和緩控釋放性能的發展動態,同時對現存問題和應用前景進行了評述。為構建新型智能響應型納米多孔復合材料具有一定的學術價值。

    關鍵詞:有機-無機雜化材料;介孔SiO2納米顆粒;藥物控釋;智能響應性

    中圖分類號:TB33; TQ460.4          文獻標識碼:A        文章編號:0258-32832022

     

    Research Progress on pH- and Temperature-responsive Hybrid Materials Based on the Mesoporous Silicas for Controlled Drug Delivery XU Xiao-huan, SUN Ji-hong* (Beijing Key Laboratory of Green Catalysis and Separation, Department of Environmental and Chemical Engineering, Beijing University of Technology, Beijing 100124, China), Huaxue Shiji, 2022, 44(3)

    Abstract: In recent years, the intelligent responsive organic-inorganic hybrid nanocomposites based on mesoporous silicas have attracted much attention in the sustained and controlled drug delivery fields due to their excellent physical and chemical properties, controllable structural characteristics and good biocompatibility. Focused on the copolymer of acrylamide and acrylic acid P(NIPAM-co-AA) and mesoporous SiO2 nanospheres, this review mainly summarized and analyzed the synthesis strategies, physic-chemical properties and structure-performance relationships of the dual pH- and temperature-sensitive mesoporous silica hybrid nanocomposites, in which the stimulus-responsive mechanism research progress and the development of drug loading, sustained and controlled drug-released properties were emphasized, and the present challenges and the developed prospects were also addressed. This contribution provided a certain academic basis for constructing novel intelligent responsive nanoporous composites.

    Key words: organic-inorganic hybrid materials; mesoporous silica nanoparticles; controlled drug delivery systems; intelligent responsiveness

    引用本文:徐小歡,孫繼紅. pH和溫度響應型介孔SiO2雜化材料的藥物控釋研究進展[J]. 化學試劑, 2022, 44(3): 328-338。

     

     

    基于TCF的熒光探針的設計與應用研究進展

     

    李朝政,陳駿,楊金華,周莉佳,裴叔宸*

    (重慶科技學院 工業發酵微生物重慶市重點實驗室,重慶  401331)

     

    摘要2-二氰基亞甲基-3-氰基-4,5,5-三甲基-2,5-二氫呋喃(TCF)是一個強電子供體,廣泛應用于光學材料和分子熒光探針。同時,TCF結構簡單,活性位點少,能通過簡單的反應與苯基偶聯。同時,基于TCF的分子探針具有大的斯托克斯位移和較高的量子產率。根據TCF熒光探針的檢測對象,將其分為陰陽離子、生物分子和其它分子,并從分子結構、性能、機理出發,綜述了5年來國內外基于TCF的熒光探針在設計和檢測方面的新進展。最后提出了構建新型TCF類分子熒光探針面臨的挑戰和發展方向。

    關鍵詞TCF;熒光探針;響應機理;設計;研究進展

    中圖分類號:O621.4         文獻標識碼:A       文章編號:0258-32832022

     

    Progress in Design and Application of TCF-Based Fluorescent Probes LI Chao-zheng, CHEN Jun, YANG Jin-hua, ZHOU Li-jia, PEI Shu-chen* (Chongqing Key Laboratory of Industrial Fermentation Microorganism, Chongqing University of Science and Technology, Chongqing 401331, China), Huaxue Shiji, 2022, 44(3),

    Abstract: 2-Dicyanomethylene-3-cyano-4,5,5-trimethyl-2,5-dihydrofuran (TCF) is a strong electron donor,which is widely used in optical materials and molecular fluorescence probes. At the same time,TCF has a simple structure, few active sites,and can be coupled to phenyl groups through a simple reaction. TCF-based molecular probes have a large Stokes shift and a high quantum yield. According to the detection object of TCF fluorescent probe, it is divided into anion and cation, biomolecule and other molecules, and starting from the molecular structure, performance and mechanism, the design and detection of TCF-based fluorescent probes at home and abroad in five years are reviewed. Finally, the challenges and development directions for constructing new TCF molecular fluorescent probes are proposed.

    Key words: TCF; fluorescent probes; response mechanism; design; research progress

    引用本文:李朝政,陳駿,楊金華,等.基于2-二氰基亞甲基-3-氰基-4,5,5-三甲基-2,5-二氫呋喃的熒光探針的設計與應用研究進展[J].化學試劑,2022,443):339-348.

     

     

    sp2-碳共價有機框架材料的研究進展

    黃小瑩1,張黎君1,孫淑香*1,徐元清*1,2

    (1. 河南應用技術職業學院 化學工程學院,河南 鄭州 450042;2. 河南大學 化學化工學院,河南 開封  475004

     

    摘要:共價有機框架材料是一類晶態高分子材料,通過定向的拓撲聚合將有機結構單元聚合為高度有序和延伸的二維或者三維框架材料。近5年來,合成化學的進展大大地促進了共價有機框架材料的結構設計與合成,實現了完全共軛的具有大π體系的sp2-碳共價有機框架材料的構筑。主要介紹了近年來通過不同的設計原則和合成策略來構筑基于sp2-碳共價有機框架材料的研究進展,展示了該類材料的性質、功能以及結構多樣性,并就關鍵的科學問題和未來的發展方向進行了展望。

    關鍵詞共價有機框架材料;共價有機框架;sp2雜化;π-共軛體系;合成方法

    中圖分類號O627.32      文獻標識碼A      文章編號0258-3283(2022)--

     

    Research Progress of sp2-C Covalent Organic Frameworks HUANG Xiao-ying1, ZHANG Li-jun1, SUN Shu-xiang*2, XU Yuan-qing*1,2 (1. School of Chemical Engineering, Henan Technical Institute, Zhengzhou 450042, China;2. Henan University, School of Chemistry and Chemical Engineering, Kaifeng 475004, China), Huaxue Shiji, 2022, 44(3),

    Abstract: Covalent organic frameworks (COFs) are a class of crystalline polymer material that integrate organic units into 2D or 3D skeletons to achieve ordered yet extended structures via topology-directed polymerization. Over past five years, recent progress in synthetic chemistry has greatly raised the ability of design and synthesis for the frameworks to attain fully π-conjugated all sp2-carbon-linked covalent organic frameworks. This review will summarize the chemistry to explore sp2 carbon frameworks by different design principles and synthetic strategies to demonstrate the properties, functions and structural diversity. The key scientific issues and prospects for the future of this field are also prognosticated.

    Key words: covalent organic frameworks; sp2 hybridization; π-conjugate; synthetic method

    引用本文:黃小瑩,張黎君,孫淑香,等. 二維sp2-碳共價有機框架材料的研究進展[J]. 化學試劑,2022,44(3)349-363.

     

     

    托盤根中總多酚提取工藝及抗氧化活性研究

    趙楠*,張春楠,柴軍紅,何婷婷

    (牡丹江師范學院 生命科學與技術學院,黑龍江 牡丹江  157011

     

    摘要:以懸鉤子屬植物托盤根為研究對象,采用超聲輔助乙醇提取托盤根中總多酚。通過對乙醇濃度、料液比、超聲時間、超聲溫度4種影響因素進行考察,在單因素實驗結果基礎上,采用正交試驗優化其最佳提取工藝,并對托盤根總多酚的抗氧化能力進行評價。結果表明,托盤活性成分的最佳提取工藝為乙醇濃度60%、超聲溫度80 ℃、超聲時間50 min、料液比1:40 g/mL。在此條件下托盤根總多酚提取率為26.16%。托盤根總多酚清除DPPH自由基及羥基自由基的IC50值分別為0.00690.346 mg/mL,表明托盤根總多酚具有一定的抗氧化能力。

    關鍵詞:托盤;總多酚;超聲提??;正交設計;抗氧化

    中圖分類號:R284.2           文獻標識碼:A           文章編號:0258-32832022

     

    Extraction and Antioxidant Activity of Total Polyphenols from Rubus Crataegifolius Bunge Roots ZHAO Nan*, ZHANG Chun-nan, CHAI Jun-hong, HE Ting-ting (College of Life Science and Technology, Mudanjiang Normal University, Mudanjiang 157011, China), Huaxue Shiji, 2022, 44(3)

    Abstract: To investigate the total polyphenols from Rubus crataegifolius Bunge roots, ultrasonic-assisted ethanol extraction was used. By investigating four influencing factors (including ethanol concentration, ultrasonic temperature and time, and solid-liquid ratio), and using orthogonal experimental design on the basis of single factor experiments, the extraction was optimized, and the antioxidant activity was evaluated. The results suggested the following optimum conditions: ethanol concentration 60%, solid-liquid ratio 1:40 g/mL, ultrasonic 50 min at 80 . Under this condition, the extraction rate of total polyphenols reached 26.16%. The IC50 of total polyphenols from Rubus crataegifolius Bunge against DPPH and hydroxyl anion free radicals were 0.0069 and 0.346 mg/mL, respectively, which illustrated good antioxidant activity of the total polyphenols.

    Key words: Rubus crataegifolius Bunge; total polyphenols; ultrasonic extraction; orthogonal design; antioxidant

    引用本文:趙楠,張春楠,柴軍紅,等. 托盤根中總多酚提取工藝及抗氧化活性研究[J]. 化學試劑, 2022: 44(3), 364-368。

     

     

    朝鮮淫羊藿中性多糖與酸性多糖的理化特征及抗氧化活性的比較

    李波1,李珺銘1,劉富饒1,王哲*1,焦麗麗*2

    (長春中醫藥大學a. 藥學院,b. 吉林省人參科學研究院,吉林 長春 130117)

     

    摘要對朝鮮淫羊藿多糖(EFPC)進行分離純化,并對其理化性質及抗氧化活性進行研究。采用水提醇沉法獲得朝鮮淫羊藿粗多糖,通過除蛋白,經DEAE-52纖維素色譜柱(0.5 mol/L NaCl溶液洗脫),得到中性多糖(EFPN)和酸性多糖(EFPA)。EFPC、EFPNEFPA糖含量分別為79.59%、87.14%91.43%,蛋白含量都小于1%,EFPNEFPA分子量分別為1.5×1041.4×105 Da2.5×1049.8×104 Da;EFPN由甘露糖、鼠李糖、阿拉伯糖、半乳糖和葡萄糖組成,其物質的量比為0.61.01.41.61.7,EFPA由甘露糖,葡萄糖,半乳糖,葡萄糖醛酸和阿拉伯糖組成,其物質的量比為1.77.41.41.81.0;EFPN在清除自由基、金屬離子螯合和還原能力方面IC50值均高于EFPA,EFPN組不同程度的提高了小鼠血清與肝臟中酶活性(P<0.01P<0.05),降低了MDA(P<0.01P<0.05)的水平。EFPN抗氧化活性較好,是天然抗氧化劑的良好來源,可進一步開發利用。

    關鍵詞朝鮮淫羊藿;中性多糖;酸性多糖;理化性質;抗氧化活性

    中圖分類號R965       文獻標識碼A      文章編號0258-32832022--

     

    Comparison of physicochemical properties and antioxidant activities neutral and acidic polysaccharides from Epimedium koreanum Nakai LI Bo1, LI Jun-ming1, LIU Fu-rao1, WANG Zhe*1, JIAO Li-li*2 (1a. College of Pharmacy, 1b. Jilin Ginseng Academy, Changchun University of Chinese Medicine, Changchun 130117, China), Huaxue Shiji, 2022, 44(3),

    Abstract: In this study, to purify polysaccharides from the Epimedium koreanum Nakai (EFPC) and then fractionated into two polysaccharides (EFPN and EFPA) by DEAE-52 with 0.5 mol/L NaCl. Then investigated for their general physicochemical properties, monosaccharide composition, molecular and their antioxidant activities. The total sugar contents of EFPC, EFPN and EFPA were 79.59%, 87.14% and 91.43%, respectively. EFPN is composed of mannose, rhamnose, arabinose galactose and glucose, with ratios of 0.61.01.41.61.7, and EFPA is composed of mannose, glucose, galactose, galacturonic acid and arabinose with ratios of 1.77.41.41.81.0. The average molecular of EFPN and EFPA were 1.5×104 Da1.4×105 Da and 2.5×104 Da9.8×104 Da. EFPN, showing a higher radical scavenging activities (IC50), metal chelating abilities(IC50) and reducing abilities than EFPA in vitro antioxidant assay. EFPN can significantly increase (P<0.05 and P<0.01) the content of antioxidant enzymes in serum and liver tissue of aging mice, significantly reduce (P<0.05 and P<0.01)lipid peroxide activities, and have good repair effect on oxidative stress injury.

    Key words: Epimedium koreanum Nakai; neutral polysaccharides; acidic polysaccharides; physicochemical properties; antioxidant activities

    引用本文:李波,李珺銘,劉富饒,等. 朝鮮淫羊藿中性多糖與酸性多糖的理化特征及抗氧化活性的比較[J]. 化學試劑,2022,44(3): 369-375。

     

     

    咪唑喹啉衍生物與小牛胸腺DNA作用機理研究

    王煒祺1,陳昌云*2,許小青1,鮑真真1,鐘嫄1,吳潔1

    (1.    江蘇衛生健康職業學院  藥學院,江蘇 南京  211800;2. 南京曉莊學院  環境科學學院,江蘇 南京  211171

     

    摘要對于咪唑喹啉衍生物(IQDs)與小牛胸腺脫氧核糖核酸(CT-DNA)的相互作用機理,本文采用熒光光譜法、黏度法、熱變性研究和瓊脂糖凝膠電泳法等實驗技術進行研究。實驗結果顯示,咪唑喹啉衍生物以嵌插模式與CT-DNA作用,衍生物以溝槽模式與CT-DNA作用,且衍生物CT-DNA的作用強于,而衍生物幾乎不與CT-DNA發生作用。利用Gaussian 98量子化學程序包構建并優化3種衍生物分子模型,在HF/6-31G基組水平上進行計算,量子化學理論計算結果表明大環C9位上的取代基對結合模式和強度起著關鍵作用,與實驗結果一致。

    關鍵詞咪唑喹啉衍生物;小牛胸腺DNA;熒光光譜;瓊脂糖凝膠電泳;量子化學計算

    中圖分類號O657      文獻標識碼A      文章編號0258-32832022--

     

    Study on the interaction mechanism of imidazolequinoline derivatives with calf thymus DNA WANG Wei-qi1, CHEN Chang-yun*2 XU Xiao-qing1, BAO Zhen-zhen1, ZHONG Yuan1, WU Jie1 (1. School of pharmacy, Jiangsu Health Vocational College, Nanjing 211800, China; 2. School of Environmental Science, Nanjing Xiaozhuang University, Nanjing 211171, China), Huaxue Shiji, 2022, 44(3),

    Abstract: The mechanism of interaction between imidazoquinoline derivatives and DNA was studied by fluorescence spectroscopy, DNA viscosity determination, DNA denatured temperature and gel electrophoresis. The quantum chemistry calculation for three derivatives was performed on HF/6-31G basis set after optimizing with Gaussian 98 program. The experimental and computational results showed that the substituents at C9 position of macrocycle play a key role in the binding mode and interaction strength. The three derivatives interacted with DNA in different ways.Ⅰ interacted with CT-DNA in the mode of intercalative binding; Ⅱ interacted with CT-DNA in the mode of groove binding; Ⅲ didn’t interact with CT-DNA.

    Key words: Imidazoquinoline derivatives; CT-DNA; Fluorescent spectroscopy; Gel electrophoresis; Quantum chemistry calculation

    引用本文王煒祺,陳昌云,許小青,等. 咪唑喹啉衍生物與小牛胸腺DNA作用機理研究[J]. 化學試劑,2022,44(3):376-384。

     

     

    二氧化硅/聚噻吩復合吸附劑處理Pb2+Cd2+

    張麗麗*

    (濮陽職業技術學院 能源與化學工程學院,河南 濮陽 457000

     

    摘要綠色環保、高效等特點是吸附劑發展的趨勢。以溶膠-凝膠法合成了SiO2,再與聚噻吩合成了SiO2/聚噻吩復合材料。采用掃描電鏡(SEM)、傅里葉紅外光譜(FT-IR)以及Zeta電位對復合材料進行了表征分析。SiO2/聚噻吩是表面粗糙的球形,且表面帶有負電荷。SiO2/聚噻吩復合材料用于吸附Pb2+Cd2+離子,改變吸附過程中的變量來研究吸附過程的影響因素,通過探討動力學和等溫線模型來研究其吸附機理。研究結果表明,pH通過改變SiO2/聚噻吩表面的電荷數來影響吸附性能,以及吸附容量與吸附劑的量不呈正相關。同時得知,SiO2/聚噻吩吸附劑吸附Pb2+Cd2+的過程符合擬二級動力學模型及Langmuir等溫線模型。以研究結果提出吸附機理:SiO2/聚噻吩表面的負電荷吸引帶有正電荷的重金屬離子,以單分層的化學吸附為主吸附過程。

    關鍵詞吸附劑;復合材料;污水處理;二氧化硅;聚噻吩

    中圖分類號:TQ3118文獻標識碼:A 文章編號:0085292021- -

     

    Treatment of Pb2+ and Cd2+ with silica/polythiophene composite adsorbent Zhang Li-li* (Puyang Vocational and Technical College, Puyang 457000, China), Huaxue shiji,2021, 44(3),

    Abstract: Green environmental protection, high efficiency is characterized by the development trend of adsorbent.SiO2/polythiopheneis composites were synthesized by sol-gel method with SiO2 and polythiophene. The composites were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and zeta potential. SiO2/polythiopheneis spherical with rough surface and negative charge on the surface.SiO2/polythiopheneis composites are used to adsorb Pb2+ and Cd2+ ions. The influencing factors of the adsorption process are studied by changing the variables in the adsorption process. The adsorption mechanism is studied by discussing the kinetics and isotherm model. The results show that pH affects the adsorption performance by changing the charge number of SiO2/polythiopheneis surface, and the adsorption capacity is not positively correlated with the amount of adsorbent. It is also known that the adsorption process of Pb2+ and Cd2+ on SiO2/polythiopheneis adsorbent conforms to the pseudo second-order kinetic model and Langmuir isotherm model. Based on the research results, the adsorption mechanism is proposed: the negative charge on the SiO2/polythiopheneis surface attracts the positively charged heavy metal ions, and the single layered chemical adsorption is the main adsorption process.

    Keywords: adsorbent; composite material; sewage treatment; silica

    引用本文張麗麗. 二氧化硅/聚噻吩復合吸附劑處理Pb2+Cd2+[J]. 化學試劑,2021,44(3):385-392。

     

     

    新型生物質果膠吸附材料的制備及水溶液中銅離子(II)吸附性能研究

    姚元勇,何來斌,張萌,陳仕學*,吳蘭艷

    銅仁學院 材料與化學工程學院 銅仁市中藥民族藥現代化研究與開發利用重點實驗室,貴州 銅仁  554300)

     

    摘要:為了評價生物質果膠堿化改性在重金屬離子廢水處理方面的吸附性能,利用水提-醇沉法提取純化豆腐柴葉中天然果膠,并通過堿化作用,制備新型生物質果膠吸附材料,同時對水溶液中重金屬銅離子進行吸附作用試驗,考察其吸附率和單位吸附量。然后,通過分析新型生物質果膠吸附材料組分半乳糖醛酸含量及酯化度,探討其吸附作用機制。實驗結果表明,天然果膠在pH 9的環境中堿化作用30 min時,可制備獲得具有高效吸附水體中銅離子的新型生物質果膠吸附材料,其吸附率和單位吸附量分別可達到89.6%0.10 g)和105 mg/g0.02 g)。另外,在果膠組分半乳糖醛酸含量和酯化度分析方面,果膠堿化作用未造成半乳糖醛酸分子的丟失,但可促使果膠中羧酸酯的水解,形成對應的羧酸鈉鹽,提升對水體銅離子的吸附性能。

    關鍵詞:重金屬銅離子;天然果膠;豆腐柴;吸附材料;銅離子

    中圖分類號X-1       文獻標識碼A      文章編號0258-32832022

     

    Preparation of Novel Biomass Pectin Adsorbing Material Modified via Alkalization And Its Adsorption Performance for Copper (II) Ion in Aqueous Solution YAO Yuan-yong, HE Lai-bing, ZHANG Meng, CHEN Shi-xue*, WU Lan-yan (Tongren Key Laboratory for Modernization Research, Development and Utilization of Traditional Chinese Medicine and National Medicine, School of Material and Chemical Engineering, Tongren university, Tongren 554300, China), Huaxue Shiji, 2022, 44(3)

    Abstract: To evaluate the adsorption performance of biomass pectin modified via alkalization in the treatment of heavy-metal ion wastewater. Natural pectin isolated from Premna microphylla leaves was purified by water-alcohol precipitation. And then novel biomass pectin adsorbing material was prepared through the alkalization and applied to adsorption performance for copper ion in aqueous solution, with observing adsorption efficiency and unit adsorption quantity. Subsequently, analyzing galacturonic acid content and esterification degree of novel biomass pectin adsorbing material was utilized to propose rational mechanism of adsorption performance. The results demonstrated that novel biomass pectin adsorbing material was successfully promoted by the alkalization of natural pectin for 30 min in pH 9 aqueous solution, with good exhibitions for copper ion in adsorption efficiency and unit adsorption quantity, they are respectively 89.6% (0.10 g) and 105 mg/g (0.02 g). Furthermore, in the aspects of diagnosing galacturonic acid content and esterification degree, the alkalization for pectin is not capable to observe the loss of galacturonic acid content from the novel biomass pectin, but can promote the hydrolysis of carboxylic ester to form relative sodium salt for enhancing adsorption performance of copper ion.

    Key words: heavy metal ion; natural pectin; Premna microphylla; absorbing material;Cu2+

    引用本文:姚元勇, 何來斌, 張萌, .新型生物質果膠吸附材料的制備及水溶液中銅離子(II)吸附性能研究[J].化學試劑, 2022, 443393-400.

     

     

    磁性聚苯胺納米纖維吸附性能的探究

    李大為,陶玉侖,李碩

    (安徽理工大學 材料科學與工程學院,安徽 淮南  232000

     

    摘要:有機酸、粉煤灰磁珠為摻雜劑,過硫酸銨為氧化劑,采用氧化聚合的方法合成了磁性聚苯胺納米纖維,對合成的磁性聚苯胺進行掃描電子顯微鏡(SEM)、傅里葉變換紅外光譜儀(FTIR)、紫外可見光分光光度計(UV)、振動磁強計(VSM)、X-射線衍射儀(XRD)等表征揭示了其形貌、結構、成分和磁性能,并使用磁性聚苯胺作吸附劑對銅離子溶液以及剛果紅溶液進行吸附脫吸附研究,發現吸附率均在95%以上。通過吸附動力學對吸附機理進行探究,得出聚苯胺吸附銅離子及剛果紅符合二級動力學模型。

    關鍵詞:磁性;有機酸;聚苯胺;吸附;動力學

    中圖分類號:TQ424;X703          文獻標識碼A        文章編號0258-32832022

     

    Investigation on the Adsorption Properties of Magnetic Polyaniline Nanofibers LI Da-wei, TAO Yu-lun*, LI shuo ( School of Materials Science and Engineering, Anhui University of Technology, Huainan 232000, China), Huaxue Shiji, 44(3), 00 ~ 00

    Abstract: Magnetic polyaniline nanofibers were synthesized by using organic acid and fly ash beads as dopants and ammonium persulfate as oxide polymerization, and were characterized by employing scanning electron microscope (SEM), Fourier transform infrared spectrometer (FTIR), UV visible spectrophotometer (UV), vibrational magnetometer (VSM) and X-ray diffraction (XRD) for their morphology, structure, composition and magnetic properties. The title polyaniline was used as adsorbent to study the adsorption and desorption of copper ion solution and Congo red solution, and the adsorption rate was found to be more than 95%. Based on the investigation on the adsorption mechanism, it can be concluded that adsorption of copper ions and Congo red on the title polyaniline obey the secondary kinetic model.

    Key words: magnetism; organic acid; polyaniline; adsorption; dynamics

    引用本文:李大為,陶玉侖,李碩. 磁性聚苯胺納米纖維吸附性能的探究[J]. 化學試劑, 2022, 44(3): 401-407。

     

     

    Mn-P共摻雜氮化碳的制備及其光催化性能研究

    艾兵*,何海南,鄧璇,孫立新,楊立喜,李德剛

    (山東理工大學 化學化工學院,山東 淄博  255049)

     

    摘要:采用四水氯化錳、磷酸氫二銨和三聚氰胺為原料制備了Mn-P共摻雜的石墨相氮化碳(g-C3N4)。使用X射線衍射光譜(XRD)、掃描電子顯微鏡(SEM)、傅里葉變換紅外光譜(FT-IR)、光致熒光光譜(PL)、紫外-可見漫反射光譜(UV?Vis DRS)、電化學阻抗譜(EIS)、瞬態光電流響應等分析測試手段對制備的催化劑進行了表征。結果表明,Mn-P 共摻雜改變了氮化碳的光電性質。通過可見光降解亞甲基藍(MB)溶液證明了Mn-P共摻雜可以有效改善氮化碳的光催化性能。Mn(2.0%)-P-CNMB的降解率在120 min 內達到62.2%,其速率常數為0.0083 min-1,是純氮化碳的2.1倍。同時,探索了Mn-P共摻雜氮化碳的光催化反應機理和循環利用。

    關鍵詞:石墨相氮化碳;磷酸氫二銨;錳;可見光催化;共摻雜

    中圖分類號:O649          文獻標識碼:A               文章編號:0258-32832022--

     

    Preparation of Mn, P Co-doped Carbon Nitride and its photocatalytic properties AI Bing*, HE Hai-nan, DENG Xuan, SUN Li-xin, YANG Li-xi, LI De-gang (School of Chemistry and Chemical Engineering, Shandong University of Technology, Zibo 255049, China), Huaxue Shiji, 2022, 44(3),

    Abstract: Mn and P co-doped carbon nitride was prepared from manganese chloride tetrahydrate, diammonium hydrogen phosphate and melamine. The prepared catalysts were characterized by X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), photoluminescence spectroscopy (PL), ultraviolet?visible diffuse reflectance spectroscopy (UV?Vis DRS), electrochemical impedance spectroscopy (EIS), and transient photocurrent analytical tests. The results showed that Mn and P co-doping changed the photoelectric properties of carbon nitride. It was proved that Mn and P co-doping could effectively improve the photocatalytic performance of carbon nitride by the degradation of methylene blue (MB) solution under visible light. The degradation rate of MB by Mn (2.0%)-P-CN could reach 62.2% within 120 minutes, and its degradation rate constant was 0.0083 min-1, which was about 2.1 times higher than that of pure g-C3N4. At the same time, the photocatalytic reaction mechanism and recycling of Mn and P co-doped carbon nitride were explored.

    Key words: g-C3N4; diammonium hydrogen phosphate; manganese; visible-light photocatalysis; co-doping

    引用本文:艾兵,何海南,鄧璇,等. Mn-P共摻雜氮化碳的制備及其光催化性能研究[J]. 化學試劑,2022,44(3): 408-414。

     

     

    基于三苯胺的D-A-π-A-D型化合物的合成及光物理性能

    竇立薇1,2,高亞楠1,2,高宏*1,3,翟兆蘭1,3

     

    1. 中國林業科學研究院 林產化學工業研究所 生物質化學利用國家工程實驗室 國家林業和草原局林產化學工程重點實驗室 江蘇省生物質能源與材料重點實驗室;江蘇 南京  210042;2. 南京林業大學 江蘇省林業資源高效加工利用協同創新中心,江蘇 南京  210037;3. 中國林業科學研究院 林業新技術研究所,北京 100091

     

    摘要:以甲氧基三苯胺為電子供體,苯并噻二唑為電子受體,咔唑為共軛π橋,通過三步Suzuki偶聯反應合成了D-A-π-A-D型熒光化合物4, 4'-[(7, 7'-(9H-咔唑-2, 7-)-(苯并噻二唑-7, 4-)]-(N,N-(4-甲氧基苯基) 苯胺(DTB-CZ),并用1HNMR、13CNMR、MALDI-TOF等手段對其結構進行表征。研究了它的光譜性能、電化學性能、軌道能級和熱性能,并與D-π-D型化合物2TPA-CZ1的性能進行了比較。初步探索了DTB-CZ作為空穴傳輸材料在PSC中的應用性能。研究結果表明,DTB-CZ在甲苯溶液中的最大吸收波長為479 nm,最大發射波長為608 nm,在薄膜狀態下最大吸收波長為495 nm,HOMO/LUMO能級為-4.91/-2.82 eV,帶隙值為2.09 eV,熱分解溫度(T5d449.56 oC,玻璃化轉變溫度(Tg)為143.10 oC。相比2TPA-CZ1,在甲苯溶液中吸收和發射波長分別紅移了104、182 nm,在薄膜狀態下吸收波長紅移109 nm;帶隙值降低0.84 eV;T5dTg 分別提高了9.56、24.7 oC。結果表明,苯并噻二唑的引入,使化合物的共軛程度增大,帶隙值降低,使得吸收和發射波長紅移,使其具有更好的熱穩定性和形態穩定性。

    關鍵詞甲氧基三苯胺;苯并噻二唑;咔唑;D-A-π-A-D;光物理性能

    中圖分類號O621.3        文獻標識碼A       文章編號0258-32832022

     

    Synthesis and Photophysical Properties of D-A-π-A-D Compound Based on Triphenylamine DOU Li-wei 1,2, GAO Ya-nan 1,2, GAO Hong* 1,3, ZHAI Zhao-lan 1,3 (1. Institute of Chemical Industry of Forest Products, National Engineering Lab. for Biomass Chemical Utilization; Key Lab. of Chemical Engineering of Forest Products, National Forestry and Grassland Administration; Key Lab of Biomass Energy and Material, Chinese Academy of Forestry, Nanjing 210042, China; 2. Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources, Nanjing Forestry University, Nanjing 210037, China; 3. Research Institute of Forestry New Technology, Chinese Academy of Forestry, Beijing 100091, China), Huaxue Shiji, 2022, 44(3)

    Abstract: D-A-π-A-D type compound DTB-CZ was synthesized by three-step Suzuki cross coupling reaction, herein, methoxytriphenylamine acted as donor (D), benzothiadiazole acted as acceptor (A) and carbazole was selected as the middle π-bridge. The structure of DTB-CZ was characterized by 1HNMR、13CNMR and MALDI-TOF. Its spectral performance, electrochemical performance, orbital energy level and thermal performance were studied and compared with the performance of compound 2TPA-CZ1 with D-π-D structure. The application performance of DTB-CZ as a hole transport material in PSC was initially explored. The research results show that the maximum absorption wavelength of DTB-CZ in toluene solution is 479 nm, the maximum emission wavelength is 608 nm, and the maximum absorption wavelength is 495 nm in the film state. The HOMO/LUMO energy level of DTB-CZ is -4.91/-2.82 eV, and the band gap value is 2.09 eV. The thermal decomposition temperature of DTB-CZ is 449.56 oC, and the glass transition temperature is 143.10 oC. Compared with that of 2TPA-CZ1, the absorption and emission wavelengths in toluene solution red-shifted 104 nm and 182 nm, respectively, and the absorption wavelength red-shifted 109 nm in the film state; the band gap value decreased 0.84 eV; the thermal decomposition temperature and glass transition temperature increased 9.56 oC and 24.7 oC, respectively. It showed that the introduction of benzothiadiazole increased the conjugation degree of the compound and reduced the band gap value, which made the absorption and emission wavelength red shift; and it had better thermal stability and morphological stability.

    Key words: methoxytriphenylamine; benzothiadiazole; carbazole; D-A-π-A-D; photophysical properties

    引用本文:竇立薇,高亞楠,高宏,等.基于三苯胺的D-A-π-A-D型化合物的合成及光物理性能[J].化學試劑,2022,443):415-421.

     

     

    玉米芯基碳點的制備、表征及其對Cr(VI)的熒光檢測研究

    黎海濤1,施家威1,郭燕1,張小濤1,黎挺挺*2

    1. 浙江醫藥高等??茖W校 食品學院,浙江 寧波  315199;2. 寧波大學 材料科學與化學工程學院,浙江 寧波  315211

     

    摘要:通過一步水熱法制備了玉米芯基碳點(CDs),所制備的CDs粒徑分布均勻,在水溶液中具有良好的分散性。通過紅外光譜、紫外-可見吸收光譜以及熒光光譜對其發光性能進行了研究?;?/span>Cr(VI)能選擇性淬滅CDs的熒光,建立了以CDs為熒光探針測定Cr(VI)濃度的新方法,當Cr(VI)的濃度范圍為2~80 μmol/L時,CDs熒光淬滅強度與Cr(VI)濃度呈現較好的線性關系,該方法檢出限可達0.98 μmol/L。該方法應用于工業廢水中Cr(VI)的測定,測得的結果與分光光度法基本一致。

    關鍵詞:碳點;熒光識別;Cr(VI)檢測;淬滅機理;低檢測限

    中圖分類號:O655.21           文獻標識碼:A              文章編號:

     

    Preparation and Characterization of Corncob Carbon Dots, and Their Application in Fluorescence Detection of Cr(VI) LI Hai-tao1,SHI Jia-wei1, GUO Yan1, ZHANG Xiaotao1, LI Ting-Ting*2 (1. Faculty of Food Science, Zhejiang Pharmaceutical College, Ningbo 315100; 2. School of Material Science and Chemical Engineering, Ningbo University, Ningbo 315211)

    AbstractCarbon dots (CDs) were synthesized by one-step hydrothermal approach with corncob as the carbon source. The resultant CDs possess uniform particle size distribution and excellent dispersibility in aqueous solution. The photophysical properties of CDs were characterized by infrared spectroscopy, UV-Vis absorption spectroscopy, and fluorescence spectroscopy. The fluorescence spectra showed that the fluorescence of CDs could be quenched by Cr(VI), and thus we employed CDs as the probe to determine the Cr(VI) concentration in aqueous solution. Cr(VI) concentration displayed a good linear relationship with the intensity of fluorescence quenching in the range of 2~80 μmol/L, the corresponding detection limit was 0.98 μmol/L. Finally, this method was used to determine the Cr(VI) concentration in industrial wastewater, and the result was nearly in accordance with that obtained from spectrophotometric method.

    Key wordscarbon dots; fluorescence detection; Cr(VI) detection; quenching mechanism;low detection limit

    引用本文:黎海濤,施家威,郭燕,等.玉米芯基碳點的制備、表征及其對Cr(VI)的熒光檢測研究[J].化學試劑,443422-426.

     

     

    可連續識別Cu2+PPi的熒光探針的合成及性能研究

    李生玲*1,常西亮1,孔祥鵬1,成果1,王明亞2

    (1.  太原工業學院 化學與化工系,山西 太原 030008;2. 中北大學 化學工程與技術學院,山西 太原 030051

     

    摘要:連續識別型熒光探針能在同一測試條件下連續識別兩種離子,使得離子的檢測更具專一性,是在普通同類型探針檢測功能方面的拓展。設計合成了以7-二乙氨基香豆素為母體、咪唑-2-甲醛為識別基團的一種高選擇性的席夫堿型熒光探針CI,用于連續識別Cu2+和焦磷酸根離子(PPi)。探針CICu2+表現出了明顯的“開-關”熒光淬滅響應,淬滅率為100%,而形成的配合物CI-Cu2+PPi呈現明顯的“關-開”熒光增強響應。探針CICu2+PPi的檢出限均為0.14 μmol/L,其與Cu2+的配位比為11,而CI-Cu2+配合物與PPi21配位。在pH 511的范圍內,探針CICI-Cu2+具有很好的識別能力。

    關鍵詞:香豆素;熒光探針;咪唑;Cu2+;PPi;連續識別

    中圖分類號O622        文獻標識碼A       文章編號0258-32832022--

    A synthesis and performance study of fluorescent probe for sequential recognition of Cu2+ and PPi LI Sheng-ling*1, CHENG Xi-liang1, KONG Xiang-peng1, CHENG Guo1, WANG Ming-ya2 (1. Department of Chemistry and Chemical Engineering, Taiyuan Institute of Technology, Taiyuan 030008, China; 2. School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, China), Huaxue Shiji, 2022, 44(3),

    Abstract: Sequential recognition fluorescent chemical probe can continuously identify two kinds of ions under the same test condition, making the ion detection more specific, which is an extension of the detection function of common probes of the same type. In this study, a highly selective Schiff base fluorescent probe CI was synthesized with 7-diethylaminocoumarin as the parent and imidazole-2-carboxaldehyde as the recognition group for sequential recognition of Cu2+ and PPi. The probe CI showed an obvious "on-off" fluorescence quenching response to Cu2+ with an efficiency of 100 %, and the CI-Cu2+ complex showed an "off-on" response to PPi fluorescence enhancement. The detection limit of probe CI for Cu2+ and PPi was 0.14 μmol/L. The binding capacity of probe CI and Cu2+ was 11, and the binding capacity of CI-Cu2+ complex and PPi was 21. The optimum pH range of probe CI and CI-Cu2+ was 511.

    Keywords: Coumarin; Fluorescent probe; Imidazole; Cu2+; PPi; Continuous recognition

    引用本文:李生玲,常西亮,孔祥鵬,等. 可連續識別Cu2+PPi的熒光探針的合成及性能研究[J]. 化學試劑, 2022, 44(3): 427-435。

     

     

    藜麥產地的紅外光譜鑒別

    嚴偉敏1,劉剛*,田雪1,歐全宏1,車前1,時有明2

    (1.云南師范大學 物理與電子信息學院,云南 昆明  650500;2.曲靖師范學院 物理與電子信息學院,云南 曲靖  655011

     

    摘要:種植環境差異導致不同產地的藜麥有差異,故對不同產地的藜麥進行區分鑒別對商家、消費者具有重要參考價值。將中紅外光譜結合主成分分析(PCA)、線性判別分析(LDA)及混淆矩陣對不同產地藜麥進行鑒別研究。結果顯示:藜麥的紅外光譜主要由淀粉、蛋白質和脂質譜峰組成,且在蛋白質和糖類譜峰上有差異。用600~4000 cm-1范圍的原始光譜進行PCA分析,前兩個主成分(PC)取得了92%的累計方差貢獻率,基于PCA分析生成的PC進行LDA分析,取得了96.25 %的分類精度?;陬A測結果的混淆矩陣作為綜合評價指標,得到PCA-LDA分類模型的精確度、召回率及特異性分別為96.25%、96.59%99.48%,說明使用PCA-LDA模型可以對藜麥產地進行有效鑒別。研究表明,紅外光譜結合多元統計分析方法,是鑒別藜麥產地的有效方法。

    關鍵詞紅外光譜;藜麥;產地鑒別;主成分分析;線性判別分析

    中圖分類號:O657.33   文獻標志碼A   文章編號:0258-32832022

     

    Identification of Quinoa Origin by Infrared Spectroscopy YAN Wei-min 1, LIU Gang*1, TIAN Xue 1, OU Quan-hong 1, CHE Qian 1, SHI You-ming 2 (1. School of Physics and Electronic Information, Yunnan Normal University, Kunming 650500, China; 2. School of Physics and Electronic Engineering, Qujing Normal University, Qujing 655011, China), Huaxue Shiji, 2022, 44(3)

    Abstract: The difference of planting environment leads to the difference of quinoa in different producing areas. So, the identification of quinoa from different producing areas is of great reference value to merchants and consumers. In this paper, infrared spectroscopy combined with principal component analysis (PCA), linear discriminant analysis (LDA) and confusion matrix were used to identify quinoa from different areas. The results showed that the infrared spectra of quinoa mainly composed of starch, protein and lipid band, and there are differences in the protein and starch peaks. PCA analysis was carried out with the original spectra in the range of 600~4000 cm-1, and 92% cumulative variance contribution rate was obtained on the first two PCs. LDA analysis based on PCs generated from PCA analysis achieved 96.25% classification accuracy. Based on the confusion matrix of the predicted results as a comprehensive evaluation index, the average accuracy, recall rate and specificity of the PCA-LDA classification model were obtained as 96.25%, 96.59% and 99.48%, respectively, indicating that the PCA-LDA model can effectively discriminate the origin of quinoa. The study showed that infrared spectroscopy combined with multivariate statistical analysis method is an effective method to identify the geographical origin of quinoa.

    Key words: infrared spectroscopy; quinoa; origin identification; principal component analysis; linear discriminant analysis

    引用本文:嚴偉敏,劉剛,田雪,等. 藜麥產地的紅外光譜鑒別[J].化學試劑,2022,443):436-441.

     

     

    不同采收期水冬瓜葉的主成分分析及抗炎鎮痛譜效關系研究

     

    韓忠耀*,張濤,黃春麗,田浩,王萬樂,盧洋,王小建,羅浩

    (黔南民族醫學高等??茖W校 藥學系 ,貴州 都勻  558000

     

    摘要:為篩選水冬瓜葉抗炎鎮痛活性成分,采用高效液相色譜(HPLC)建立不同采收期10批次水冬瓜葉藥材指紋圖譜,對其進行主成分分析,并基于皮爾遜相關分析法探討不同采收期水冬瓜葉藥材抗炎鎮痛的譜效關系。結果顯示,不同采收期水冬瓜葉藥材HPLC指紋圖譜中有17個共有峰,10批次藥材的相似度為0.875 ~ 0.973。聚類分析將不同采收期水冬瓜葉藥材分為3類。主成分分析共得到3個主成分。經皮爾遜相關分析,峰17、峰14、峰12、峰15、峰13、峰5、峰16和峰4可能為水冬瓜葉藥材鎮痛作用的物質基礎,峰6、峰8(異槲皮苷)、峰11、峰7(金絲桃苷)、峰5、峰3、峰4、峰13、峰9和峰1可能為水冬瓜葉藥材抗炎作用的物質基礎。

    關鍵詞:水冬瓜葉;指紋圖譜;譜效關系;皮爾遜相關分析法;化學模式識別;抗炎鎮痛

    中圖分類號:O657.7;R285.5        文獻標識碼:A         文章編號: 0258-32832022

     

    Principal Component Analysis and Spectrum-effect Relationship of Anti-inflammatory and Analgesic of the Leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in Different Collecting Seasons HAN Zhong-yao, ZHANG Tao, HUANG Chun-li, TIAN Hao, LU Yang, WANG Wan-le, WANG Xiao-jian, LUO Hao(Department of Pharmacy, Qiannan Medical College for Nationalities, Duyun 558000, China), Huaxue Shiji, 2022,

    Abstract: In order to screen the anti-inflammatory and analgesic active components of the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu, high performance liquid chromatography (HPLC) was used to establish the fingerprints of 10 batches of the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in different collecting seasons, and the principal component analysis was carried out. Based on Pearson correlation analysis, the spectrum-effect relationship of anti-inflammatory and analgesic effects of the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in different collecting seasons was discussed. The results showed that there were 17 common peaks in the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in different collecting seasons, and the similarity of 10 batches of medicinal materials was 0.8750.973. Cluster analysis divided the medicinal materials of 10 batches of the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in different collecting seasons into three categories. Three principal components were obtained by principal component analysis. Pearson correlation analysis was used to calculate the correlation coefficient between each common peak and analgesic inhibition rate and anti-inflammatory swelling inhibition rate.The results showed that peak 17, peak 14, peak 12, peak 15, peak 13, peak 5, peak 16 and peak 4 may be the material basis of analgesic effect of the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in different collecting seasons, peak 6, peak 8 (isoquercitrin), peak 11, peak 7 (hyperin), peak 5, peak 3, peak 4, peak 13, peak 9 and peak 1 may be the material basis of anti-inflammatory effect of the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu in different collecting seasons.

    Key words: the leaves of Toricellia Angulata Oliv.var.intermedia (Harms) Hu; fingerprint; spectrum-effect relationship; person relational analysis; chemical components; anti-inflammatory and analgesic

    引用本文:韓忠耀,張濤,黃春麗,等. 不同采收期水冬瓜葉的主成分分析及抗炎鎮痛譜效關系研究[J]. 化學試劑,2022,443442-449.

     

     

    超聲輔助懸浮固化液液微萃取-液相色譜熒光法測定血清中阿齊沙坦

    龔愛琴*,姜業朝,陳娟,陳麗萍

    (揚州工業職業技術學院 化學工程學院,江蘇 揚州  225127

    摘要:建立一種懸浮固化分散液液微萃取-液相色譜熒光法測定血清中阿齊沙坦含量的新方法。在超聲輔助下,乳化后的萃取劑1-十一醇高效快速萃取溶液中的阿齊沙坦,將萃取液離心后冰水浴中冷卻,萃取劑凝固漂浮在水面而與溶液分離,分離后的1-十一醇用乙醇溶解后利用液相色譜熒光法測定其中阿齊沙坦的含量。實驗中對液相色譜測定條件、萃取條件進行了優化,包括激發與發射波長、流動相組成、萃取劑用量、萃取溶液pH、超聲時間、離心時間、冷卻時間等。在優化條件下,工作曲線的線性范圍為0.024.0 μg/mL,最低檢測限為6.0 ng/mL,回收率為93.1%100.4%。專屬性實驗及血清樣品測定結果表明該方法可以用于人血清中阿齊沙坦含量的測定。

    關鍵詞:阿齊沙坦;1-十一醇;液液微萃??;HPLC;熒光

    中圖分類號:O657. 7       文獻標識碼:A     文章編號:0258-32832022- -

     

    Ultrasound-assisted solidification of floating organic drop micro extraction coupled to high performance liquid chromatography with fluorescence detection for the determination of azilsartan in serum GONG Ai-qin*, JIANG Ye-chao, CHEN Juan, CHEN Li-ping (Chemical Engineering Institute, Yangzhou Polytechnic Institute, Yangzhou 225127, China), Huaxue Shiji, 2022, 44(3),

    Abstract: A new method of ultrasound-assisted solidification of floating organic drop micro extraction coupled to high performance liquid chromatography with fluorescence detection (HPLC-FLD) for the determination of azilsartan in serum was proposed. With the help of ultrasound, azilsartan could be extracted efficiently and rapidly into emulsified extractant 1-undecanol. After centrifugation, the solution was cooled at ice bath and 1-undecanol was solidified and floated on the water, which made 1-undecanol easily to separate from aqueous solution. Finally the azilsartan in 1-undecanol was dissolved in ethanol and measured by HPLC-FLD. In examination the chromatographic conditions and extraction conditions were studied and optimized, including excitation and emission wavelengths, composition of mobile phase, the volume of 1-undecanol, solution pH, ultrasonic time, centrifugation time, cooling time and so on. Under the optimized conditions, the calibration curve was linear over the range of 0.024.0 μg/mL, and the limit of detection (LOD) was 6.0 ng/mL. The average recoveries were between 93.1% and 100.4%. The results of specific experiment and serum sample determination indicated the studied method could be used to test azilsartan in human serum.

    Key words: azilsartan; 1-undecanol; Liquid-liquid micro extraction; HPLC; Fluorescence

    引用本文龔愛琴,姜業朝,陳娟,等. 超聲輔助懸浮固化液液微萃取-液相色譜熒光法測定血清中阿齊沙坦[J]. 化學試劑,2022,44(3):450-454。

     

     

    UPLC-MS/MS法測定食用植物油中15種全氟化合物

    張文*,閆君,陳婷,潘建忠,王行智,張新中

    (蘭州市食品藥品檢驗檢測研究院 國家市場監管重點實驗室(食品中農藥獸藥殘留監控) 甘肅省種植中藥材外源性污染物監測工程研究中心,甘肅 蘭州  730050)

     

    摘要:建立了UPLC-MS/MS同時測定食用植物油中15種全氟化合物(包括全氟烷基羧酸類、全氟磺酸類、全氟磺酰胺、全氟調聚醇)的檢測方法。采用ACQUITY UPLC BEH-C181.7 μm, 2.1 mm×100 mm)色譜柱,以5 mmol/L乙酸銨的5%甲醇水溶液和95%甲醇水溶液為流動相,梯度洗脫,流速為0.3 mL/min,質譜選擇多反應監測模式對15種全氟化合物進行定性和定量檢測。樣品采用1%甲酸乙腈重復提取兩次,提取液旋蒸蒸發至凈干,V(甲醇)V() = 32溶液復溶,14000 r/min離心除雜制得待測液,與QuEChERS方法比較,回收率高、操作簡單。結果顯示:15種全氟化合物在8 min內得到有效分離,線性相關性好,相關系數均大于0.9951,檢出限為0.02020.0365 μg/kg,定量限為0.06740.1217 μg/kg,1.5、3.0、4.5 μg/kg 3個添加濃度的平均回收率為63.5%101.3%,相對標準偏差為0.8%9.4%。本方法可應用于食用植物油中全氟化合物的檢測。

    關鍵詞:全氟化合物;液相色譜-質譜聯用儀;食用植物油;檢測;全氟羧酸;全氟磺酸;全氟磺酰胺;全氟調聚醇

    中圖分類號TS207;O657         文獻標識碼A     文章編號0258-32832022

     

    Determination of 15 Perfluorinated Compounds in Edible Vegetable Oil by UPLC-MS/MS ZHANG Wen*, YAN Jun, CHEN Ting, PAN Jian-zhong, WANG Xing-zhi, ZHANG Xin-zhong (Gansu Engineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines, Key Laboratory of Pesticide and Veterinary Drug Monitoring for State Market Regulation, Lanzhou Institute for Food and Drug Inspection and Testing, Lanzhou 730050, China), Huaxue Shiji, 2022, 44(3)

    AbstractA UPLC-MS/MS method was established for simultaneous determination of 15 perfluorinated compounds (including perfluorinated alkyl carboxylic acids, perfluorinated sulfonic acids, perfluorinated sulfonamides and perfluorinated telomers) in edible vegetable oils. An ACQUITY UPLC BEH-C18 (1.7 μm, 2.1 mm×100 mm) column was used for gradient elution with 5 mmol/L ammonium acetate in 5% methanol solution and 95% methanol solution as mobile phases at a flow rate of 0.3 mL/min. The mass spectrometry employs the multiple reaction monitoring mode for qualitative and quantitative determination of fifteen perfluorinated compounds. The sample was extracted by 1% formic acid acetonitrile twice, and the extract was rotary-evaporated to dryness, which was then redissolved by (3+2) methanol-aqueous solution, and centrifuged to remove impurities at 14000 r/min. Compared with QuEChERS method, the present process runs simply with high recovery rate. The results showed that fifteen perfluorinated compounds were effectively separated within 8 min with good linear correlation coefficients greater than 0.9951, the detection limits over the range 0.0202-0.0365 μg/kg, and the quantification limits in the region 0.0674-0.1217 μg/kg. The average recoveries of 1.5, 3.0 and 4.5 μg/kg were 63.5% to 101.3% with relative standard deviations (RSDs) of 0.8% to 9.4%. This method can be applied to the determination of perfluorinated compounds in edible vegetable oil.

    Key words: perfluorinated compound; liquid chromatograph-mass spectrometer; edible vegetable oil; detection; perfluorocarboxylic acid; perfluorinated sulfonic acid; perfluorinated sulfonamide; perfluorotelomeric alcohols

    引用本文:張文,閆君,陳婷,等. UPLC-MS/MS法測定食用植物油中15種全氟化合物[J]. 化學試劑, 2022, 44(3): 455-461。

     

     

    銻元素溶液標準物質的研制

    孫倩蕓1,呂鄧義2,高捷1,張森1,王云1,郭波*1

    1.山東省計量科學研究院,山東濟南250014;2.山東省食品藥品檢驗研究院,山東濟南250101

     

    摘要:為滿足銻元素檢測需求,研制了銻元素溶液標準物質。該標準物質以高純銻和MOS級硝酸為原料,在對高純金屬純度定值的基礎上,采用重量-容量法進行配制和定值。高純銻采用雜質扣除法測定其純度。采用ICP-MS半定量方法對雜質進行定性分析,通過電感耦合等離子體質譜法(ICP-MS)方法對金屬雜質進行準確測定,通過惰性氣體熔融-紅外吸收法、惰性氣體熔融-熱導法測定氣體雜質元素C、S、O、N、H。經過標準物質的均勻性檢驗和穩定性檢驗后,將配制值作為標準值,同時評定了所研制標準物質濃度定值的不確定度。結果證明,銻元素溶液標準物質的濃度為1000μg/mL,相對擴展不確定度為1%k=2)。

    關鍵詞:銻標準物質;金屬純度;雜質扣除法;電感耦合等離子體質譜法;不確定度

    中圖分類號:O657.6       文獻標識碼:A        文章編號:0258-32832022

     

    Development of Standard Reference Material for Antimony Solution SUN Qian-yun1, LV Deng-yi2, GAO Jie1, ZHANG Sen1, WANG Yun1, GUO Bo*11. Shandong Institute of Metrology, Jinan250014, China; 2. Shandong Institute of Food and Drug Testing, Jinan 250101, ChinaHuaxue Shiji, 2022, 44(3)

    AbstractTo meet the requirements of antimony detection, the standard reference material of antimony solution was developed. The standard reference material was prepared by using high-purity antimony and MOS grade acid as raw materials by weight-capacity method, and the purity of antimony was determined by impurity deduction method. The metal impurities were analyzed by ICP-MS semi-quantitative method and were accurately determined by inductively coupled plasma mass spectrometry ( ICP-MS ). The gas impurities C, S, O, N and H were determined by inert gas melting-infrared absorption method and inert gas melting-thermal conductivity method.  After the verifications of homogeneity and stability, the value of standard reference material was defined, and the uncertainty was estimated. The results confirmed that the concentration of antimony solution reference material was 1000 μg/mL, while the relative expanded uncertainty was 1%( k=2 ).

    KeywordsSRM of antimony; metal purity; impurity deduction; ICPMS; uncertainty

    引用本文:孫倩蕓,呂鄧義,高捷,等.銻元素溶液標準物質的研制[J].化學試劑,2022,44(3):462-467。

     

     

    芳香羧酸脫羧-偶聯反應研究

     

    鐘輝a,吳聰a,文旺a,丁陽a,周旭東a,b,盛文兵*a,b

    (湖南中醫藥大學 a. 藥學院,b. 中醫藥民族醫藥創新發展國際實驗室,湖南 長沙  410208

     

    摘要:芳香族羧酸脫羧-偶聯反應能夠有效構建C-CC-雜原子鍵,在天然活性物質、藥物中間體以及特殊材料合成等方面具有重要意義,并且該方法具有很好的區域選擇性、原子經濟性及環境友好性等特點。近年來以芳香羧酸為基本原料的脫羧-偶聯反應得到深入研究,新穎催化劑不斷涌現,反應條件不斷完善,為該類反應的應用提供了理論依據。從偶聯反應的類型、機理、不同過渡金屬催化劑等方面展開綜述,為進一步研究并開發該類反應提供參考。

    關鍵詞:芳香羧酸;脫羧-偶聯反應;過渡金屬催化;非金屬催化;紫外光催化;低共熔溶劑

    中圖分類號O621.29      文獻標識碼A      文章編號0258-32832022

     

    Study on the Decarboxylation-Coupling Reaction of Aromatic Carboxylic Acid ZHONG Huia, WU Conga, WEN Wanga, DING Yanga, ZHOU Xu-donga,b, SHENG Wen-bing*a,b (a. School of Pharmacy, b. TCM and Ethnomedicine Innovation & Development International Laboratory, Hunan University of Chinese Medicine, Hunan Changsha, 410208, China), Huaxue Shiji, 2022, 44(3),

    Abstract: The decarboxylation-coupling reaction of aromatic carboxylic acid can effectively construct C-C or C-heteroatomic bonds, which is of great significance in natural active substances, drug intermediates and special material synthesis, and the method has the characteristics of good regional selectivity, atomic economy and environmental friendliness. In recent years, the decarboxylation-coupling reaction with aromatic carboxylic acid has been deeply studied, and many novel catalysts are constantly emerging, providing a theoretical basis for the application of such reactions. In order to provide a meaningful reference for further research, coupling reaction type, mechanism and the different transition metal catalysts are summarized in this mini-review.

    Key words: aromatic carboxylic acids; decarboxylation-coupling reaction; catalyzed by metal

    引用本文:鐘輝,吳聰,文旺,等.芳香羧酸脫羧-偶聯反應研究[J].化學試劑,2022,44(3)468-476.

     

     

    N-芐基吲哚類熊果酸衍生物的合成及抗肝癌活性

    田寧1,劉曉娟2,張大軍1,欒天*1

    1. 沈陽醫學院 藥學院,遼寧 沈陽  110034;2. 阜新市產業技術研究院,遼寧 阜新  123000

     

    摘要:為開發高效低毒的抗肝癌天然產物衍生物,依據藥物拼合原理設計并合成了一系列未見文獻報道的熊果酸衍生物。將熊果酸與不同取代的N-芐基吲哚片段通過Claisen-Schmidt縮合反應得到目標化合物,其化學結構均經過核磁氫譜﹑核磁碳譜以及質譜的聯合確證。采用噻唑藍(MTT)法考察其體外抗肝癌活性,結果表明,2-{[1-2-氟芐基)-1H-吲哚基]-3-次甲基}-3-羰基熊果酸(4b)與2-{[1-3-氟芐基)-1H-吲哚基]-3-次甲基}-3-羰基熊果酸(4c)對HepG2BEL-7402兩種肝癌細胞株的抑制活性優于熊果酸及陽性對照藥氟尿嘧啶,同時對正常肝細胞L02的毒性顯著降低?;衔?/span>4c的體外抗肝癌活性最為理想(針對HepG2IC50值為3.22 μmol/L,選擇性指數為6.89),分子對接實驗模擬其作用靶標或為RNA聚合酶II,可對其深入研究用以開發高效低毒的抗肝癌藥物。

    關鍵詞:熊果酸;吲哚;衍生物;合成;抗肝癌

    中圖分類號:R914.5    文獻標識碼:A    文章編號:0258-32832022

     

    Synthesis and Anti-hepatocellular Carcinoma in Vitro of Ursolic Acid Derivatives Bearing N-benzylindole Moieties TIAN Ning1, LIU Xiao-juan2, ZHANG Da-jun1, LUAN Tian*1 (1. Department of Pharmacy, Shenyang Medical College, Shenyang 110034, China; 2. Fuxin Industrial Technology Research Institute, Fuxin 123000, China), Huaxue Shiji, 2022, 44(3)

    Abstract: To develop natural derivatives with high efficiency and low toxicity for anti-hepatoma, a series of novel ursolic acid derivatives were designed and synthesized via the principle of pharmacochemical molecular combination. The target compounds were obtained by Claisen-Schmidt condensation reaction between ursolic acid and different substituted N-benzylindole, then characterized via 1H-NMR, 13C-NMR, and mass spectrometry, and investigated for anti-hepatocellular activity by MTT method. (1S,2R,4aS,6aS,6bR,12aR,E)-11-((1-(2-Fluorobenzyl)-1H-indol-3-yl)methylene)-1,2,6a,6b,9,9,12a-heptamethyl-10-oxo-1,3,4,5,6,6a,6b,7,8,8a,9,10,11,12,12a,12b,13,14b-octadecahydropicene-4a(2H)-carboxylic acid (4b) and (1S,2R,4aS,6aS,6bR,12aR,E)-11-((1-(3-fluorobenzyl)-1H-indol-3-yl)methylene)-1,2,6a,6b,9,9,12a-heptamethyl-10-oxo-1,3,4,5,6,6a,6b,7,8,8a,9,10,11,12,12a,12b,13,14b-octadecahydropicene-4a(2H)-carboxylic acid4cshowed higher antiproliferative activity against the HepG2 and BEL-7402 cell lines in comparison with the positive-control drug 5-fluorouracil and ursolic acid, and exhibited significantly lowered cytotoxic activities against human normal liver cells (L02). Compound 4c exhibited the most potent antiproliferative activity and commendable selectivity between cancer and normal cells (IC50 = 3.22 μmol/L against the HepG2 cells, Selectivity index = 6.89). The results of a docking study that involved placing compound 4c into the RNA polymerase II binding site revealed that its mode of action was possibly as a RNA polymerase II inhibitor. In conclusion, compound 4c may be a valuable candidate for further studies aiming at the development of effective and harmless anti-hepatoma drugs.

    Key words: ursolic acid; benzpyrole; derivatives; synthesis; anti-hepatoma

    引用本文:田寧,劉曉娟,張大軍,等. N-芐基吲哚類熊果酸衍生物的合成及抗肝癌活性[J]. 化學試劑,2022,443477-483。

     


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