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    《化學試劑》2022年第5期中英文摘要(附整期文章PDF文檔)

    發布時間: 2022-05-13 16:56:38   試劑信息網

    基于氟硼二吡咯亞甲基熒光探針的研究進展

    朱金彪,閆力強*,吳雄志*

    (桂林理工大學 化學與生物工程學院,廣西 桂林  541006

     

    摘要氟硼二吡咯亞甲基BODIPY)熒光染料具有易于修飾、高摩爾消光系數、高熒光量子產率、優異的光穩定性、對溶劑的極性和pH敏感性低等許多突出特性,被廣泛用于有機小分子熒光探針的構建。綜述了2019年以來BODIPY熒光探針在金屬陽離子、陰離子、活性氧和生物硫醇等檢測方面的研究進展,梳理了這些探針的設計思路,對比了它們的檢測性能,并展望和預測了該類熒光探針的發展趨勢,為新型BODIPY熒光探針的設計與開發提供參考。

    關鍵詞氟硼二吡咯;熒光探針;金屬陽離子;陰離子;活性氧;研究進展

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

     

    Progress of Fluorescent Probes Based on Fluoroborane Dipyrromethene ZHU Jin-biao, YAN Li-qiang*, WU Xiong-Zhi* (College of Chemistry and Bioengineering, Guilin University of Technology, Guilin 541006, China), Huaxue Shiji, 2022, 44(5),

    Abstract: Fluoroborondipyrromethene (BODIPY) dye hasa lot of prominent properties, such as easy modification, high molar extinction coefficient and fluorescence quantum yield, good photostability, low sensitivity to solvent polarity and pH, which has been widely used as a fluorophore in the construction of organic small molecule fluorescent probes. In this work, the progresses of BODIPY-based fluorescent probes in the detections of metal cations, anions, reactive oxygen species (ROS) and thiols since 2019 were reviewed, the design ideas and detection performances, and predict the development trend also were summarized. This review may provide an inspiration for the design and development of new BODIPY-based fluorescent probes.

    Key words: fluoroboron dipyrromethene; fluorescent probe; metal cations; anions; reactive oxygen species; research progress

    引用本文朱金彪,閆力強,吳雄志. 基于氟硼二吡咯亞甲基熒光探針的研究進展[J]. 化學試劑,2022,44(5):633-642。

     

     

    核取代萘二酰亞胺衍生物超分子自組裝體系的研究進展

    仇中選1,張娟2,辛飛飛*3

    (1. 青島職業技術學院 生物與化工學院,山東 青島  230031;2. 中國石油大學(北京) 非常規油氣科學技術研究院,北京  102249;3. 青島科技大學 化學與分子工程學院,山東 青島  266042)

     

    摘要超分子自組裝是體系中各結構單元之間的一種自發的組織行為,能夠形成納米級或者微米級的微結構,可用于制備具有特定性質以及功能化的材料。核取代萘二酰亞胺衍生物(cNDIs)因其獨特的結構特點與光電性能,是超分子自組裝體系中一類重要的構筑基元,在超分子化學領域以及材料科學領域等表現出極大的應用價值。如何提高cNDIs超分子組裝體的結構與性能調控效率,拓展其功能,促進其實際應用是現階段的主要研究熱點。綜述結合國內外cNDIs自組裝體系的文獻報道,總結并闡述了調控cNDIs分子自組裝行為的三種主要方式:設計cNDIs分子結構,改變體系環境,使用模板。最后,對該類超分子體系的研究方向與發展趨勢進行了簡要展望。

    關鍵詞核取代萘二酰亞胺;超分子化學;可調控;自組裝;微觀結構

    中圖分類號:O641.3    文獻標識碼:A       文章編號:0258-32832022

     

    Supramolecular Self-assembly of Core Substituted Naphthalenediimides QIU Zhong-xuan1, ZHANG Juan2, XIN Fei-fei*3 (1. School of Biological and Chemical Engineering, Qingdao Technical College, Qingdao 266555, China; 2. Unconventional Petroleum Research Institute, China University of Petroleum, Beijing 102249, China; 3. College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042, China), Huaxue Shiji, 2022, 44(5),

    AbstractSupramolecular self-assembly rests on the spontaneous organization of components and forms various micro- or nanostructures to prepare functional materials with unique properties. Core-substituted naphthalenediimides (cNDIs) which possess unique molecular structures and opto-electrical properties are widely employed in supramolecular chemistry. Now, the main researches on cNDIs-based supramolecular assemblies include: increasing the modulation efficiency of microstructures and properties; extending the functionalities and promoting the applications. This work reviews the recent progress in supramolecular self-assemblies based on cNDIs. Three main modulating patterns of self-assemblies: we summarized including the design of cNDIs molecular structures, changing external environment and templated self-assembly. Finally, the development potential of this field is briefly discussed.

    Key words: core-substituted naphthalenediimides; supramolecular chemistry; controllable; self-assembly; microstructures

    引用本文:仇中選,張娟,辛飛飛. 核取代萘二酰亞胺衍生物超分子自組裝體系的研究進展[J]. 化學試劑, 2022, 44(5):643-652。

     

     

    堿土金屬配合物催化丙交酯開環聚合的研究

    劉娜1,由曉蕾1,王玲芳2,張金策1,魏杰*1,房大維*1

    1. 遼寧大學 稀散元素化學研究所,遼寧 沈陽  110036;2. 鹽城工學院 材料科學與工程學院,江蘇 鹽城 224051

     

    摘要良好的生物相容性和生物可降解性使得聚丙交酯各個領域廣泛應用,而聚丙交酯的性能是由其微觀結構決定,因此開發高效的催化體系催化丙交酯開環聚合制備結構精確可控的聚丙交酯具有非常重大的意義。堿土金屬Ca/Sr/Ba配合物其無毒、生物相容性和環境友好等優點被廣泛應用于催化反應中,尤其在催化環酯類單體開環聚合方面表現出優催化活性。為了更清楚地了解堿土金屬配合物性質,近十年來不同配體、不同中心金屬組成的堿土金屬催化劑合成,以及其在丙交酯開環聚合中催化活性、可控性和立體選擇性進行了綜述,并對其應用前景作出了高度展望。

    關鍵詞鈣配合物;鍶配合物;鋇配合物;丙交酯;開環聚合

    中圖分類號:O631      文獻標識碼:A      文章編號:0258-32832022- -

     

    Ring-opening Polymerization of Lactide Catalyzed by Alkaline Earth Metal Complexes LIU Na1, YOU Xiao-lei1, WANG Ling-fang2, ZHANG Jin-ce1, WEI Jie*1, FANG Da-wei*1 (1. Institute of Rare and Scattered Elements Chemistry, Liaoning University, Shenyang 110036, China; 2. School of Materials Science and Engineering, Yancheng Institute of Technology, Yancheng 224051, China), Huaxue Shiji, 2022, 44(5),

    Abstract: Polylactides (PLAs) have been widely used in various fields due to its good biocompatibility and biodegradability. The microstructure of PLA governs the properties of polymers. Therefore, it is of great significance to establish an efficient catalytic system to catalyze the ring-opening polymerization (ROP) of lactide to prepare PLA with a precise and controllable structure. Alkaline earth metal (Ca/Sr/Ba) complexes have attracted much attention of researchers due to their non-toxicity, biocompatibility and environmental friendliness. To understand the property of these complexes, it covers the latest research progress about the application of alkaline earth metal catalysts in the ROP of lactide since 2010 in this work. Meanwhile, a high prospect for their applications was also maken.

    Key words: calcium complexes; strontium complexes; barium complexes; lactide; ring-opening polymerization

    引用本文劉娜,由曉蕾,王玲芳,等. 土金屬配合物催化丙交酯開環聚合的研究[J]. 化學試劑,2022,44(5):563-661。

     

     

    兩種河南產迷迭香精油成分分析及抗氧化活性研究

    葉兆偉1,李金平2,葉潤1,李琪琪1,陳瓊*1

    1. 信陽農林學院 制藥工程學院,河南 信陽 464000;2. 河南息半夏藥業有限公司,河南 信陽 464000

     

    摘要:為了鑒別和研究迷迭香生長習性及其精油組成特點,以生長在河南信陽的種迷迭香綠色窄葉、寬葉為研究對象,考察其生物學性狀,并利用氣相-質譜儀(GC-MS)分析了精油的化學成分;以清除羥基自由基(·OH)能力為指標,考察當地迷迭香精油的抗氧化活性。結果表明,當地窄葉迷迭香精油主要成分包括桉葉素(29.826%)、(1S)-1,7,7-三甲基-雙環[2.2.1]-2-酮(18.939%)、γ-松油烯(8.051%)、冰片(7.434%)、莰烯(5.542%);寬葉迷迭香精油主要成分有(1R)-2,6,6-三甲基二環[3.1.1]-2-烯(28.141%)、桉葉素(23.076%)、(1S)-4,6,6-三甲基二環[3.1.1]-3--2-酮(9.758%)、冰片(6.244%)、莰烯(4.833%)等。此種迷迭香精油在11.8 mg/mL濃度范圍內,羥基自由基清除率變化呈線性上升趨勢,當精油濃度為1.8 mg/mL時,窄葉迷迭香精油對羥基自由基清除率達到90.33%,寬葉迷迭香精油羥基自由基清除率達到87.06%;窄葉、寬葉迷迭香品種不同,精油含量及成分有差別,窄葉精油對羥基自由基清除能力比相同濃度下寬葉精油的清除能力強,精油的清除能力均好于維生素CVc)。

    關鍵詞:迷迭香;精油;GC-MS;羥基自由基;抗氧化

    中圖分類號:R284.1      文獻標識碼:A      文章編號:0258-32832022--

     

    Composition Analysis and Antioxidant Activity of Two Essential Oils from Rosemary officinalis in Henan YE Zhao-wei1, LI Jin-ping2,YE Run1, LI Qi-qi1,  CHEN Qiong*1 (1. Xinyang Agriculture and Forestry University, School of biology and pharmaceutical engineering, Xinyang 464000, Henan China;2. Henan Xibanxia Co., Ltd, Xinyang 464000, Henan China) Huaxue Shiji, 2021, 44(5),

    Abstract: To identify and obtain the growth habit and essential oil composition of rosemary officinalis, the biological characters of two kinds of green leaf between narrow and wide rosemary officinalis grown in Xinyang, Henan Province were investigated. The chemical components of the essential oil were analyzed by gas chromatography-mass spectrometry (GC-MS). The antioxidative activity of rosemary officinalis essential oil was investigated with the ability of scavenging hydroxyl free radical (·OH) as an index. The main components of essential oil from local narrow rosemary officinalis include Eucalyptus (29.826%), (1S) -1,7,7- three methyl - bicyclic [2.2.1] Geng -2- ketone (18.939%).γ- Terpinene (8.051%), borneol (7.434%), camphene (5.542%); The main components of Rosmarinus officinalis essential oil are: (1R) -2,6,6- three methyl bicyclic [3.1.1] heptane -2- (28.141%), Eucalyptus (23.076%), (1S) -4,6,6- three methyl bicyclic [3.1.1] heptane -3- ene -2- ketone (9.758%), borneol (6.244%), and borneol (4.833%). The scavenging rate of hydroxyl radical in the two kinds of rosemary officinalis essential oils increased linearly in the concentration range of 11.8 mg/mL. When the concentration of essential oil was 1.8 mg/mL, the scavenging rate of rosemary officinalis essential oil to hydroxyl radical reached 90.33%, and the scavenging rate of hydroxyl radical of Rosmarinus officinalis essential oil reached 87.06%. The content and composition of essential oil are different in different varieties of narrow and wide leaf rosemary officinalis. The scavenging ability of narrow leaf essential oil is stronger than that of wide leaf essential oil at the same concentration, and the scavenging ability of essential oil is better than vitamin C (VC).

    Key words: rosemary officinalis; essential oil; GC-MS; Hydroxyl radical; antioxidant ability

    引用本文:葉兆偉,李金平,葉潤,等. 兩種河南產迷迭香精油成分分析及抗氧化活性研究[J]. 化學試劑, 2022, 44(5): 662-667。

     

     

    2-三氟甲基喹唑啉衍生物的合成及抗腫瘤活性研究

    吳輝a,b,c,余佳a,c,余剛a,c,曾曉萍a,c,徐廣燦a,c,徐必學*a,c

    (貴州醫科大學 a. 省部共建藥用植物功效與利用國家重點實驗室,b. 藥學院,c. 貴州省中國科學院天然產物化學重點實驗室, 貴州 貴陽  550014)

     

    摘要設計合成新型2-三氟甲基喹唑啉類化合物,以期發現高效低毒的抗腫瘤活性目標分子。2-氨基-5-硝基苯甲酸為原料,經過三氟乙?;?、環化、氯代及偶聯等反應,設計合成102-三氟甲基喹唑啉類化合物,并通過1H NMR、13C NMR、19F NMR進行結構確證。采用四氮唑藍MTT)法評價目標化合物的體外抗腫瘤活性,合成的大部分目標化合物對前列腺癌細胞(PC3、LNCaP)、人慢性髓系白血病細胞(K5623種癌細胞都有一定的抑制作用,其中,N-4-甲氧基苯基)-N-甲基-2-(三氟甲基)喹唑啉-4,6-二胺(5a)的IC50分別為25.2PC3)、515.7LNCaP)和248.7 nmolK562),該結果為2-三氟甲基喹唑啉類化合物在抗腫瘤方面的進一步研究提供參考。

    關鍵詞喹唑啉;三氟甲基;合成;MTT法;抗腫瘤活性

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

     

    Synthesis and Antitumor Activity of 2-Trifluoromethylquinazoline Derivatives WU Huia,b,c, YU Jiaa,c, YU Ganga,c, ZENG Xiao-pinga,c, XU Guang-cana,c, XU Bi-xue*a,c (a. State Key Laboratory of Functions and Applications of Medicinal Plants, b. School of Pharmaceutical Sciences, c. Key Laboratory of Chemistry for Natural Products of Guizhou and Chinese Academy of Sciences, Guizhou Medical University, Guiyang 550014, China), Huaxue Shiji, 2022, 44(5)

    Abstract: To discover high efficiency and low toxicity target compounds, ten novel derivatives of 2-trifluoromethylquinazoline were designed and synthesized from 2-amino-5-nitrobenzoic acid by trifluoacylation, cyclization, chlorination and coupling reaction. The structures of all target compounds were confirmed by 1H NMR, 13C NMR, 19F NMR and their anti-tumor activities in vitro were demonstrated by MTT assays. Most of them have a certain inhibitory activity against prostate cancer cell lines (PC3, LNCaP), human chronic myeloid leukemia cell line (K562). The half maximal inhibitory concentration values of compound N-(4-Methoxyphenyl)-N-methyl-2-(trifluoromethyl)quinazoline-4,6-diamine (5a) against PC3, LNCaP and K562 cell lines are 25.2, 515.7 and 248.7 nmol, respectively. The results could provide reference for further investigation of the derivatives of 2-trifluoromethylquinazoline as antitumor agents.

    Key words: quinazoline; trifluoromethyl; synthesis; MTT assays; antitumor activity

    引用本文:吳輝, 余佳, 余剛, . 2-三氟甲基喹唑啉衍生物的合成及抗腫瘤活性研究[J]. 化學試劑, 2022, 44(5): 668-673。

     

     

    紅景天內生微生物代謝產物化感作用研究

    劉香余,唐小淵,章煜,黃丹葉,陳愉,鄭渝,齊智敏,盧軒*

    (大連大學 生命科學與技術學院,遼寧 大連  116622)

     

    摘要:研究紅景天內生菌Fusarium sp. HJT-P-5代謝產物。采用薄層層析色譜(TLC)、正/反相柱色譜、凝膠柱色譜、以及高效液相色譜(HPLC)等多種現代分離技術對HJT-P-5代謝產物進行分離純化,結合理化性質核磁共振波譜數據進行結構鑒定。從HJT-P-5乙酸乙酯萃取物中分離得到4個單體化合物,選取模式植物擬南芥對分離得到的單體化合物進行活性評價。結果表明,高濃度的4個化合物均降低擬南芥平均根長和平均鮮重,證明植物衰敗凋落后,紅景天內生菌代謝產物累積達到一定程度后,進而抑制其他植物的生長,從而提高自身的生態競爭能力,具備開發成除草劑的潛力。

    關鍵詞紅景天;內生菌;活性評價;次級代謝產物;除草劑

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

     

    Metabolites of Fusarium sp. HJT-P-5 LIU Xiang-yu, TANG Xiao-yuan, ZHANG yu, HUANG Dan-ye, CHEN Yu, ZHENG Yu, QI Zhi-min, LU Xuan* (School of College of Life Science and Technology, Dalian University, China) Huaxue Shiji, 2022, 44(5),

    Abstract: Using thin layer chromatography (TLC), normal/reverse phase column chromatography, gel column chromatography, and high performance liquid chromatography (HPLC) and other modern separation techniques to separate and purify HJT-P-5 metabolites. The structure was confirmed by various techniques such as nature, ultraviolet spectroscopy, nuclear magnetic resonance, mass spectrometry, etc. Four monomer compounds were isolated from the ethyl acetate extract of HJT-P-5, and the model plant Arabidopsis thaliana was selected to evaluate the activity of the isolated monomer compounds. The four compounds at high concentrations all reduced the average root length and average fresh weight of Arabidopsis thaliana. This work proved from the side that the endophytic microbial metabolites can promote plant seed germination and biomass accumulation; after plant decay, Rhodiola rosea after the accumulation of metabolites of bacteria in the days reaches a certain level, they can inhibit the growth of other plants, thereby improving their own ecological competitiveness. This work provides new ideas and basis for solving the problem of Rhodiola rosea resources.

    Key words: Rhodiola; endophytes; biological activity; secondary metabolites; heibicide

    引用本文:劉香余,唐小淵,章煜,等. 紅景天內生微生物代謝產物化感作用研究[J]. 化學試劑,2022,44(5):674-678。

     

     

    金屬-有機框架在離子電容器中的應用與研究

    林瑋昆,史曉艷*,孫志鵬*

    廣東工業大學 材料與能源學院,廣東 廣州 510006

     

    摘要:離子電容器作為一種新型儲能器件,其兼具了超級電容器的大功率密度與電池的高能量密度的特性,在便攜式電子產品和混合動力電動汽車等儲能領域中有著廣泛的應用前景。作為離子電容器的核心組件,其電極材料的性能直接決定了整個器件的性能。因此,為進一步推動離子電容器的發展,開發出性能優異的電極材料勢在必行。其中,金屬-有機框架材料MOFs由于其具有大比表面積、高孔隙率、孔道規則且可調、結構和功能可設計性強等特點,MOFs及其衍生物被廣泛應用于儲能領域。本文將重點綜述MOFs及其衍生物作為離子電容器電極材料的應用研究,討論MOFs在應用于離子電容器電極材料時的電化學特性及其改性策略,為設計合成新型性能優異的MOFs基離子電容器電極材料提供理論依據和參考。

    關鍵詞離子電容器;金屬-有機框架;電極材料;復合材料;電化學

    中圖分類號:TM53      文獻標識碼:A       文章編號:0258-32832022--

     

    Research Progress on Metal-Organic Framework for Hybrid Ion CapacitorsLIN Wei-kun1, SHI Xiao-yan*1, SUN Zhi-peng*1(School of Materials and Energy, Guangdong University of Technology, Guangzhou 510006,China) , Huaxue Shiji,2022,44(5),

    Abstract: As a hybrid energy storage device, hybrid ion capacitors (HICs) combine the advantages such as high power density of supercapacitors and high energy density of batteries. Therefore, they are believed to have a wide application prospect in portable electronic products, hybrid electric vehicles, and many other energy storage fields. As the core component of the HICs, the electrochemical properties of electrode materials have a direct impact on the performance of the whole device. Thus, it is an urgent task to develop excellent electrode materials for improving the overall performance of HICs. Metal-organic framework materials (MOFs) are coordination polymers with ordered pore structures formed by coordination bonds between organic ligands and metal ions or clusters. The features such as possessing large specific surface area, high porosity, regular and adjustable channels, and strong designability of MOFs and their derivatives make them desirable electrode materials for energy storage areas. More recently, they are studied as electrode materials of HICs, and excellent performance is obtained. This paper reviews the applications of MOFs and their derivatives as electrode materials for HICs.

    Key words: hybrid ion capacitors; metal-organic frameworks; electrode materials; composite materials; electrochemistry

    引用本文:林瑋昆,史曉艷,孫志鵬. 金屬-有機框架在離子電容器中的應用與研究 [J]. 化學試劑, 2022, 44(5):679-690。

     

     

    基于鋅-MOF衍生自摻雜氮多孔炭在超級電容器中的研究

    黃思赟1*,李帥1,丁萬1,王一2

    (1. 貴州應用技術職業學院,貴州 福泉  550500;2. 貴州大學 大數據與信息工程院,貴州 貴陽  550025)

     

    摘要:通過簡單的水熱法工藝制備鋅-MOF并調節炭化溫度得到自摻雜氮多孔炭ZBTC-T,通過X射線衍射(XRD)、X射線光電子能譜(XPS)、氮氣吸附曲線、掃描電子顯微鏡(SEM)和透射電子顯微鏡(TEM)對自摻雜氮多孔ZBTC-T的結構進行了表征,說明了微觀結構和宏觀性能之間的關系。自摻雜氮多孔炭ZBTC-T結合了金屬和炭的優勢以及保留鋅-MOF中的氮原子從而展現出優異的電化學性能,自摻雜氮多孔炭ZBTC-850具有7.98%的高含氮量和735.42 cm2/g的比表面積,在電流密度為1.0 A/g,具有212.9 F/g的優異比電容,經過5000次充放電循環中保持其原始值85.04%,突出良好的倍率性能優勢并在高性能方面表現出廣闊的應用前景。

    關鍵詞:-MOF;自摻雜氮多孔炭;電化學性能;超級電容器

    中國分類號:O646         文獻標識碼:A       文章編號:0258-32832022--

     

    Research on the Application of Zinc-based MOF Derived from Nitrogen-doped Porous Carbon in Supercapacitors HUANG Si-yun*1, LI Shuai 1, DING Wan 1, WANG Yi 2 (1. Guizhou Vocational Institute of Applied Technology, Fuquan 550500, China; 2. College of Big Data and Information Engineering, Guizhou University, GuiYang 550025, China), Huaxue Shiji, 2022, 44(5),

    AbstractSelf-doped nitrogen porous carbon (ZBTC-T) with high surface areas were easily synthesized from a Zn-based metal-organic framework (MOF) by hydrothermal method. Structure and performance were carefully studied by XRD, XPS, BET surface area method, scanning electron microscopy and high resolution transmission electron microscopy. Self-doped nitrogen porous carbon ZBTC-T combines the advantages of metal and carbon and retains nitrogen atoms in zinc MOF, showing excellent electrochemical properties, the surface area and nitrogen content of the ZBTC-850 was found to be 735.42 cm2/g and 7.98%. The electrochemical properties of self-doped nitrogen porous carbon (ZBTC-T) were evaluated by using cyclic voltammetry and galvanostatic charge-discharge studies and the specific capacitance as high as 212.9 F/g in 6 mol/L KOH electrolyte. The system showed excellent cyclability and broad application prospects with a efficiency of 85.04% at a high current density of 1.0 A/g for 5000 cycles.

    Key words: zinc-MOF; self-doped nitrogen porous carbon; electrochemical performance; supercapacitor

    引用本文:黃思赟,李帥,丁萬,. 基于鋅-MOF衍生自摻雜氮多孔炭在超級電容器中的研究[J]. 化學試劑,2022,445691-696。

     

     

    ZIF-8@SAPb(II)吸附性能和機理研究

    付秋平,張海潤,石登紅,婁杰,莫昌琍,羅軍,嚴偉*

    貴陽學院 化學與材料工程學院,貴州 貴陽  550005

     

    摘要:海藻酸鈉Sodium Alginate, SA為前驅體,將沸石咪唑骨架材料ZIF-8加入SA中,制備出ZIF-8@SA復合材料,并研究了ZIF-8@SAPb(II)吸附性能。探討了接觸時間、Pb(II)初始濃度、吸附劑用量、溫度和吸附-脫附次數等因素ZIF-8@SA吸附Pb(II)效果的影響。對吸附過程進行了吸附等溫線、吸附動力學和吸附熱力學分析。結果表明,等溫吸附過程符合Langmuir模型,303.15 K時,Langmuir模型擬合得到的理論最大吸附量為330.364 mg/g。吸附動力學過程符合擬二級動力學模型。熱力學分析表明,ZIF-8@SAPb(II)吸附過程是自發的、吸熱的。ZIF-8@SAPb(II)具有很好的吸附效果。

    關鍵詞ZIF-8;海藻酸鈉;吸附;Pb(II);水處理

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

     

    Adsorption Performance and Mechanism of ZIF-8@SA for Pb(II) FU Qiu-ping, ZHANG Hai-run, SHI Deng-hong, LOU Jie, MO Chang-li, LUO Jun, YAN Wei* (College of Chemistry and Materials Engineering, Guiyang University, Guiyang 550005, China), Huaxue Shiji, 2022, 44(5),

    Abstract: In this work, sodium alginate, SA, was used as the precursor, ZIF-8 was added into SA to prepare ZIF-8@SA composites, and the adsorption performance of ZIF-8@SA for Pb(II) was investigated. The influences of contact time, initial concentration of Pb(II), dosage of adsorbent, temperature and adsorption-desorption times on the adsorption of Pb(II) by ZIF-8 SA were discussed. The adsorption process was analyzed by adsorption isotherm, adsorption kinetics and adsorption thermodynamics. The isothermal adsorption process was in accordance with the Langmuir model, and the theoretical maximum adsorption amount was 330.364 mg/g at 303.15 K. The adsorption kinetic process conforms to the pseudo-second-order kinetic model. Thermodynamic analysis shows that the adsorption of Pb(II) by ZIF-8@SA is a spontaneous endothermic process. The adsorption efficiency of Pb(II) by ZIF-8@SA is very high.  

    Key words: ZIF-8; sodium alginate; adsorption; Pb(II); water treatment

    引用本文付秋平, 張海潤, 石登紅, . ZIF-8@SAPb(II)吸附性能和機理研究[J]. 化學試劑, 2022, 44(5)697-702.

     

     

    碳納米管表面分子印跡聚合物的制備及固相萃取韭菜中呋喃丹

    張文驥*1,耿廣軍2

    1. 中國刑事警察學院 刑事科學技術學院 ,遼寧 沈陽 110035;2. 沈陽市公安局交警支隊,遼寧 沈陽 110000

     

    摘要:以羧基化修飾的多壁碳納米管為分散載體、丙烯酸(MAA)為功能單體、三羥甲基丙烷三甲基丙烯酸酯(TRIM)為交聯劑,采用交聯法在多壁碳納米管表面合成對呋喃丹具有特異性識別的分子印跡聚合物(MWNT-MIPs),并用掃描電鏡(SEM)、透射電鏡(TEM)、傅里葉變換紅外(FT-IR)光譜和熱重分析(TGA)等對該印跡聚合物進行表征。結果表明,所制備的呋喃丹分子印跡聚合物可接枝于碳納米管表面。聚合物的平衡吸附量可達113.5 μg/mg,吸附效果優于其非印跡材料和普通分子印跡材料,且對呋喃丹的吸附效果具有特異性。在10.05 mg/kg添加水平內,韭菜中呋喃丹的回收率為89.7%93.2%,優于相同質量的MIP柱。相對標準偏差(RSD)在3.2%4.8%之間,檢出限(LOD)為0.15 mg/kg。采用呋喃丹MWNT-MIPs為填料的SPE法是測定韭菜中呋喃丹殘留是一種很好的樣品的前處理方法。

    關鍵詞:呋喃丹;多壁碳納米管;分子印跡;韭菜;殘留

    中圖分類號R917      文獻標識碼:A      文章編號:0258-32832022--

     

    Preparation of Surface Molecularly Imprinting Polymers on Multi-Walled Carbon Nanotubes and Solid Phase Extraction of Carbofuran from Leek ZHANG Wen-ji*1, GENG Guang-jun2 (1.School of Forensic Sciences, Criminal Investigation Police University of China, Shenyang 110035,China; 2.Traffic Police Detachment of Shenyang Public Security Bureau, Shenyang 110000, China), Huaxue Shiji, 2022, 44(5),

    Abstract: A novel molecularly imprinted polymers (MIPs) based on multi-walled carbon nanotubes (MWNTs) was synthesized using carbofuran as template, methacrylic acid (MAA) as functional monomer, and trimethylolpropane trimethacrylate (TRIM) as cross-liking agent, and was confirmed using SEM, TEM, FT-IR and TGA. The carbofuran MIPs have been successfully grafted onto the surface of MWNTs as a thin layer with high stability. The results of absorption capacity test showed that the synthesized MWNT-MIPs displayed good selective recognition to carbofuran with equilibrium adsorption of 113.5 μg/mg. The MWNT-MIPs showed superior absorption performance to MWNT-NIPs and MIPs, and specific recognition to carbofuran. The recovery of carbofuran was within the range from 89.7% to 93.2%, when carbofuran was added to the leeks sample at the level of 10.05 mg/kg, higher than the MIP column. The RSD was within 3.2%4.8% and the LOD was 0.15 mg/kg. The method using carbofuran MWNT-MIPS as SPE filler is an applicable method for the determination of carbofuran residues in leeks

    Key words: carbofuran; multi-walled carbon nanotubes; molecularly imprinting; leeks; residue

    引用本文:張文驥,耿廣軍.碳納米管表面分子印跡聚合物的制備及固相萃取韭菜中呋喃丹[J]. 化學試劑,2022,44( 5): 703-709。

     

     

    CeO2改性水熱炭對厭氧發酵體系H2S減量研究

    張凱1,2,韋秀麗*1,李平1,蔣滔1,劉科1

    (1. 重慶市農業科學院 農業工程研究所,重慶 401329;2. 重慶大學 環境與生態學院,重慶 400045)

     

    摘要:以人糞渣為原料,通過微波水熱法在1.8 MPa條件下制備CeO2改性水熱炭,研究改性水熱炭對新鮮牛糞厭氧發酵過程中H2SCH4產量的影響。結果表明,當CeO2摻雜量為30%的水熱炭投加量為0.65 g/g牛糞固體時,H2S的產量較未添加復合物時降低了88.09%,而CH4的產生量并未發生明顯變化,這可能與不同活性位點的相互競爭、正負電荷相互作用以及改性水熱炭對硫的吸附、氧化和沉淀有關。由此可見,CeO2/水熱炭能夠在不影響CH4產量的情況下實現H2S減量,對緩解厭氧發酵系統管道腐蝕,維持厭氧發酵系統的穩定運行具有積極影響。

    關鍵詞:CeO2改性;微波水熱炭;厭氧發酵;H2S減量

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

     

    CeO2 Modified Hydrochar and Application in H2S Reduction of Anaerobic Fermentation System ZHANG Kai1,2, WEI Xiu-li*1, Li Ping1, JIANG Tao1, LIU Ke1 (1. Institute of Agricultural Engineering, Chongqing Academy of Agricultural Sciences, Chongqing 401329, China; 2. College of Environment and Ecology, Chongqing University, Chongqing 400045, China), Huaxue Shiji, 2022, 44(5),

    Abstract: CeO2 modified hydrochar was prepared from human fecal residue by microwave hydrothermal method at 1.8 MPa. The effect of modified hydrochar on the yield of H2S and CH4 in the anaerobic fermentation of fresh cow feces was investigated. When the dosage of hydrothermal carbon with 30% CeO2 doping is 0.65g/g cow dung solid, the yield of H2S decreased by 88.09% compared with that without complex, but the yield of CH4 did not change significantly. This may be related to the competition of different active sites, the interaction of positive and negative charges, and the adsorption, oxidation and precipitation of sulfur by modified hydrochar. CeO2/ hydrochar can reduce H2S without affecting CH4 production, which has a positive impact on alleviating pipeline corrosion of anaerobic fermentation system and maintaining stable operation of anaerobic fermentation system.

    Key words: CeO2 modification; microwave hydrochar; anaerobic fermentation; H2S reduction

    引用本文:張凱,韋秀麗,李平,等. CeO2改性水熱炭對厭氧發酵體系H2S減量研究[J]. 化學試劑,2022,44(5): 710-714。

     

     

    一種BAPTA熒光探針的合成、光譜性能與識別機制

     

    成昭,鄭蕾,徐玥*,何昊

    西安醫學院 藥學院,陜西 西安  710021

     

    摘要:以苯乙烯類發色團苯并咪唑作為熒光基團、多羧酸受體作為識別基團,基于分子內電荷轉移機制定向構筑探針結構,合成得到一種對Zn2+、Cu2+、Hg2+具有響應的熒光探針。定性及定量識別實驗顯示,探針對目標物Zn2+、Cu2+、Hg2+表現特征響應,探針與目標物11定量結合,熒光性能隨pH、時間變化而相對穩定、線性關系良好,能夠用于μmol/L濃度范圍目標離子的定性檢測和定量分析。此外,通過熒光、紫外等光譜學手段與核磁分析,初步闡明了探針對Cu2+、Hg2+Zn2+的不同識別機制,對于探針結構優化與性能篩選研究提供了依據。

    關鍵詞熒光探針;多羧酸受體;識別機制;熒光響應;合成

    中圖分類號O622.6        文獻標識碼:A        文章編號:0258-32832022--

     

    Synthesis, Spectral Properties and Recognition Mechanism of A BAPTA Fluorescent Probe CHENG Zhao, ZHENG Lei, XU Yue*, HE Hao (School of Pharmacy, Xi’an Medical University, Xi’an 710021, China), Huaxue Shiji, 2022, 44(5),

    Abstract: Based on the recognition mechanism of intramolecular charge transfer, a fluorescent probe for the detection of aqueous Cu2+/Hg2+/Zn2+ was synthesized by incorporating polycarboxylic receptor and benzimidazole as the fluorophore. Qualitative and quantitative analyses on probe-Cu2+/Hg2+/Zn2+ indicated the probe-target systems’ steady optical properties versus pH/time and good linear relationships. It could be applied to qualitative and quantitative detections of target ions at the concentration of μmol/L, giving off characteristic fluorescence responses and demonstrating 1:1 complexation stoichiometry after the recognition process. Furthermore, polycarboxylic-metal ions interactions were furtherly explored and possible combination mechanisms were revealed via FS, UV-Vis and 1HNMR, offering some evidence for the future research concerning the probe’s structural modification and properties optimization.

    Key words: fluorescent probe; polycarboxylic receptor; recognition mechanism; fluorescent response; synthesis

    引用本文成昭,鄭蕾,徐玥,等. 一種BAPTA熒光探針的合成、光譜性能與識別機制[J]. 化學試劑,2022,445715-723.

     

     

    色酮-3-甲醛席夫堿新型熒光探針高選擇性檢測CN離子

     

    趙俊,蔡小華*

    (貴州民族大學 化學工程學院,貴州 貴陽  550025)

     

    摘要:以色酮-3-甲醛和3-氨基吡唑為原料,通過一鍋法縮合反應得到新型猝滅型席夫堿熒光探針Z。在VDMSO:VH2O= 3:2的溶液中,通過選擇性、靈敏度、抗干擾、穩定性及pH影響等實驗,證實該探針具有較好的穩定性,能夠高靈敏度和選擇性地識別CN-,最低檢測限為1.9 × 10-8 mol/L。進一步熒光滴定實驗和機理研究,推測探針ZCN-的識別為加成反應型,結合比為1 : 1,結合常數為0.4 × 103 L/mol。探針Z具有較好實用性,能夠方便地用于苦杏仁中CN-定性檢測。

    關鍵詞:色酮-3-甲醛,3-氨基吡唑;席夫堿;熒光探針;CN-識別

    中圖分類號:O626      文獻標識碼:A      文章編號:0258-32832022

     

    A Novel Fluorescent Probe Based on Chromone-3-formaldehyde Schiff Base for Highly Selective CN Ion Detection ZHAO Jun, CAI Xiao-hua* (School of Chemical Engineering, Guizhou Minzu University, Guiyang 550025, China), Huaxue Shiji, 2022, 44(5),  

    Abstract: A novel fluorescence quenching Schiff base probe Z was synthesized by one pot condensation reaction of chromone-3-formaldehyde and 3-aminopyrazole. In a solution of V(DMSO):V(H2O) = 3:2, the selectivity, sensitivity, anti-interference, stability and pH effect experiments show that the probe has good stability. It can identify CN- with high sensitivity and selectivity, and its minimum detection limit is 1.9 × 10-8 mol/L. Further fluorescence titration experiment and mechanism study speculated that probe Z for CN- recognition goes through an addition reaction type, its binding ratio and binding constant is 1:1 and 0.4 × 103 L/mol, respectively. Probe Z has good practicability and can be easily used for the qualitative determination of CN- in bitter almond.

    Key words: chromone-3-formaldehyde; 3-aminopyrazole; fluorescent probe; Schiff base; CN-detection

    引用本文趙俊, 蔡小華.色酮-3-甲醛夫堿新型熒光探針高選擇性檢測CN離子[J]. 化學試劑, 2022, 44(5)724-728.

     

     

    FeOOH/MoS2的制備及其活化過一硫酸鹽的性能

     

    劉欣悅,吳丹,胡婉潔,趙煥新*,張志傲

    (沈陽化工大學 環境與安全工程學院,遼寧 沈陽 110142

     

    摘要:通過化學沉淀-水熱法制備了FeOOH/MoS2復合催化劑,以苯酚為目標污染物,探究其活化過一硫酸鹽(PMS)的性能。SEMXRD結果表明,FeOOH成功負載于MoS2納米片上。FeOOHMoS2摻雜比為1:3的復合催化劑活化PMS性能最好,在最佳反應條件下,反應20min后,苯酚降解率為96.60%,且該反應符合準一級動力學模型。自由基捕獲實驗證實,SO4?-是體系中主要的活性氧物種。另外,考察了實際水體和常見的無機陰離子對催化降解反應的影響,苯酚降解率在實際水體中略有下降,無機陰離子對苯酚降解的干擾從大到小依次為HCO3->H2PO4->NO3-,Cl-的影響可忽略不計。以上研究可為高活性PMS催化劑的設計提供新思路。

    關鍵詞FeOOH/MoS2;過一硫酸鹽;活化;苯酚;硫酸根自由基

    中圖分類號:X703.1       文獻標識碼:A      文章編號:0258-32832022--

     

    Synthesis of FeOOH/MoS2 and its Activation Performance for Peroxymonosulfate LIU Xin-yue, Wu Dan, Hu Wan-jie, ZHAO Huan-xin*, ZHANG Zhi-ao (College of Environmental and Safety Engineering, Shenyang University of Chemical Technology, Shenyang 110142, China), Huaxue Shiji, 2022, 44(5),

    Abstract: FeOOH/MoS2 composite catalyst was synthesized by the chemical precipitation-hydrothermal method. The phenol was used as the target pollutant to explore its performance of activating peroxymonosulfate (PMS). FeOOH was successfully loaded on MoS2nanosheets. The composite catalyst with a ratio of 1:3 had the best activation performance for PMS. Under optimal reaction conditions, phenoldegradation rate reached 96.60% after 20 minutes. And this reaction was in accordance with the pseudo first-order kinetic model. Free radical capture experiments confirms that SO4?- is the major reactive oxygen species in FeOOH/MoS2/PMS system. In addition, the effect of actual water and common inorganic anions on the catalytic degradation reaction was investigated. The degradation rate of phenol is reduced in actual water. The interference of inorganic anions on phenol degradation is in the order of HCO3->H2PO4->NO3-, and the influence of Cl- is negligible. The above research can provide new ideas for the design of high-activity PMS catalysts.

    Keywords: FeOOH/MoS2; peroxymonosulfate; activated; phenol; sulfate radical

    引用本文劉欣悅,吳丹,胡婉潔,. FeOOH/MoS2的制備及其活化過一硫酸鹽的性能[J]. 化學試劑,2022,445729-735.

     

     

    室溫下柱層析法同時提取刺玫果肉中維生素C和花色苷及其體外活性研究

    崔遙,戴鸝瑩,鐘方麗,王曉林*,王若男

    (吉林化工學院 化學與制藥工程學院,吉林 吉林  132022) 

     

    摘要探究柱層析法提取刺玫果維生素C和花色苷的工藝條件及體外活性。以提取液中維生素C質量和花色苷吸光度為指標,通過對溶劑濃度、pH、酸度調節劑、吸漲率MV、浸泡平衡時間等因素的考察確定最佳提取工藝。通過測定刺玫果維生素C、花色苷α-葡萄糖苷酶的抑制率1,1-二苯基-2-三硝基苯肼(DPPH?的清除率,考察其體外降血糖、抗氧化活性。結果表明,在最佳提取條件下,刺玫果肉維生素C和花色苷的提取率均在95%以上,浸膏中維生素C含量達到15%以上、花色苷的色價為8.07。刺玫果肉維生素C、花色苷提取物抑制α-葡萄糖苷酶活性均強于陽性對照阿卡波糖;清除DPPH?IC50分別為0.0031、0.0221 mg/mL。柱層析法可以同時提取刺玫果肉中的維生素C和花色苷,避免因單獨地提取一種活性成分而造成原料和溶劑的浪費,研究結果為刺玫果開發提供了科學依據。 

    關鍵詞刺玫果肉;維生素C;花色苷;柱層析法;體外活性

    中圖分類號:TS201    文獻標識碼:A       文章編號:0258-32832022--

     

    Simultaneous Extraction of Vitamin C and Anthocyanins from the Fruit Pulp of Rosa davurica Pall. by Column Chromatography at Room Temperature and Their Activities in Vitro CUI Yao, DAI Li-ying, ZHONG Fang-li, WANG Xiao-lin*, WANG Ruo-nan (School of Chemistry and Pharmaceutical Engineering, Jilin Institute of Chemical Technology, Jilin 132022, China), Huaxue Shiji, 2022, 44(3),

    Abstract: The extraction conditions and activities in vitro of vitamin C and anthocyanins from the fruit pulp of Rosa davurica Pall. by column chromatography were investigated. Using quality of vitamin C and absorbance of anthocyanin as indexes, the optimal extraction process was determined base on the examination of factors such as solvent concentration, pH, acidity regulator, swelling-up rate. Both the α-glucosidase inhibitory rate and the DPPH? clearance rate of vitamin C and anthocyanin were determined to investigate their hypoglycemic and antioxidant activities in vitro. Under the optimal extraction conditions, the extraction rates of vitamin C and anthocyanin in the fruit pulp of Rosa davurica Pall. were above 95%, the content of vitamin C in extract was above 15%, and the color value of anthocyanin was 8.07. The α-glucosidase inhibition activity of vitamin C and anthocyanin in extract of the fruit pulp of Rosa davurica Pall. was stronger than positive control acarbose. The IC50 of DPPH? were 0.0031 mg/mL and 0.0221 mg/mL, respectively. Column chromatography can simultaneously extract vitamin C and anthocyanins which may avoid the waste of raw materials and solvents caused by extracting one active ingredient at one time. The results provided scientific basis for the R&D of Rosa davurica Pall.

    Key words: fruit pulp of Rosa davurica Pall.; Vitamin C; Anthocyanins; column chromatography; vitro activity

    引用本文:崔遙,戴鸝瑩,鐘方麗,等. 室溫下柱層析法同時提取刺玫果肉中維生素C和花色苷及其體外活性研究[J]. 化學試劑,2022,44(5): 736-743。

     

     

    石墨炔碳材料在新型電池中的研究進展

    何珺

    (揚州市職業大學醫學院,江蘇 揚州  225009)

    石墨炔(graphdiyne,GDY)因其卓越的二維平面全碳多孔特性,在多個領域具有巨大的應用潛力。特別是GDY獨特的結構特點和物理本征特性如可擴展的面內孔洞、適宜的層間距、規則的納米結構、優良的導電性及其良好的離子傳輸性能,使GDY成為很有應用前景的新型儲能裝置如鉀離子電池、金屬硫電池、金屬空氣電池等器件中的電極材料。重點對近年石墨炔碳材料在新型金屬離子電池,金屬空氣電池,金屬硫電池以及雙離子電池等電池儲能器件相關的研究成果進行了綜述。此外,還對GDY在新型電池儲能器件中的發展趨勢進行了綜合評價,并對未來石墨炔類碳材料在能源存儲領域的進一步發展進行了展望。

    關鍵詞:石墨炔;新型電池;碳材料;儲能;研究進展

    中圖分類號:O625      文獻標識碼:A       文章編號:0258-3283(2022)--

     

    Progress of Graphdiyne Carbon Materials in Novel Batteries HE Jun * (Medical College of Yangzhou Vocational University, Yangzhou 225009, China) Huaxue Shiji, 2021, 44(5), ~

    Abstract: Graphdiyne (GDY) has exhibited great application potential in various fields for the excellent two-dimensional full carbon planar and porous characteristics. Particularly, the unique structural characteristics and physical intrinsic characteristics, such as expandable in-plane holes, appropriate layer spacing, regular nanostructures, excellent conductivity and good ion transport performance, endowing GDY and its derivates can be used as an electrode material in many novel energy storage devices with great application prospects, such as sodium ion battery, potassium ion battery, metal air battery, metal sulfur battery and so on. This work focused on the research results of GDY based carbon materials in battery energy storage devices including novel ion battery, metal air battery, metal sulfur battery and double ion battery in recent years. In addition, the development trend of GDY in new battery energy storage devices is comprehensively evaluated, and the further development of GDY based carbon materials in energy storage is prospected.

    Key wordsgraphdiyne; novel batteries; carbon material; energy storage; research progress

    引用本文:何珺. 石墨炔碳材料在新型電池中的研究進展[J]. 化學試劑, 2022, 44(5): 744-754。

     

     

    QuEChERS-分散液液微萃取結合GC-MS測定土壤中的多環芳烴殘留

    王傳咪1, 2,譚華東*2, 3,武春媛*2,3,翟金玲1

    (1. 海南大學 熱帶作物學院,海南 ??? 570228;2. 中國熱帶農業科學院 環境與植物保護研究所,海南 ??? 571101;3. 國家農業環境儋州觀測實驗站,海南 儋州  571737)

    摘要:建立了分散液液微萃?。?/span>DLLME)結合氣相色譜串聯質譜(GC-MS)測定土壤中痕量多環芳烴(PAHs)新方法。采用QuEChERSQuick、Easy、Cheap、Effective,RuggedSafe)和DLLME對土壤中的15PAHs進行了提取與富集,考察提取溶劑、凈化劑用量、萃取溶劑種類及用量對提取效果的影響。結果表明,10 g土壤樣品以20 mL V(甲醇)∶V(二氯甲烷)=11混合溶劑為提取溶劑、150 mg W(PSA)W(C18)=41吸附劑凈化,2 mL上清液加100 μL甲苯作為分散、萃取劑時最佳。所建方法在6500 μg/L范圍內呈良好的線性關系,且R20.9995;檢測限(LODs)和定量限(LODs)分別為0.11.80.36.1 μg/kg。在1、5、25 μg/kg加標水平下,PAHs回收率為70.2%108.5%,相對標準偏差(RSDs)為1.0%11.6%。該方法簡便、快速、易于提取和富集,適用于包括澄邁縣在內土壤中PAHs靈敏測定。

    關鍵詞:多環芳烴;QuEChERS;分散液液微萃??;氣相色譜串聯質譜;土壤

    中圖分類號:O656.31      文獻標識碼:A          文章編號:0258-32832022--

     

    Determination of Polycyclic Aromatic Hydrocarbons in Soil by QuEChERS-dispersive Liquid-liquid Microextraction Combined with GC-MS WANG Chuan-mi1,2, TAN Hua-dong*2,3, WU Chun-yuan*2,3, ZHAI Jin-ling1 (1. College of Tropical Crops, Hainan University, Haikou 570228, China; 2. Institute of Environment and Plant Protection, Chinese Academy of Tropical Agricultural Sciences, Haikou 571101, China; 3. National Danzhou Observation and Experiment Station for Agricultural Environment, Danzhou 571737, Hainan, China), Huaxue Shiji, 2022, 44(5),~

    Abstract: A new method for the determination of trace polycyclic aromatic hydrocarbons (PAHs) in soil by dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography-tandem mass spectrometry (GC-MS) was established. Fifteen PAHs in soil were extracted and enriched by QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and DLLME. The effects of extraction solvent, decontaminant dosage, type and dosage of extraction solvent on extraction efficiency were investigated. The 10g soil samples were extracted with 20 mL V(methanol)V(dichloromethane)=11 mixed solvent, purified with 150 mg W(PSA)W(C18)=41 adsorbent. When 2 mL supernatant was added with 100 μL toluene as dispersing and extracting agent, the effect was the optimal. There was the good linearity for the established method in the range of 6500 μ g/L, and R20.9995; the detection limits (LODs) and quantitative limits (LODs) were 0.11.8 and 0.36.1μg/kg, respectively. The recoveries of PAHs ranged from 70.2% to 108.5% and the relative standard deviations (RSDs) ranged from 1.0% to 11.6% at the level of 1, 5 and 25μg/kg. The method is simple, rapid, easy to extract and enrich, it is suitable for sensitive determination of PAHs in soil including Chengmai County.

    Keywords: Polycyclic aromatic hydrocarbons; QuEChERS; dispersive liquid-liquid microextraction; gas chromatography-mass spectrometry; soil

    引用本文:王傳咪,譚華東,武春媛,等. QuEChERS-分散液液微萃取結合GC-MS測定土壤中的多環芳烴殘留[J]. 化學試劑,2022,445755-761。

     

     

    HPLC-DAD-ELSD聯用法同時測定華佗救心丸中13種成分的含

    朱雅琴1, 2, 3,趙冰4,祝宇龍1,閆富龍1,張云靜1, 2, 3,吳德玲1, 2, 3,彭燦1, 2, 3,吳歡*1, 2, 3

    (1. 安徽中醫藥大學 藥學院,安徽 合肥230012;2. 藥物制劑技術與應用安徽省重點實驗室,安徽 合肥230012;3. 中藥復方安徽省重點實驗室,安徽 合肥230012;4. 華佗國藥股份有限公司,安徽 亳州236800)

     

    摘要建立一種快速的HPLC-DAD-ELSD聯用方法,同時測定華佗救心丸中皂苷類、蟾蜍甾烯類以及膽酸類13種成分的含量。采用HPLC-DAD-ELSD聯用,色譜柱Caprisil C18( 250 mm×4.6 mm,5 μm),柱溫35 ℃,并以乙腈作為流動相進行梯度洗脫。紫外檢測波長296 nm203nm,ELSD檢測參數漂移管溫度60 ℃、氣體壓力241 kPa,檢測時間18 min。華佗救心丸中的13分析成分線性r值均大于0.99,線性關系良好(r ≥ 0.99),平均加樣回收率96.31%103.30%范圍內,RSD值為1.42%2.75%。該方法更快速全面的同時測定華佗救心丸中13分析成分含量,專屬性強、精確度高,可為華佗救心丸質量控制和進一步的品質提升提供參考。

    關鍵詞華佗救心丸;高效液相色譜法-全波長檢測-蒸發光散射器聯用;蟾蜍甾烯類;膽酸類;皂苷類

    中圖分類號:R284.1        文獻標碼:A 文章編號:0258-32832022--

     

    Simultaneous Determination of 13 Components in HuatuoJiuxin Pills by HPLC-DAD-ELSD

    ZHU Ya-qin1, 2, 3, ZHAO Bing4, ZHU Yu-long1, YAN Fu-long1, ZHANG Yun-jing1, 2, 3, WU De-ling 1, 2, 3, PENG Can 1, 2, 3, WU Huan* 1, 2, 3(1. School of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012; 2. Anhui Province Key Laboratory of Pharmaceutical Preparation Technology and Application, Hefei 230012; 3 Anhui Key Laboratory of Chinese Medicinal Formula., Hefei 230012; 4. Huatuo Medicines Co., Ltd, Bozhou 236800), HuaxueShiji, 2022, 44(5),

    Abstract:  The HPLC-DAD-ELSD method was established to simultaneously determine the contents of 13 saponins, bufadienolides and bile acids in HuatuoJiuxin Pills. The established HPLC-DAD-ELSD method was adopted, in which a Caprisil C18 column (250 mm×4.6 mm, 5 μm) was used, the column temperature was 35 , and water-acetonitrile was used as the mobile phase for gradient elution.In addition, the wavelength of UV detection was 296 nm and 203 nm. The temperature of the drift tube in the detection parameters of the evaporative light scattering detector (ELSD) was 60 , the gas pressure was 241 kPa and the gain was 100. Finally, the total detection time was 18 min. Results: The linear r values of the 13 analytical components in HuatuoJiuxin Pills were all greater than 0.99, so that the linear relationship was well (r  0.99). The average recovery rate of sample addition was in the range of 96.31% to 103.30%, and the RSD was 1.42% to 2.75%. Conclusion: This method can simultaneously determine the content of 13 analytical components in Huatuo Jiuxin Pills more quickly and comprehensively, with strong specificity and high accuracy, which can provide references for the quality control and further quality improvement of HuatuoJiuxin Pills.

    Key words:HuatuoJiuxin Pills; HPLC-DAD-ELSD; bufadienolides; cholic acids; saponins

    引用本文:朱雅琴,趙冰。祝宇龍,等. HPLC-DAD-ELSD聯用法同時測定華佗救心丸中13種成分的含量[J]. 化學試劑,2022,44(4): 762-766。

     

     

    乙酰苯胺元素含量標準物質的研制

    王海峰*,李佳,孫國華

    (中國計量科學研究院,北京  100029

     

    摘要:有機元素分析儀用于測定有機化合物、煤炭等能源產品以及食品的碳、氫和氮元素含量,儀器需要有機純物質元素含量標準物質來校準。研制了乙酰苯胺元素含量標準物質,編號為GBW 06203。使用區域熔融裝置提純乙酰苯胺原料,然后分裝制成標物候選物。采用氣相色譜質譜法和差示掃描量熱法測定其有機雜質含量,采用卡爾·費休庫侖法測量其水分,采用灼燒殘渣稱重法測量其無機雜質含量,然后根據質量平衡原理計算主組分的含量。然后根據主組分和雜質的含量及其分子中待測元素的含量,計算得到標準物質的碳、氫和氮元素含量標準值。標準值溯源至純物質的質量、溫度和原子量上。碳、氫和氮元素含量的標準值分別為71.087%、6.712%10.363%,不確定度(U,k=2)分別為0.003%、0.002%0.001%。標準物質的準確度達到了國際先進的水平。標準物質可用于杜馬斯法等有機元素分析儀的校準,也可用于油品氮含量標準物質的配制,保障有機元素含量的量值準確。

    關鍵詞:碳;氫;氮;元素分析;標準物質

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

     

    Certified Reference Material of Acetanilide for Elemental Content WANG Hai-feng, LI Jia, SUN Guo-hua (National institute of metrology of China, Beijing 100029, China), Huaxue Shiji, 2022, 44(5),

    Abstract: Organic elemental analyzer was used to determine the content of carbon, hydrogen, and nitrogen of organic compounds, energy products, such as coal, and food. The analyzer should be calibrated by using the certified reference material (CRM) of organic pure substance for elemental content. The CRM of acetanilide for elemental content labelled as GBW 06203 was developed. The raw acetanilide was purified by zone melting and then packaged as candidates of CRM. Gas chromatography – mass spectrometry (GC-MS) and differential scanning calorimetry (DSC) were used to determine the organic impurities content. Karl Fischer coulometric titration and the residue on ignition was used to determine the water content and inorganic impurities content, respectively. Then, the main component content was calculated based on the mass balance theory. The certified value of carbon, hydrogen and nitrogen content was calculated by using the individual component content and the aimed elemental content in its molecule. The certified value is traceable to the mass of pure substance, temperature, and atomic weight. The certified content of carbon, hydrogen, and nitrogen was 71.087%, 6.712%, and 10.363%, respectively, with the uncertainty (U, k=2) of 0.003%, 0.002%, and 0.001%, respectively. The accuracy of CRM is on the advanced world level. The CRM can be used to calibrate the Dumas type organic elemental analyzer and prepare the CRM of petroleum for nitrogen content, which is helpful for the accuracy of the organic elemental content.

    Keyword: carbon; hydrogen; nitrogen; elemental analysis; certified reference material

    引用本文:王海峰,李佳,孫國華. 乙酰苯胺元素含量標準物質的研制[J]. 化學試劑,2022,445:767-772

     

     

    穩定同位素標記丹磺酰氯-D6的合成方法研究

    劉家興1,汪滿江措1,張國寧2,臧清策1,王玉成2,張瑞萍*1

    (1. 中國醫學科學院 北京協和醫學院藥物研究所 天然藥物活性物質與功能國家重點實驗室,北京 100050;2. 中國醫學科學院 北京協和醫學院醫藥生物技術研究所,北京 100050)

     

    摘要:本研究旨在報道一種原料易得、毒性小、產率高的丹磺酰氯-D6 (Dansyl chloride-D6,DnsCl-D6)的化學合成方法。以碘甲烷-D3為同位素標記原料,5-氨基-1-萘磺酸、三氯氧磷和五氯化磷為反應原料,經兩步取代反應制備得到丹磺酰氯-D6。以投入的碘甲烷-D3的物質的量計算,丹磺酰氯-D6總產率為82%,經高分辨質譜測定丹磺酰氯-D6的同位素豐度為98.6 atom%D。該方法可以為穩定同位素標記衍生化試劑的合成提供參考。

    關鍵詞:穩定同位素標記;衍生化試劑;丹磺酰氯;碘甲烷-D3;化學合成

    中圖分類號:TQ421.6      文獻標識碼:A       文章編號:0258-32832022

     

    Synthesis of Stable Isotope Labelled Dansyl Chloride-D6 LIU Jia-xing1, WANG Man-jiang-cuo1, ZHANG Guo-ning2, ZANG Qing-ce1, WANG Yu-cheng2, ZHANG Rui-ping*1 (1. State Key Laboratory of Bioactive Substance and Function of Natural Medicines, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, China; 2. Institute of Medical Biotechnology, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, China), Huaxue Shiji, 2022, 44(5), 00 ~ 00

    Abstract: A method with low cost, low toxicity and high yield for dansyl chloride-D6 was established. The synthesis process consisted of two-stage substitution reaction with 5-amino-1-naphthalenesulfonic acid and iodomethane-D3 as precursors while dansyl chloride-D6 (DnsCl-D6) as product. The yield of DnsCl-D6 was 82% based on the consumed iodomethane-D3. The targeted product was confirmed by HR-MS. Its isotopic abundance was 98.6 atom%D. This method can be used for stable isotope labeling derivation reagent synthesis.

    Key words: stable isotope labeling; derivation reagent; dansyl chloride; iodomethane-D3; chemical synthesis

    引用本文:劉家興,汪滿江措,張國寧,等. 穩定同位素標記丹磺酰氯-D6的合成方法研究[J]. 化學試劑, 2022, 44(5): 773-776。

     

     

    苯甲酸催化的三組分[3+2]環加成反應合成六氫吡咯并[2,1-a]異喹啉化合物

    蔣少棟,江多鍍,馬曉明,劉建武,嚴生虎,張躍*

    (常州大學 藥學院,江蘇 常州  213164

     

    摘要為發展六氫吡咯并[2,1-a]異喹啉化合物的合成方法,以苯甲酸為催化劑,4?分子篩為添加劑,催化芳香醛、1,2,3,4-四氫異喹啉和N-取代馬來酰亞胺經串聯的醛胺縮合和[3+2]環加成反應,合成了一系列六氫吡咯并[2,1-a]異喹啉化合物。主要考察了催化劑、溶劑、反應時間及反應溫度對產物產率的影響,最終確定在60 下,以10 mL超干甲苯為溶劑,20 mol%苯甲酸為催化劑,加入250 mg分子篩,以n(芳香醛)n(1,2,3,4-四氫異喹啉)n(N-取代馬來酰亞胺) = 11.31.2反應2 h。產物結構經1H NMR、13C NMRHRMS等手段表征,產物4f空間立體結構由單晶X射線衍射確定。

    關鍵詞苯甲酸;1,2,3,4-四氫異喹啉;[3+2]環加成反應;六氫吡咯[2,1-a]異喹 

    中圖分類號:TQ20        文獻標識碼:A       文章編號:0258-32832022

     

    Benzoic Acid Catalyzed Three-component [3+2] Cycloaddition for the Synthesis of Hexahydroyrrolo[2,1-a]isoquinoline Compounds JIANG Shao-dong, JIANG Duo-du, MA Xiao-ming, LIU Jian-wu, YAN Sheng-hu, ZHANG Yue* (School of Pharmacy, Changzhou University, Changzhou 213164, China), Huaxue Shiji, 2022, 44(5)

    Abstract: A novel protocol for the synthesis of hexahydroyrrolo[2,1-a]isoquinoline compounds was developed, using benzoic acid as catalyst via three-component reaction with aromatic aldehydes, 1,2,3,4-tetrahydroisoquinoline and N-substituted maleimides through sequential condensation and [3+2] cycloaddition with 4? molecular sieves as additives. The effects of catalyst, solvent, reaction time and reaction temperature on the yields of the products were investigated. The optimized conditions for the one-pot synthesis were found to conduct the reaction with aromatic aldehydes, 1,2,3,4-tetrahydroisoquinoline and N-substituted maleimides (mol ratio 1:1.3:1.2) using benzoic acid (20 mol%) as catalyst, in the presence of 250 mg 4? molecular sieves in 10 mL ultra-dry toluene at 60 °C for 2 h. The products were confirmed by 1H NMR, 13C NMR, HRMS, the stereochemistry of compound 4f was confirmed by single crystal X-ray diffraction.

    Key words: benzoic acid; 1,2,3,4-tetrahydroisoquinoline; [3+2] cycloaddition; hexahydropyrrolo[2,1-a]isoquinoline

    引用本文:蔣少棟, 江多鍍, 馬曉明, .苯甲酸催化的三組分[3+2]環加成反應合成六氫吡咯并[2,1-a]異喹啉化合物[J].化學試劑, 2022, 44(5)777-785。

     

     

    Fries重排合成3-乙?;?/span>-2-羥基苯甲醛肟

    王琳a,侯家寧a,盧璽盟a,田宇a,常遠a,耿佳鑫a,馮玉玲a,b,孫京國*a,b

    (河北師范大學a. 化學與材料科學學院;b. 化學國家級實驗教學示范中心 河北 石家莊 050024

     

    摘要鄰羥基苯乙酮衍生物是合成查爾酮、黃酮、萘醌、農藥等生物活性化合物的重要中間體,采用傳統Lewis酸催化缺乏競爭力存在環境壓力,選用PPAFries重排反應的催化劑及溶劑,設計了(1)水楊醛經酯化、肟化、Fries重排和(2水楊醛經肟化、酯化、Fries重排2反應路線,實驗結果表明,路線(2)較好,水楊醛在氧化鋅催化下與羥胺反應生成水楊醛肟,再經乙酸酐與酚羥基和肟羥基反應同時引入乙?;?,兩步產率均超過90.0%。80%PPA為催化劑,在150℃條件下反應2h,完成酚酯的選擇性Fries重排合成新化合物3-乙?;?/span>-2-羥基苯甲醛肟AHbdO,產率22.4%,HPLC純度99.33%?;衔锓肿咏Y構經1H NMR、13C NMR、TLC-MS確證,研究為此類化合物反應提供了一種新的高效綠色合成方法。

    關鍵詞肟化;酯化;Fries重排;合成

    中圖分類號O626.6      文獻標識碼A      文章編號0258-32832022-

     

    Synthesis of 3-Acetyl-2-hydroxybenzaldehyde Oxime by Fries Rearrangement WANG Lina, HOU Jia-ninga, LU Xi-menga, TIAN yua, CHANG yuana, GENG jia-xina, FENG yu-linga,b , SUN Jing-guo*a,b (1. School of Chemistry and Materials Science; 2. National Experimental Teaching Demonstration Center of Chemistry (Hebei Normal University), Hebei Normal University, Shijiazhuang 050024, China), Huaxue Shiji, 2022, 44(5),

    Abstract: O-Hydroxyacetophenone derivatives are important intermediates for the synthesis of bioactive compounds such as chalcone, flavonoids, naphthoquinones, pesticides, etc. Lack of competitiveness and environmental pressures with traditional Lewis acid catalysis. In this work, PPA was used as the catalyst and solvent for the Fries rearrangement reaction, and two reaction routes were designed: (1) Salicylaldehyde via esterification, oximation, Fries rearrangement and (2) Salicylaldehyde via oximation, esterification, and Fries rearrangement. The results showed that route (2) was preferable. Salicylaldehyde reacted with hydroxylamine under the catalysis of zinc oxide to form salicylaldoxime, which was then reacted with phenol hydroxyl and oxime hydroxyl by acetic anhydride to simultaneously introduce acetyl group. The yields of the two steps were more than 90.0%. Then 80%PPA was used as the catalyst to react at 150℃ for 2h to complete the selective Fries rearrangement of phenol ester to synthesize the new compound 3- acetyl -2- hydroxybenzaldehyde oxime (AHbdO) with the yield of 22.4% and the purity of 99.33% by HPLC. The structure was confirmed by 1H NMR, 13C NMR and TLC-MS. This work provides a new efficient and green synthesis method for the reaction of these compounds.

    Key words: Oximation; Esterification; Fries rearrangement; Synthesis

    引用本文王琳,侯家寧,盧璽盟,等.Fries重排合成3-乙?;?/span>-2-羥基苯甲醛肟[J]. 化學試劑,2022,445786-790.

     

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