• <blockquote id="cw04w"><samp id="cw04w"></samp></blockquote>
  • <blockquote id="cw04w"></blockquote>
  • 當前位置:首頁 > 化學試劑 > 熱點文章 > 正文

    《化學試劑》2022年第6期中英文摘要(附整期文章PDF文檔)

    發布時間: 2022-06-06 09:00:04   試劑信息網

    【綜述與專論】

    絲氨酸蛋白酶有機小分子熒光探針的研究進展

    堯功梅1,龐承云2,蒙柳衛1,李清*1

    (1.      廣西醫科大學 藥學院,廣西 南寧  530021;2.廣西醫科大學附屬腫瘤醫院 藥學部,廣西 南寧  530021

     

    摘要絲氨酸蛋白酶與人類生命健康息息相關。人體內絲氨酸蛋白酶水平的異常會引起疾病,危害人類生命安全。絲氨酸蛋白酶熒光探針對于檢測體內和體外的絲氨酸蛋白酶數量、活性動態以及臨床疾病的治療有重要意義。因此,重點回顧了近5年來文獻中報道的性能優異的常見絲氨酸蛋白酶熒光探針,以各種絲氨酸蛋白酶的顯色標記為出發點,總結了目前絲氨酸蛋白酶的熒光探針的合成和性能研究,旨在為絲氨酸蛋白酶的熒光探針設計策略與檢測應用提供理論參考。

    關鍵詞:絲氨酸蛋白酶;熒光探針;設計策略;發光機理;性能研究;檢測應用

    中圖分類號R944;R95            文獻標識碼A          文章編號0258-32832022

     

    Recent Advances on the Design Strategy and Application Status of Small Organic Molecular Fluorescent Probes of Serine Protease YAO Gong-mei1, PANG Chen-yun2, MENG Liu-wei1, LI Qing*1 (1. College of Pharmacy, Guangxi Medical University, Nanning 530021, China; 2. Department of Pharmacy, Affiliated Tumor Hospital of Guangxi Medical University, Nanning 530200, China), Huaxue Shiji, 2022, 44(6)

    Abstract: Serine proteases are closely related to human life and health. Abnormal levels of serine proteases in the human body can cause diseases and endanger human life. Serine protease fluorescent probes are of great significance for detecting the number and activity dynamics of serine proteases in vivo and in vitro, as well as the treatment of clinical diseases. Therefore, this review article focuses on reviewing common serine protease fluorescent probes with excellent performance in the past five years. Based on the chromogenic labeling of various serine proteases, this review summarizes the current synthesis and performance research of fluorescent probes for serine proteases, aiming to provide a theoretical reference for the design strategies and detection applications of fluorescent probes for serine proteases.

    Key words: serine protease; fluorescent probe; performance study

    引用本文:堯功梅,龐承云,蒙柳衛,等. 絲氨酸蛋白酶有機小分子熒光探針的研究進展[J]. 化學試劑,2022,446791-800.

     

     

    基于納米材料的比色適配體傳感器的應用

    韓高寰,李靜*,張冰,王之飛,湯順潔,趙志換,高文超*

    (太原理工大學 生物醫學工程學院,山西 太原  030024

     

    摘要:比色分析是一種檢測目標物的方法,具有肉眼可見、操作方便、快捷、實時等優點,被廣泛應用于醫療分析、環境監測、食品安全和質量分析等領域。納米材料具有優良的光學性能和催化性能,目前通常被當作信號轉化元件應用在比色傳感器中。核酸適配體(Aptamer,Apt具有特異性識別功能且易于修飾和編輯,在比色傳感器的設計中主要作為識別元件,也可以作為信號轉化元件和信號放大元件?;诩{米材料的比色適配體傳感器同時具備了兩種材料的優點,可以實現對大多數目標物的檢測,是極具潛力的比色傳感器研究方向。文章總結了基于納米材料和Apt結合的比色傳感器的構建方案和顯色原理,并簡要歸納了其在農藥、癌癥標志物、生物小分子、抗生素、重金屬離子等目標物檢測當中的研究進展。

    關鍵詞:傳感器;適配體;納米材料;分析檢測;

    中圖分類號:O657.3      文獻標識碼: A     文章編號:0258-32832022

     

    Colorimetric Apta-sensors Based on Nanomaterials and Its Applications HAN Gao-huan,LI Jing*,ZHANG Bing,WANG Zhi-fei,TANG Shun-jie,ZHAO Zhi-huan, GAO Wen-chao* (School of Biomedical Engineering, Taiyuan University of Technology, Taiyuan 030024, China), Huaxue Shiji,2022,44(6)

    Abstract: Colorimetric analysis is an efficient method for detecting objects, it has been widely used in medical analysis, environmental monitoring, food safety, and quality analysis owing to their visible, easy/fast operation, high real-time merits, and so on. While nanomaterials have excellent optical and catalytic properties, which are often used as signal conversion components in colorimetric sensors. Aptamers have specific recognition functions, they are easy to be modified and edited, therefore have been mainly used as recognition components for designing colorimetric sensors, as well as signal conversion and amplification components. The colorimetric sensors based on the combination of nanomaterials and aptamers integrate the advantages of each component and can realize the detection of most target objects, which is one promising colorimetric sensor research area. In this review article, the construction scheme and color rendering principle of the colorimetry Apta-sensors are summarized. Furthermore, the main applications of detecting pesticides, cancer markers, biologically small molecules, antibiotics, heavy metal ions, and other target objects are also briefly summarized.

    Key words: sensor; aptamer; nanomaterials; analytical detection

    引用本文:韓高寰,李靜,張冰,等. 基于納米材料的比色適配體傳感器的應用 [J]. 化學試劑,2022,446801-809。

     

     

    【生化與藥用試劑】

    雷公藤紅素與人血清白蛋白的相互作用

    劉浩1,樊世萌1,歐陽敬禹1,尤祥宇*1,蘇江濤1,李玲玲2,肖紅衛3

    1. 湖北工業大學 生物工程與食品學院,湖北 武漢 430068;2. 武漢文理學院 醫學院,湖北 武漢 430345;3. 湖北省農業科學院 畜牧獸醫研究所 動物胚胎工程與分子育種湖北省重點實驗室,湖北 武漢 430072

     

    摘要:通過使用熒光光譜、分光光度法以及等溫滴定量熱法等研究方法,研究了人血清白蛋白(HSA)與雷公藤紅素的結合方式,采用分子對接的方式分析相互作用模式。熒光光譜結果可知,雷公藤紅素與HSA主要通過氫鍵和范德華力結合,并且雷公藤紅素猝滅HSA內源熒光的機制為靜態猝滅,同時兩者的結合過程主要受溫度影響。在兩者的結合過程中,會導致HSA的構象與微環境發生微小的改變。結合分子對接結果可知,兩者的結合過程可能主要是通過疏水相互作用、范德華力等弱相互作用進行結合。為雷公藤紅素在血液中的運輸及傳遞提供了理論支持,對深入理解雷公藤紅素的藥效學和藥代動力學性質具有重要的意義。

    關鍵詞:人血清白蛋白;雷公藤紅素;熒光;等溫滴定量熱法;分子對接

    中圖分類號:R961      文獻標識碼:A      文章編號:0258-32832022--

     

    Interaction between Celastrol and Human Serum Albumin LIU Hao1, Fan Shi-meng1, Ouyang Jing-yu1,You Xiang-yu*1, Su Jiang-tao1, Li Ling-ling2,XIAO Hong-wei3 (1.School of Food and Biological Engineering, Hubei Universityof Technology, Wuhan 430068, China; 2.Medical School, Wuhan University of Arts and Science, Wuhan 430345, China; 3. Hubei Provincial Key Laboratory of Animal Embryo Engineering and Molecular Breeding, Institute of Animal Husbandry and Veterinary Medicine, Hubei Academy of Agricultural Sciences, Wuhan 430072, China), Huaxue Shiji, 2022, 44(6),

    Abstract: In this paper, fluorescence spectroscopy, spectrophotometry, and isothermal titration calorimetry were used to study the binding mode of simulated human serum albumin (HSA) and celastrol, and molecular docking was used to analyze the interaction mode. Fluorescence spectrum results showed that celastrol and HSA are mainly bound via hydrogen bond and intermolecular force, and the mechanism of celastrol quenching HSA endogenous fluorescence is static quenching, and the binding process of celastrol and HSA is mainly affected by temperature. In the combination process, it was revealed that the conformation and microenvironment of HSA will change slightly. Combining the molecular docking results, the bonding process of the two may be mainly governed by weak interactions such as hydrophobic interaction and intermolecular force. This study provides theoretical support for the transport and delivery of celastrol in blood and is of great significance for further understanding the pharmacodynamics and pharmacokinetic properties of celastrol.

    Key words: human serum albumin; celastrol; fluorescence;isothermal titration calorimetry; molecular docking

    引用本文:劉浩,樊世萌,歐陽敬禹,等. 雷公藤紅素與人血清白蛋白的相互作用[J]. 化學試劑,2022, 446810-815.

     

     

    3,5-二芳基取代吡唑為Cap的新型選擇性HDAC6抑制劑:設計、合成及抑酶活性評價

    何格1,張明明1,李志1,徐星星1,袁真1,王琴1,馬曉東*1,2

    1. 安徽中醫藥大學 藥學院,安徽 合肥 230038;2. 安徽省中醫藥科學院 藥物化學研究所,安徽 合肥 230012

     

    摘要:為發現新型組蛋白去乙?;敢种苿?/span>Histone deacetylase inhibitors, HDACis,基于現有代表性選擇性HDAC6抑制劑的結構特征,采用構象限制型的3, 5-二芳基取代吡唑Cap單元構建目標分子,經Claisen-Schmidt反應、環合、親核取代、水解、縮合、羥胺解反應合成了9個化合物,并通過氫譜和質譜對其進行結構確證。抑酶活性測試結果顯示,化合物4-((3,5-(4-氯苯基)-1H-吡唑-1-)甲基)-N-羥基苯甲酰胺(5aHDAC6具有良好的抑制活性(IC50 = 0.25 μmol/L)和一定的亞型選擇性。

    關鍵詞:設計;合成;組蛋白去乙?;?/span>6抑制劑;抑酶活性評價;選擇性

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

     

    Novel Selective HDAC6 Inhibitors Bearing 3, 5-Diaryl-substituted 1H-Pyrazole as Capmoiety: The Design, Synthesis and Evaluation of Enzymatic Activity HE Ge1, ZHANG Ming-ming1, LIZhi1, XU Xing-xing1, YUAN Zhen1, WANG Qin1, MA Xiao-dong*1,2 (1. College of Pharmacy, Anhui University of Chinese Medicine, Hefei 230038, China; 2. Department of Medicinal Chemistry, Anhui Academy of Chinese Medicine, Hefei 230012, China), Huaxue Shiji, 2022, 44(6), 00 ~ 00

    Abstract: This study is conducted to discover novel histone deacetylase inhibitors (HDACis). Based on the structural characteristics of the representative histone deacetylase 6 (HDAC6) selective inhibitors, nine target compounds that feature conformationally restricted 3, 5-diaryl-substituted 1H-pyrazole as the Cap moiety were designed based on structural characteristics of the representative selective HDAC6is, and synthesized via Claisen-Schmidt reaction, cyclization reaction, substitution reaction, hydrolysis, condensation with THP protected hydroxylamine and deprotection. Their molecular structures have been confirmed by 1H NMR and MS. The biochemical assay showed that compound 4-((3,5-bis(4-chlorophenyl)-1H-pyrazol-1-yl)methyl)-N-hydroxybenzamide (5a) exhibited acceptable HDAC6 inhibitory activity (IC50 = 0.25 μmol/L) and moderate selectivity.

    Key words: design; synthesis; histone deacetylase 6 inhibitor; biochemical assay; selectivity

    引用本文:何格,張明明,李志,等. 3,5-二芳基取代吡唑為Cap的新型選擇性HDAC6抑制劑:設計、合成及抑酶活性評價[J]. 化學試劑, 2022, 44(6):816-821。

     

    【功能材料】

    改性柚子皮生物炭吸附亞甲基藍性能研究

    張妍杰,王歡,蔡玉福,邊子琦,趙興,劉彥琳,趙永華*

    (遼寧工業大學 化學與環境工程學院,遼寧 錦州  121001

     

    摘要:采用硝酸-高錳酸鉀活化法對制備的柚子皮生物炭進行改性處理,并將其作為吸附劑探究了其對亞甲基藍的吸附性能。通過靜態吸附實驗考察了亞甲基藍溶液的pH、初始濃度、吸附時間、吸附溫度、吸附劑投加量等條件對吸附效果的影響,并確定了該吸附過程的吸附動力學、吸附等溫線和吸附熱力學。實驗結果表明,在改性生物炭投加量為0.6 g/L、pH 7、亞甲基藍溶液濃度為100 mg/L、50 oC吸附180 min的條件下,改性生物炭對亞甲基藍的吸附容量為68.28 mg/g。通過準二級動力學方程和Freundlich方程更好的描述了該吸附過程,同時吸附熱力學表明該吸附過程是一個自發吸熱過程。

    關鍵詞:柚子皮;生物炭;亞甲基藍;吸附

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

     

    Adsorption of Methylene Blue by Modified Pomelo Peel Biochar ZHANG Yan-jie, WANG Huan, CAI Yu-fu, BIAN Zi-qi, ZHAO Xing, LIU Yan-lin, ZHAO Yong-hua*(School of Chemistry & Environmental Engineering, Liaoning University of Technology, Jinzhou 121001, China), Huaxue Shiji, 2022, 44(6)

    Abstract: Pomelo peel-derived biochar was firstly modified by using nitric acid-potassium permanganate activation method and used as adsorbent for methylene blue (MB), the adsorption performance for methylene blue was investigated. The influences of pH, initial MB concentration, adsorption time, adsorption temperature, and the amount of adsorbent on the adsorption performance of Pomelo peel-derived biochar were investigated by static adsorption experiments, and the adsorption kinetics, adsorption isotherms, and adsorption thermodynamics were determined. The results showed that the adsorption capacity of MB was 68.28 mg/g under the condition of adsorbent concentration of 0.6 g/L, pH of 7, methylene blue concentration of 100 mg/L, and adsorption at 50 oC for 180 min. The adsorption process could be better described by the quasi-second-order kinetic equation and Freundlich equation. Adsorption thermodynamics revealed that the adsorption was spontaneous and endothermic. Key words: pomelo peel; biochar; methylene blue; adsorption

    引用本文:張妍杰, 王歡, 蔡玉福, .改性柚子皮生物炭吸附亞甲基藍性能研究[J].化學試劑, 2022, 446):822-827.

     

     

    納米零價鐵吸附法去除廢水中的Pb2+

    左國強*,蘇小莉,劉改云,宋欣宇,張露露

    (濟源職業技術學院 冶金化工系,河南 濟源  459000

     

    摘要:通過液相還原法,采用NaBH4還原Fe2+制備了粒徑約為50 nm的納米零價鐵(nZVI),并應用于含Pb2+廢水,詳細考察了顆粒大小、酸度、溫度、投入量、初始濃度和反應時間對Pb2+去除率的影響。結果表明,過量的NaBH4有利于nZVI網狀結構的生成,也有利于nZVI對溶液中Pb2+的去除,常溫下,調節溶液pH46,nZVI的投加量為0.5 g/L,當Pb2+初始濃度小于200 mg/L時,nZVI可在20 min內完成對Pb2+的去除,當Pb2+的初始濃度為300500 mg/L時,反應時間延長至60 min才能完全去除,而當Pb2+的初始濃度為600 mg/L時,去除率最大僅為84.2%。動力學實驗表明,nZVI對溶液中Pb2+的吸附符合Lagergren準二級動力學模型,其吸附過程受化學吸附控制。LangmuirFreundlich等溫吸附模型對該過程的擬合程度都較高,表明Pb2+的去除過程中單分子吸附和多分子吸附共存。當Pb2+的初始濃度小于10 mg/L時,濾液中的Fe2+濃度低于生活飲用水衛生標準《GB5749—2006》中規定的限量要求,不會對環境造成二次污染。

    關鍵詞:納米零價鐵(nZVI);鉛;吸附;廢水;吸附動力學

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

     

    Research on the Removal of Pb2+ from Wastewater by Nanometer Zero-Valent Iron ZUO Guo-qiang, SU Xiao-li, LIU Gai-yun, SONG Xin-yu, ZHANG Lu-lu (Department of Metallurgy and Chemical Engineering, Jiyuan Vocational and Technical College, Jiyuan 459000, China), Huaxue Shiji, 2022, 44(6)

    AbstractNanoscale zero-valent iron (nZVI) with average particle of 50 nm was synthesized in aqueous solutions by reduction of Fe2+ with NaBH4. Experiment to remove Pb2+ in solution by nZVI was carried out. The effects of particle size, pH, temperature, dosage, initial concentration and reaction time on removal efficiency of Pb2+ were investigated. The results showed that, it was beneficial to the formation of network structure and the removal of Pb2+ in the solution, when the amount of NaBH4 was in large excess. At room temperature, adjust the pH of the solution to 46, and the dosage of nZVI was 0.5 g/L, nZVI could remove Pb2+ in 20 min, while the initial Pb2+ concentration was less than 200 mg/L. However, in order to remove Pb2+ completely, the reaction time was extended to 60 min, when the initial concentration of Pb2+ is 300500 mg/L. When the initial concentration of Pb2+ was 600 mg/L, the maximum removal efficiency was only 84.2%. Kinetic experiments showed that, the adsorption kinetics of Pb2+ on nZVI in solution was in accordance with Lagergren-pseudo -second- order model, which was mainly controlled by chemical adsorption. The adsorption behavior was highly compatible with Langmuir and Freundlich isothermal adsorption models, indicating that removal of Pb2+ was monolayer adsorption coexisting with multi-layer adsorption. When the initial Pb2+ concentration was less than 10 mg/L, the concentration of Fe2+ in the filtrate was lower than the limited demand of Standards for Drinking Water Quality GB5749—2006, which would not cause secondary pollution to the environment.

    Key wordsnanoscale zero-valent iron (nZVI); Pb; adsorption; wastewater;adsorption kinetic

    引用本文:左國強,蘇小莉,劉改云,等. 納米零價鐵吸附法去除廢水中的Pb2+[J]. 化學試劑, 2022, 44(6): 828-834。

     

     

    氯化鐵改性椰殼活性炭去除2,4-二氯苯酚的吸附性能研究

    劉雪平,閆曉樂,張煥,張瀚月,田麗,宋忠賢,毛艷麗,張霞,延旭,康海彥*

    (河南城建學院 河南省水體污染與防治重點實驗室,河南平 頂山  467000

     

    摘要以椰殼活性炭為原料,進行氯化鐵改性,探究其對2,4-二氯苯酚吸附性能影響的研究。通過靜態吸附實驗得到了最佳改性條件,使得2,4-二氯苯酚吸附性能進一步得到提升,并結合實際水體酸堿性探究,對模擬廢水實驗進行了pH探究,進一步優化了材料對實際水體的適用性。研究表明,氯化鐵濃度為0.8mol/L、改性時間為24h條件下改性得到的炭材料(BC-F)吸附性能最佳;吸附劑的最佳使用量應為0.04g吸附過程應在弱酸或堿性環境中進行,在實際水體中實用性較好;且該吸附過程符合準一級動力學和Freundlich等溫吸附方程,以化學吸附為主。

    關鍵詞椰殼活性炭;氯化鐵改性;吸附;2,4-二氯苯酚;動力學

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

     

    Adsorption Performance of FeCl3 Modified Coconut Shell Activated Carbon for the Removal of 2,4-Dichlorophenol LIU Xue-ping, YAN Xiao-le, ZHANG Huan, ZHANG Han-yue, TIAN Li, SONG Zhong-xian, MAO Yan-li, ZHANG Xia, YAN Xu, KANG Hai-yan*Henan Key Laboratory of Water Pollution Control and Rehabilitation, Henan University of Urban Construction, Pingdingshan 467000, China, Huaxue Shiji, 2022, 44(6),

    Abstract: In this study, ferric chloride-modified coconut shell-derived activated carbon (AC) was prepared, the effect of ferric chloride modification on the adsorption performance of 2,4-dichlorophenol was investigated. The optimum modification conditions were obtained through static adsorption experiments, which significantly improved the adsorption performance of 2,4-dichlorophenol. The pH of the simulated wastewater experiment was also investigated in combination with the acidity and alkalinity of actual wastewater to further optimize the applicability of the as-modified material. This study presented that the best adsorption performance of ferric chloride-modified AC was obtained with a dosage of 0.8 mol/L ferric chloride concentration and a modification time of 24 h; also, the adsorption process is suggested to be carried out in a weakly acidic or alkaline environment, which is close to the practical condition in the actual wastewater. Furthermore, the adsorption process was testified to conform to the quasi-level kinetics and Freundlich isothermal adsorption equation that was governed by chemisorption.

    Key words: coconut shell activated carbon; FeCl3 modified; adsorption; 2,4-DCP; Kinetics

    引用本文劉雪平,閆曉樂,張煥,等. 氯化鐵改性椰殼活性炭去除2,4-二氯苯酚的吸附性能研究[J]. 化學試劑,2022,44(6):835-840。

     

     

    板栗殼活性炭對中性紅和活性藍19的吸附行為

    韋琴*,周帆

    (武漢工商學院 環境與生物工程學院,湖北 武漢  430065

     

    摘要:以板栗殼為原料制備板栗殼活性炭,以振蕩時間、pH和溫度3個單因素考察了板栗殼活性炭對中性紅和活性藍19的吸附效果,分析了等溫吸附過程并從吸附動力學角度探討了兩種染料的吸附機理。結果表明:板栗殼活性炭對中性紅染料的最佳吸附條件是pH 4、溫度為35 ℃,振蕩時間為120 min;對活性藍19最佳吸附條件是pH 2、溫度為40 ℃,振蕩時間為150 min。板栗殼活性炭對兩種染料的吸附過程與Freundlich模型擬合度更高,該過程主要是多分子層吸附。用準二級動力學方程(R20. 99)比準一級動力學方程更適合描述板栗殼活性炭對兩種染料的吸附特性。板栗殼活性炭對兩種染料的吸附以化學吸附為主。

    關鍵詞板栗殼活性炭;中性紅;活性藍19;吸附行為;Freundlich模型

    中圖分類號:TQ0      文獻標識碼:A      文章編號:0258-32832022--

     

    Adsorption Behavior of Chestnut Shell Activated Carbon for Neutral red and Active Blue 19 WEI Qin*, ZHOU Fan (College of Environmental and Biological Engineering, Wuhan Technology and Business University, Wuhan 430065, China), Huaxue Shiji, 2022, 44(6),

    Abstract: Herein, activated carbon (AC) was prepared from the chestnut shell. The effect of chestnut shell-derived AC on the adsorption of neutral red and active blue 19 was explored by varying the following parameters including oscillation time, pH, and temperature. The isothermal adsorption process was analyzed and the mechanism for adsorbing the two dyes was discussed from the viewpoint of adsorption kinetics. Results showed that the optimal adsorption conditions for neutral red dye were pH of 4.0, the temperature of 35 ℃, and the oscillation time of 120 min. The optimum adsorption conditions for active blue 19 were pH of 2.0, the temperature of 40 ℃, and the oscillation time of 150 min. The adsorption processes of the two dyes on chestnut shell-derived AC matched better with the Freundlich model, indicating that the process was governed by multi-molecular layer adsorption. Furthermore, the quasi-second-order kinetic equation (R2>0.99) was more suitable than the quasi-first-order kinetic equation to describe the adsorption characteristics, suggesting that these two dyes were chemically adsorbed on chestnut shell-derived AC.

    Key words: chestnut shell activated carbon; neutral red; activated blue 19; the adsorption behavior; Freundlich model

    引用本文:韋琴,周帆. 板栗殼活性炭對中性紅和活性藍19的吸附行為[J]. 化學試劑,2022,44(6): 841-845。

     

     

    CdI2-phen/bpy溶劑熱體系中Cd(II)配合物的合成、晶體結構及熒光傳感性能研究

    朱圣加,陳飛,張柔,付玉,許偉*,羅云杰

    (寧波大學 材料科學與化學工程學院,浙江 寧波  315211)

     

    摘要:在溶劑熱條件下,利用CdI2分別與鄰菲啰啉(phen)、2,2-聯吡啶(bpy)反應得兩例新的Cd配合物Cd(phen)2I2Cd(bpy)2I2。通過X-射線單晶衍射、紅外光譜、熱重分析等方法對其表征。晶體結構分析表明,Cd(II)離子與兩個phenbpy配體上4N原子以及2I原子配位形成畸變的八面體配位,借助π-π堆積和CH···I氫鍵相互作用形成超分子構筑。此外,還研究了配合物Cd(phen)2I2 對不同金屬陽離子的熒光傳感性能,結果表明Fe3+具有出較高選擇性和明顯的熒光猝滅響應。

    關鍵詞:鎘(II)配合物;晶體結構;熒光傳感;Fe3+

    中圖分類號:O652.3        文獻標識碼:A       文章編號:0258-32832022

     

    Synthesis, Crystal Structure and Fluorescence Sensing Properties of Cd(II) Complex in CdI2 -phen/bpy Solvothermal System ZHU Sheng-jia, CHEN Fei, ZHANG Rou, FU Yu, XU Wei*, LUO Yun-jie (School of Material Science Chemical Engineering, Ningbo University, Ningbo 315211, China), Huaxue Shiji, 2022,

    446

    AbstractTwo new Cd complexes: Cd(phen)2I2 and Cd(bpy)2I2 were prepared under solvothermal conditions by reacting CdI2 with 1,10-phenoline (phen) and 2,2 '-bipyridine (bpy), respectively. The complexes were characterized by using IR, TG, and X-ray single crystal diffraction. The crystal structure analysis revealed that each Cd(Ⅱ) ion is coordinated with four N atoms from the two phen or bpy ligands, and two I atoms are forming a distorted octahedral coordination geometry. The supramolecule was constructed via π-π stacking and CH··I hydrogen bond interactions. The fluorescent sensing of complex 1 to a series of metal cations was investigated. The results showed that Fe3+ ion had higher selectivity and apparent fluorescence quenching response.

    Key wordsCd(II) complex; crystal structure; fluorescent sensing; Fe3+

    引用本文:朱圣加,陳飛,張柔,等. CdI2-phen/bpy溶劑熱體系中Cd(II)配合物的合成、晶體結構及熒光傳感性能研究[J]. 化學試劑,2022,446846-849.

     

     

    銅濾膜基環丙沙星分子印跡復合膜的制備、吸附性能及SERS活性研究

    張杰a,唐麗a,卜明a,馬玉坤b,王海君*a,王靜a

    (齊齊哈爾醫學院 a.藥學院,b.醫藥科學研究院,黑龍江 齊齊哈爾  161006)

     

    摘要:為實現環丙沙星的快速識別,制備了可以選擇性吸附環丙沙星的具有表面增強拉曼活性的銅濾膜基分子印跡復合膜。以環丙沙星為模板分子,銅濾膜為基膜,甲基丙烯酸為功能單體,乙二醇二甲基丙酸酯為交聯劑,偶氮二異丁腈為引發劑,甲醇、二氯甲烷的混合溶劑為反應溶劑和致孔劑,通過自由基聚合制備了分子印跡復合膜。紅外光譜表征膜的結構,顯微鏡表征膜的形貌。對膜的吸附性能和表面增強拉曼散射活性進行了系統研究。復合膜為一層白色、連續、均勻的薄膜,表面光滑無裂紋。120 min左右膜對環丙沙星的吸附達到平衡,最大吸附量為8.11 μg/cm2,至少可以重復使用6次,印跡因子為4.0。膜具有表面增強拉曼散射活性,對環丙沙星檢測的最低濃度為1.00×10-8 mol/L。

    關鍵詞:環丙沙星;分子印跡;復合膜;銅濾膜;表面增強拉曼散射

    中圖分類號:O657.1      文獻標識碼:A      文章編號:0258-32832022--

     

    Preparation and Adsorption Properties of Ciprofloxacin Molecularly Imprinted Composite Membrane with SERS Activity based on Copper Filter Membrane ZHANG Jiea, TANG Lia, BU Ming a, MA Yu-kun b, WANG Hai-jun*a, WANG Jing a (a.College of Pharmacy; b. Research Institute of Medicine & Pharmacy, Qiqihar Medical University, Heilongjiang Qiqihar 161006), Huaxue Shiji, 2022, 44(6),

    Abstract: In order to realize the rapid recognition of ciprofloxacin (CIP), a molecularly imprinted composite membrane (RC-MIM) with Surface-Enhanced Raman Scattering (SERS) activity based on copper filter membrane was prepared, which could selectively absorb CIP. Using CIP as the template molecule, copper filter membrane as the base membrane, methacrylic acid (MAA) as the functional monomer, and ethylene glycol dimethylpropionate (EGDMA) as the crosslinking agent, azodiisobutyronitrile (AIBN) as the initiator, mixed solvent (methanol and dichloromethane) respectively as the reaction solvent and porogen, RC-MIM was prepared via free radical polymerization. The structure of the RC-MIM was characterized by infrared spectroscopy and the morphology by optical microscope. The adsorption performance and SERS activity of the membrane were systematically studied, revealing that RC-MIM was a white, continuous, and uniform membrane with a smooth surface and free of crack. The adsorption of ciprofloxacin on the membrane reached equilibrium after about 120 min, and the maximum adsorption capacity was 8.11 μg/cm2. The membrane could be reused at least 6 times, and the imprinting factor was 4.0. Due to the SERS activity of RC-MIM, the minimum detection concentration of ciprofloxacin was 1.00×10-8 mol/L.

    Key words: ciprofloxacin; molecularly imprinted; composite membrane; copper filter membrane; Surface-Enhanced Raman Scattering

    引用本文:張杰,唐麗,卜明,等. 銅濾膜基環丙沙星分子印跡復合膜的制備、吸附性能及表面增強拉曼散射活性研究[J]. 化學試劑,2022,446850-857.

     

     

    過渡金屬取代磷鉬酸催化劑的制備及氧化脫硫性能研究

    高爽,張俊茹,李佳其,于悅,韓璐,肖舒寧,袁運鴻,陳曉陸*

    (營口理工學院 化學與環境工程學院 遼寧省化學助劑合成與分離重點實驗室,遼寧 營口  115014

     

    摘要:以有機氨功能化的SBA-15為載體,制備過渡金屬取代的磷鉬酸PMo11M, M = Fe, Co, Cu)負載型催化劑。利用XRD、FT-IR、BET、TEM、TG等手段對催化劑結構進行表征,結果表明,過渡金屬成功負載到載體SBA-15上;催化劑的整體結構沒有發生明顯改變,催化劑活性組分均勻地分散在介孔SBA-15的表面和孔道中。結合XPS數據和氧化脫硫實驗結果,發現催化劑表面的氧空位,可以活化活性氧物種,有助于催化劑脫硫性能的提升。以二苯并噻吩(DBT)為底物,進行氧化脫硫反應,考察引入的過渡金屬對催化劑結構的改變和催化活性的影響。得到Co取代催化劑(PMo11Co-NH2-SBA-15)的脫硫效果最好,DBT的轉化率達到91.15%。PMo11Co-NH2-SBA-15催化劑具有良好的循環穩定性。

    關鍵詞:過渡金屬;氧化脫硫;SBA-15;磷鉬酸;二苯并噻吩

    中圖分類號:O643.3            文獻標識碼:A    文章編號:0258-32832022

     

    Preparation of Transition Metal Substituted Phosphomolybdic Acid and Catalytic Performance in Oxidation Desulfurization GAO Shuang, ZHANG Jun-ru, LI Jia-qi, YU Yue, HAN Lu, XIAO Shu-ning, YUAN Yun-hong, CHEN Xiao-lu* (Liaoning Key Laboratory of Chemical Additive Synthesis and Separation, Department of Chemical Engineering, Yingkou Institute of Technology, Yingkou 115014, China), Huaxue Shiji, 2022, 44(6)

    AbstractThe supported catalysts of transition metal-substituted phosphomolybdic acid (PMo11M, M = Fe, Co, Cu) were prepared using organic ammonia-modified SBA-15 substrate. The as-made catalysts were characterized by using XRD, FT-IR, BET, TEM, and TG. Results showed that the transition metals have been successfully loaded on the organic ammonia-modified SBA-15 support. The overall structure of the catalyst has not changed apparently, and the active components of the catalyst were uniformly distributed on the surfaces of mesopores of SBA-15. Combined with XPS data and oxidative desulfurization experimental results, it was found that the oxygen vacancy on the catalyst surface can efficiently generate active oxygen species, which is helpful to improve the desulfurization performance. The oxidative desulfurization reaction was carried out with dibenzothiophene (DBT) as a substrate. The effects of transition metals on the structure and catalytic activity of the catalysts were investigated. It was found that the PMo11Co-NH2-SBA-15 catalyst possessed the best desulfurization performance, achieving a conversion of 91.15% for DBT and very good cycling stability.

    Key words: transition metal; oxidation desulfurization; SBA-15; phosphomolybdic acid; dibenzothiophene

    引用本文:高爽,張俊茹,李佳其,等. 過渡金屬取代磷鉬酸催化劑的制備及氧化脫硫性能研究[J]. 化學試劑, 2022, 44(6): 858-864。

     

     

    【分離提取技術】

    正交試驗法優化復方玉液湯提取工藝及對小鼠的急性毒性研究

    張文祥,郭鳳,陳鵬德,吳思宇,姚藍*

    (新疆醫科大學 中醫學院,新疆 烏魯木齊  830057

     

    摘要:優化玉液湯的提取工藝并考察其對小鼠的急性毒性。通過設置3個考察因素:料液比、藥材浸泡時間、提取時間,確立3個評價指標:總皂苷含量、干膏得率、總多糖含量。在此基礎上設計正交試驗并根據綜合評分結果確定玉液湯的最佳提取工藝。按此提取工藝對玉液湯進行回流提取,所得藥液進行小鼠的急性毒性研究。小鼠給藥后連續觀察14 d,在此期間內記錄小鼠的基本狀態、檢測各組小鼠血常規和生化指標;取小鼠心、肝、脾、肺、腎計算臟器指數,HE染色觀察各組小鼠臟器病理變化。最終確定玉液湯水提工藝最佳條件為:料液比 110g/L)、藥材浸泡1 h、回流 2.5 h。小鼠連續給藥14 d內未出現中毒和死亡情況,且給藥組與對照組比較,體質量、攝食量、攝水量、血常規、生化指標和各臟器的臟器指數均未有統計學差異;各組小鼠主要臟器病理學未見異常。優化條件下的玉液湯水提工藝含量穩定,且服用安全無毒。

    關鍵詞:玉液湯;水提工藝;急性毒性;總皂苷;干膏得率;總多糖;

    中圖分類號:R284.2    文獻標識碼:A    文章編號:0258-3283202107

     

    Orthogonal Experiment of Optimizing the Extraction Process of Compound Yuye Decoction and Study on Its Acute Toxicity to Mice ZHANG Wenxiang, GUO Feng, CHEN Pengde, WU Siyu, YAO Lan (College of Traditional Chinese Medicine, Xinjiang Medical University, Urumqi 830057, China) Huaxue Shiji, 2021, 44(6)

    Abstract: The objective of this work is to optimize the extraction process of nectar soup and explore its acute toxicity on mice. Methods include studying the liquid/material ratio, the soaking time of medicinal herbs, and the extracting time. The evaluation factor of this study is the content of total saponins, the dry ointment yield, total polysaccharide content. The best extraction process of nectar soup was obtained based on the design of an orthogonal experiment. Reflux extraction of Yuye decoction was carried out according to the abovementioned extraction process, and the acute toxicity of the solution was studied using mice. The mice were observed for 14 days after administration. During this period, the basic state of the mice, blood routine, and biochemical indexes of each group were recorded. The heart, liver, spleen, lung, and kidney of mice were collected to calculate the viscera index, and the pathological changes of viscera were observed by HE staining. Results indicated that the optimal extraction conditions of Yuye decoction were the solid-liquid ratio of 1:10, soaking for 1h, and reflux for 2.5 h. No poisoning or death of mice occurred within 14 days of continuous administration, meanwhile, there were no statistically significant differences in body weight, food intake, water intake, blood routine, biochemical indexes, and organ indexes between the administration group and the control group. No abnormality was found in the pathology of the main organs in each group. In conclusion, the content of Yuye decoction is stable and safe under our optimized conditions.

    Key words: Yuye decoction; water extraction process; acute toxicity;total saponin ;dry paste yield;total polysaccharides;

    引用本文:張文祥,郭鳳,陳鵬德,等. 正交實驗法優化復方玉液湯提取工藝及對小鼠的急性毒性研究[J]. 化學試劑, 2022, 44(6): 865-871。

     

     

    【電化學和新能源】

    基于石墨烯金粒子的腎上腺素分子印跡電化學傳感器研究

    孫晨陽,康天放*,魯理平,程水源

    (北京工業大學 區域大氣復合污染防治北京市重點實驗室 環境與生命學部,北京  100124)

     

    摘要:制備了石墨烯和金納米粒子的復合物(GS-AuNP),用掃描電鏡對其進行了表征。將該復合物和殼聚糖(CS)依次修飾到玻碳電極(GCE)表面,制得修飾電極(CS/GS-AuNP/GCE)。以3-氨基苯硼酸鹽酸鹽(APBA)為單體,腎上腺素(EP)分子為模板,采用循環伏安法在該修飾電極表面進行電聚合,制備了分子印跡聚合物(MIP)膜,洗脫掉模板分子EP后得到分子印跡傳感器(MIP/CS/GS-AuNP/GCE),用于腎上腺素的檢測。溶液中的EP可與傳感器表面的MIP特異性結合,在富集一定時間后,通過差分脈沖伏安法(DPV)檢測溶液中EP的濃度。在優化的實驗條件下,DPV峰電流分別在1.0×10-71.0 × 10-5 mol/L1.0 ×10-51.0 × 10-4 mol/L EP的濃度范圍內隨EP濃度的增大而呈線性增大,檢出限為5×10-8 mol/L。制備的MIP/CS/GS-AuNP/GCE傳感器成功應用于實際樣品中的腎上腺素含量檢測,回收率在98%105%之間。

    關鍵詞:GS-AuNP復合物;電化學傳感器;分子印跡聚合物;電聚合;腎上腺素

     

    Molecularly Imprinted Electrochemical Sensor for Epinephrine Based on the Composite of Graphene and Gold Particles SUN Chen-yang, KANG Tian-fang*, LU Li-ping, CHENG Shui-yuan ( Key Laboratory of Beijing on Regional Air Pollution Control, Faculty of Environment and Life, Beijing University of Technology, Beijing 100124, China), Huaxue Shiji , 2022 , 44(6)

    Abstract: The composite of the graphene sheet (GS) and gold nanoparticles (AuNP) was prepared and characterized by using scanning electron microscope. The as-made composite and chitosan (CS) were modified onto the surface of a glassy carbon electrode in sequence to prepare a modified electrode (denoted as CS/GS-AuNP/GCE). Using 3-aminophenylboratic acid (APBA) as monomer and epinephrine (EP) molecules as a template, electropolymerization was carried out on the surface of the modified electrode by cyclic voltammetry. After eluting the template EP, the molecularly imprinted electrochemical sensor (MIP/CS/GS-AuNP/GCE) was obtained. EP can specifically bind to the MIP on the surface of the sensor. After a certain period of enrichment, the concentration of EP in the solution can be detected by differential pulse voltammetry (DPV). Under optimized experimental conditions, the DPV peak current increased linearly with the increase of EP concentration in the ranges of 1.0 × 10-7 ~ 1.0 × 10-5 mol/L and 1.0 × 10-5 ~ 1.0 × 10-4 mol/L. The detection limit is 5×10-8 mol/L. In conclusion, the MIP/CS/GS-AuNP/GCE sensor was successfully applied to the detection of EP in actual samples with a good recovery rate of 99.9% to 104.7%.

    Key wordsGS-AuNP composite; electrochemical sensor; molecularly imprinted polymer; electropolymerization; epinephrine

    引用本文:孫晨陽,康天放,魯理平,等. 基于石墨烯金粒子的腎上腺素分子印跡電化學傳感器研究 [J]. 化學試劑, 2022, 44(6) :872-879。

     

     

    茜素綠染料的Ti/PbO2電極與Ti/IrO2+Ta2O5電極催化降解比較研究

     

    沈宏*1,章維維2,姚春冀1,楊葉1,范宏亮1,鞠莉1

    1. 杭州醫學院公共衛生學院,浙江 杭州 310007;2. 杭州嘉澍環境監測有限公司,浙江 杭州 311000

     

    摘要:主要研究了Ti/PbO2電極與Ti/IrO2+Ta2O5電極催化氧化體系對茜素綠(AG)染料廢水的催化降解效果。結果表明,當AG初始濃度100 mg/L,電解質濃度0.1 mol/L,電流密度30 mA/cm2,pH5.86,處理70 min后,Ti/PbO2電極和Ti/IrO2+Ta2O5電極催化氧化體系對AG和化學需氧量(COD)的處理效率分別可高于81.4%51.6%。相較于Ti/IrO2+Ta2O5電極,具有四棱錐形結構晶粒的Ti/PbO2電極穩定性較高,且Ti/IrO2+Ta2O5電極表面由于存在干泥狀裂痕結構,工作過程中易出現表面局部剝落現象,形成的TiO2鈍化膜則會導致槽壓升高和電極活性下降,影響體系的催化氧化效率。

    關鍵詞:形穩電極(DSA);Ti/PbO2電極;Ti/IrO2+Ta2O5電極;茜素綠;電催化降解

    中圖分類號:O643.3      文獻標識碼:A      文章編號:0258-32832022--

     

    Degradation of Alizarin Green (AG) by Ti/PbO2 Electrode and Ti/IrO2+Ta2O5 Electrode SHEN Hong*1, ZHANG Wei-wei2, YAO Chun-ji1, YANG Ye1, FAN Hong-liang1, JU Li1(1. College of Public Health, Hangzhou Medical College, Hangzhou 310007, China; 2. Hangzhou Jiashu Environmental Monitoring Co., Ltd., Hangzhou 311000, China), Huaxue Shiji, 2022, 44(6),

    Abstract: In this work, the degradation efficiencies of alizarin green (AG) by Ti/PbO2 electrode and Ti/IrO2+Ta2O5 electrode were studied. The optimal degradation conditions were obtained: initial AG concentrations of 100 mg/L, Na2SO4 concentrations of 0.1 mol/L, the current density of 30 mA/cm2, and pH of 5.86. After being treated under this specific optimal condition for 70 min, the removal rates of AG and COD were higher than 81.4% and 51.6%, respectively. Compared with Ti/IrO2+Ta2O5 electrode with a mud-cracked surface, the Ti/PbO2 electrode possessed higher stability due to its pyramid crystal structure. Because of the surface spalling phenomenon observed during the degradation experiments, passivated TiO2 film was formed, leading to the increase of cell voltage and degraded electrocatalytic oxidation capability.

    Key words: dimensionally stable anode (DSA); Ti/PbO2 electrode; Ti/IrO2+Ta2O5 electrode; alizarin green (AG); electrocatalytic degradation

    引用本文:沈宏,章維維,姚春冀,等. 茜素綠染料的Ti/PbO2電極與Ti/IrO2+Ta2O5電極催化降解比較研究[J]. 化學試劑,2022,446):880-887.

     

     

    基于Nafion/GSH-Fe3O4@Cs/Pt/GCE檢測丙烯酰胺

    尚平*1,楊永2,趙榮敏1,崔文廣3

    1. 石家莊職業技術學院 食品與藥品工程系,河北 石家莊  050081;2. 石家莊職業技術學院 學生工作部,河北 石家莊  050081;3. 石家莊學院 化工學院,河北 石家莊  050035

     

    摘要:制備Nafion/還原性谷胱甘肽-四氧化三鐵@//玻碳電極(Nafion/Glutathione-ferric oxide@Carbon/ Platinum/Glassy carbon electrode, Nafion/GSH-Fe3O4@Cs/Pt/GCE)傳感器,對丙烯酰胺(Acrylamide, AM)進行定量分析。合成了核殼結構的四氧化三鐵@碳納米復合材料(Ferric oxide@Carbon nanocomposites, Fe3O4@Cs),并在此基礎上負載鉑納米粒子(Platinum nanoparticles, Pt),制備新型的Fe3O4@Cs/Pt納米復合材料。以還原性谷胱甘肽(Glutathione, GSH)為探針,在Fe3O4@Cs/Pt的基礎上,制備了Nafion/GSH-Fe3O4@Cs/Pt/GCE傳感器。通過對GSH固載量、Nafion濃度、加成時間、加成溫度等條件的優化確定傳感器的最佳工作條件。研究發現,Fe3O4@Cs/Pt具有良好的導電性和生物相容性,能有效提高傳感器的靈敏度;AM濃度負對數與其與GSH間加成率在1×10-101×10-5 mol/L呈良好的線性關系,線性方程為Y =     -6.025X + 73.632(XAM濃度的負對數),R2=0.9974,檢出限為5.624×10-11 mol/L,且該傳感器短期穩定性較好。該方法簡單、方便可用于丙烯酰胺的定量分析。

    關鍵詞:納米粒子;還原性谷胱甘肽;丙烯酰胺;傳感器;檢測

    中圖分類號:TS207.7   文獻標識碼:A     文章編號:0258-32832022

     

    Detection of Acrylamide Based on Nafion/GSH-Fe3O4@Cs/Pt/GCE SHANG Ping*1, YANG Yong2, ZHAO Rong-min1, CUI Wen-guang3 (1. Department of Food and Drug Engineering, Shijiazhuang University of Applied Technology, Shijiazhuang 050081, China; 2.Department of Student Affairs, Shijiazhuang University of Applied Technology, Shijiazhuang 050081, China; 3.College of Chemical Engineering, Shijiazhuang University, Shijiazhuang 050035, China), Huaxue Shiji, 2022, 44 (6)

    Abstract: Nafion/Glutathione-Ferric oxide@carbon/Platinum/Glassy carbon electrode, (Nafion/GSH-Fe3O4@Cs/Pt/GCE) sensor was prepared for the quantitative analysis of acrylamide (AM). Platinum nanoparticles (Pt) were loaded onto the core-shell structured Fe3O4@Cs nanocomposites to obtain the Fe3O4@Cs/Pt composites. Afterward, the Nafion/GSH-Fe3O4@Cs/Pt/GCE sensor was prepared based on Fe3O4@Cs/Pt using glutathione (GSH) as a probe molecule. The optimum working conditions of the as-made sensor were determined by optimizing the parameters such as the fixed GSH loading, Nafion concentration, addition time, and addition temperature, et al. The results showed that the Fe3O4@Cs/Pt had a good conductivity and biocompatibility, thus could effectively improve the sensor sensitivity. A good linear relationship between the negative logarithm of AM concentration and its addition rate with GSH was obtained in a range of 1×10-10 ~ 1×10-5 mol/L, the linear equation was Y=-6.025X+73.632 (X was the negative logarithm of AM concentration), R2= 0.9974, and the detection limit was 5.624×10-11 mol/L. The sensor also showed very good stability in the short term. Our method is simple and convenient and can be used for the quantitative analysis of acrylamide.

    Key words: nanoparticles; glutathione; acrylamide; sensor; detection

    引用本文:尚平,楊永,趙榮敏,等. 基于Nafion/GSH-Fe3O4@Cs/Pt/GCE檢測丙烯酰胺[J]. 化學試劑,2022,446888-893。

     

     

    【分析與測試】

    醇類香料單體在加熱卷煙中的轉移行為研究

    徐如彥1,朱夢薇2,饒先立1,王鳴1,胡玉軒1,李朝建1,師東方1,石懷斌1,鄭曉云*1

    (1. 江蘇中煙工業有限責任公司,江蘇 南京  210019;2. 鄭州輕工業大學 食品與生物工程學院,河南  鄭州 450002)

     

    摘要:為研究醇類香料單體在加熱卷煙中的轉移規律,將28種醇類香料單體添加到加熱卷煙煙芯中,建立了加熱卷煙煙芯中醇類香料單體的檢測分析方法,并分析了醇類香料單體在加熱卷煙抽吸前后的轉移行為。結果顯示:貯存期間,28種醇類香料單體的煙芯持留率為7.13%91.70%、降溫段遷移率為09.10%、濾嘴遷移率為030.76%、散失率為1.83%81.65%。抽吸過程中,28種醇類香料單體的主流煙氣粒相物轉移率為2.29%34.02%、煙芯殘留率為1.17%24.01%、濾嘴截留率為8.27%29.46%。互為同系物的醇類單體遵守隨著分子量增大、沸點增高,煙芯持留率、向主流煙氣粒相物轉移率增加,散失率減小的規律?;橥之悩嬻w的醇類單體遵循物質結構穩定性越好、沸點越高,煙芯持留率和向主流煙氣粒相物轉移率越高,散失率越小的規律。香葉醇、橙花醇、肉桂醇的煙芯持留率高、散失率小、向主流煙氣粒相物轉移率高,適用做加熱卷煙香精調配香原料。

    關鍵詞:電加熱卷煙;醇類香料;持留率;遷移率;轉移率;截留率;散失率

    中圖分類號:TS411                文獻標識碼:A     文章編號:0258-32832022

     

    Study on Transfer Behavior of Alcohol Flavor Monomers in Heated Cigarettes XU Ru-yan1, ZHU Meng-wei2, RAO Xian-li1, WAN Ming1, HU Yu-xuan1, LI Chao-jian1, SHI Dong-fang1, SHI Huai-bin1, ZHENG Xiao-yun*1 (1. China Tobacco Jiangsu Industrial Co., Ltd., Nanjing 210019, China; 2. College of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450002, China), Huaxue Shiji , 2022 , 44(6)

    Abstract: In order to study the transfer principle of alcohol flavor monomers in heated cigarettes, 28 kinds of alcohol flavor monomers were added into heated cigarette cores, and a method for the detection and analysis of alcohol flavor monomers in heated cigarette cores was established. The transfer behavior of alcohol flavor monomers before and after smoking was analyzed. Results showed that during the storage period, the retention rate of the cigarette core of 28 kinds of alcohol flavor monomers was 7.13%~91.70%, the mobility of the cooling section was 0~9.10%, the mobility of the filter rod was 0~30.76%, and the loss rate was 1.83%~81.65%. During the smoking process, the mainstream smoke particle-phase transfer rate of 28 alcohol flavor monomers was 2.29%~34.02%, the residual rate of cigarette core was 1.17%~24.01%, and the rejection rate of filter rod was 8.27%~29.46%. Alcohol monomers that are homologous to each other obey the law that with the increase of the molecular weight and the boiling point, the retention rate of the smoke core and the rate of transferring to the mainstream smoke particle-phase matter increase, while the loss rate decreases. Alcohol monomers that are isomers of each other follow the principle that the better the stability of the material structure and the higher the boiling point, the higher the retention rate of the smoke core and the transfer rate of particulate matter to the mainstream smoke will be, also the smaller the loss rate. As revealed by our study, the geraniol, nerol, and cinnamyl alcohols have relatively high core retention rates, low loss rates, high transfer rates to mainstream smoke particles, and are suitable choices for heating cigarette flavoring and flavoring raw materials.

    Key wordsheat-not-burn product;alcohol spices;retention rate;mobility rate;transfer rate;rejection rate;loss rate

    引用本文:徐如彥,朱夢薇,饒先立,等. 醇類香料單體在加熱卷煙中的轉移行為研究[J]. 化學試劑,2022,446894-903。

     

     

    HPLC測定人血清中三種抗HIV

    龔愛琴

    (揚州工業職業技術學院 化學工程學院,江蘇 揚州  225127

    摘要:建立一種用高效液相色譜法同時測定人血清中三種抗HIV藥(拉米夫定、富馬酸替諾福韋二吡呋酯和ACC007)的新方法。測定時采用Dionex C185 μm,4.60 mm×250 mm)色譜柱;流動相為甲醇:水,采用梯度洗脫方式,流速為0.6 mL/min;檢測波長為260 nm。結果發現在優化色譜條件下,拉米夫定、富馬酸替諾福韋二吡呋酯和ACC007的線性范圍分別為2.07103.5、5.15206.0、2.0651.45 μg/mL,檢出限分別為1.05、2.60、1.03 μg/mL,加樣回收率分別為98.54%103.8%、98.29%102.5%、101.7%108.4%。本方法簡單快速,可用于人血清中三種藥物含量的測定。

    關鍵詞:抗 HIV藥;拉米夫定;富馬酸替諾福韋二吡呋酯;ACC007;HPLC

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

     

    Simultaneous Determination of Three Anti HIV Drugs in Serum by HPLC GONG Ai-qin (Chemical Engineering Institute, Yangzhou Polytechnic Institute, Yangzhou 225127, China), Huaxue Shiji,2021,44(6), ~

    Abstract: In this work, a new method for the simultaneous determination of lamivudine, tenofovir disoproxil fumarate, and ACC007 in human serum was developed with high-performance liquid chromatography (HPLC). A Dionex C18 chromatographic column (5 μm, 4.60 mm*250 mm) was used with the methanol-water mobile phase (gradient elution) and a flow rate of the mobile phase of 0.60 mL/min. The detection wavelength was 260 nm. Under the optimized chromatographic conditions: the linear ranges of lamivudine, tenofovir disoproxil fumarate and ACC007 were 2.07 ~ 103.5, 5.15 ~ 206.0, 2.06 ~ 51.45 μg/mL, respectively; the detection limits for lamivudine, tenofovir disoproxil fumarate and ACC007 were 1.05, 2.60, and 1.03 μg/mL, respectively; and accordingly, the recoveries in the spiked samples were 98.54%~103.8%, 98.29%~102.5%, and 101.7%`108.4%, respectively. The proposed method is simple and fast and can be used for the determination of these three drugs in human serum.

    Key words: Anti HIV drug, lamivudine, tenofovir disoproxil fumarate, ACC007, HPLC

    引用本文:龔愛琴. HPLC測定人血清中三種抗HIV [J]. 化學試劑, 2022, 44(6): 904-907。

     

     

    中緬管輸進口原油微量元素分析研究

     

    李秀林1,韓家曦2,劉汗青1,武夢琦1,王群威3,楊新周*4

    (1.  瑞麗海關,云南 瑞麗  678600;2. 瑞麗中檢檢驗認證有限公司,云南 瑞麗  678600;3. 寧波海關技術中心,浙江 寧波  315010;4. 德宏師范高等??茖W校 理工學院,云南 芒市  678400

     

    摘要:測定中緬管輸原油中9種元素,為原油國別鑒定、原油溯源提供依據,為中緬管輸原油運輸及下游的冶煉過程提供科學基礎。采用灰化堿熔-電感耦合等離子體發射光譜法對中緬管輸原油中9種元素進行測定。結果表明,中緬管輸進口5個國家的原油中含有Al、Si、V、Ni、Fe、Na、Ca、Zn 8種元素,原油中均未檢出P元素。8種元素中Fe含量占比75.73%,V含量占比10.87%,Si含量占比4.73%,Ni含量占比4.18%,其余元素占比4.56%。通過分析得出,中緬管輸進口的5國原油Si/V、Ni/V比值均小于1,呈現出海相原油的特性,不同油種元素的含量存在一定差異,且有一定的規律性,各油種間Ni/V、Si/V比值相差不大,Fe/V比值的波動較大,可以按此來對5個國家原油進行溯源。

    關鍵詞:灰化堿溶;電感耦合等離子體發射光譜法;中緬管輸原油;元素 ?

    中圖分類號O657.3      文獻標識碼 A      文章編號:0258-32832022

     

    Analysis of Trace Elements in Crude Oil Imported from China-Burma Pipeline LI Xiu-lin1, HAN Jia-xi2, LIU Han-qing1, WU Meng-qi1, WANG Qun-wei3,YANG Xin-zhou *4 (1. Ruili Customs, Ruili 678600, China; 2.Ruili Inspection and Certification Co, LTD, Ruili 678600, China; 3. Ningbo Customs Technology Center, Ningbo, Zhejiang 315010; 4.Dehong Teachers College College of Science and Technology, Mangshi 678400, China), Huaxue Shiji, 2022, 44(6)

    Abstract: The determination of nine elements in crude oil transported by China-Myanmar pipeline provides a basis for crude oil identification and traceability, and provides a scientific basis for crude oil transportation and downstream smelting process. Nine elements in crude oil from China-Myanmar pipeline were determined by ashlized alkali fusion inductively coupled plasma emission spectrometry. Eight elements, such as Al, Si, V, Ni, Fe, Na, Ca and Zn, were detected in the crude oils from the five countries imported from the China-Myanmar pipeline. but P element was not detected in the crude oils. The contents of Fe, V, Si, Ni and other elements are 75.73%, 10.87%, 4.73%, 4.18% and 4.56% respectively.Through analysis, the sino-burmese pipeline crude oil imports of five countries Ni/V and Si/V ratio is less than 1, presents the characteristics of crude oil at sea, oil of different kinds of element contents in there is a difference, and has the certain regularity, between each kind of Ni/V and Si/V ratio were similar, the Fe/V ratio of volatile, can according to the five countries of crude oil for traceability.

    Key words: ashing alkali soluble; inductively coupled plasma atomic emission spectrometry; the China-Myanmar pipeline carries crude oil; element

    引用本文:李秀林,韓家曦,劉汗青,等.中緬管輸進口原油微量元素分析研究[J].化學試劑,2022,446908-914.

     

     

    利用不穩定Konig體系的中間產物光度法快速測定水中氰化物

    李曉惠*,劉海軍,許艷廣

    (遼寧科技學院 藥化學院,遼寧 本溪  117004)

     

    摘要:以異煙酸、雙甲酮分別作為Konig反應的開環、縮合試劑,產生的聚甲炔染料在該異煙酸-雙甲酮體系中易分解,該體系為不穩定的Konig體系,但其中間產物具有較高的摩爾吸收系數(ε,采用分光光度法獲得其中間產物的At曲線,相應建立了快速測定氰化物的新方法。在擬定的實驗條件下,該體系的中間產物在531 nm處產生最大吸收,ε2.36 × 104 L/(mol·cm),其At曲線呈近似平頂峰形,氰化物濃度在0.0100.800 mg/L范圍內與At曲線中的Amax呈良好的線性關系(R = 0.9998,單個樣品的測試時間小于5 min。方法用于焦化廢水中氰化物的測定,回收率在97.9%101.1%之間,RSD1.5%,其測定值與標準方法的測定值吻合,該研究為將Konig反應拓展應用至不穩定體系提供技術參考。

    關鍵詞:不穩定Konig體系;雙甲酮;中間產物;分光光度法;氰化物;測定

    中圖分類號:O657.32; X832          文獻標識碼:A          文章編號0258-32832022

     

    Rapid Determination of Cyanide in Water by Spectrophotometry with Intermediate Product of Unstable Konig System LI Xiao-hui*, LIU Hai-jun, XU Yan-guang (Department of Biomedical and Chemical Engineering, Liaoning Institute of Science and Technology, Benxi 117004, China), Huaxue Shiji, 2022, 44(6)

    Abstract: In this study, isonicotinic acid and dimedone were used as the ring-opening reagent and condensation reagent of the Konig reaction, respectively. The in situ produced polymethine dye was easily decomposed in the isonicotinic acid-dimedone system which can be determined as an unstable Konig system. However, the intermediate product had a higher molar absorption coefficient (ε), the A~t curve of the intermediate product was obtained by using a new method based on spectrophotometry for the rapid determination of cyanide. In the given experimental condition, the intermediate product of the system has a maximum absorption at 531 nm, featuring an ε of 2.36 × 104 L·mol-1·cm-1. The A~t curve is approximately flat-top peak shaped, the cyanide concentration is in a good linear relationship with the Amax of A~t curve (R = 0.9998) within the range of 0.010 ~ 0.800 mg/L, the testing time of a single sample is less than 5 min. The recovery of our method was between 97.9% ~ 101.1% and the RSD was less than 1.5% when applied to determine the cyanide in coking wastewater, the measured values were in good agreement with that of the standard method. Our study provides technical references for extending the application of the Konig reaction to unstable systems.

    Key wordsunstable Konig system; dimedone; intermediate product; spectrophotometry; cyanide; determination

    引用本文:李曉惠, 劉海軍, 許艷廣. 利用不穩定Konig體系的中間產物光度法快速測定水中氰化物[J].化學試劑, 2022, 44(6)915-919.

     

     

    【標準物質與標準品】

    土壤基質中不同目標濃度重金屬標準樣品的研制

    陳晉,徐冬梅,唐曉菲,張敏*?

    (安徽省生態環境監測中心,安徽 合肥 230071

     

    摘要:介紹了一種土壤重金屬標準樣品的研制過程。土壤樣品經勻漿、干燥、研磨、混勻分瓶包裝后,用X射線熒光光譜法對土壤標準樣品進行了均勻性、穩定性檢驗,同時對制備的標準樣品進行了定值和不確定度評估。試驗結果表明:土壤標準樣品均勻性良好,各元素和氧化物的瓶間均勻性不確定度ubb范圍為0.02 mg/kg0.043%;在常溫避光保存條件下,該土壤標準樣品在為期12個月的穩定性檢驗過程中無不穩定變化趨勢;再處理過程對土壤的性質幾乎沒有影響。該方法是一種簡單、有效的制備目標濃度、特定污染因子土壤重金屬標準樣品的方法。

    關鍵詞:X射線熒光光譜法;重金屬;土壤;標準樣品;目標濃度

    中圖分類號:X833      文獻標識碼:A      文章編號0258-32832022--

     

    Development of Reference Materials for Heavy Metals in Soil Matrix CHEN Jin, XU Dong-mei, TANG Xiao-fei, ZHANG Min*(Anhui Eco-Environment Monitoring Center, Hefei 230071, China), Huaxue Shiji, 2022, 44(6),

    AbstractThe method for the preparation of two heavy metals standard materials with different targeting concentrations in soils matrix has been developed. The samples were prepared by a compound process, including the steps of mixing, drying, grounding, and packing; followed by, homogeneity testing and stability testing were conducted. The value of the standard materials was determined by ICP-OES, ICP-MS, and AFS. The soil standard materials exhibited good homogeneity and stability. Additionally, the uncertainty of the uniformity between bottles (ubb) was 0.02 mg/kg~0.043%, indicating very good uniformity. The standard materials can be stably stored at room temperature for over 12 months without detectable unstable tendency. The reprocessing process exhibited negligible influence on the properties of the standard soil materials. Our method paves a reliable foundation for the development of standard soil materials for simulating heavy metals in the soil matrix.

    Key wordsX-ray fluorescence spectrometry; heavy metals; soil; reference materials

    引用本文:陳晉,徐冬梅,唐曉菲,等. 土壤基質中不同目標濃度重金屬標準樣品的研制[J]. 化學試劑,2022,446):920-925.

     

     

    【合成與工藝技術】

    2-1,3-二氫異苯并呋喃)-1-苯乙酮類衍生物的合成

    趙美玲1,2, 劉芊芊2, 張翠蘭2, 龍思會*1, 李立*2, 劉娥2

    (1.武漢工程大學 化工與制藥學院,湖北 武漢 430205;2.荊楚理工學院 化工與藥學院,湖北 荊門 448000

     

    摘要:在鈷催化體系下,以鄰苯二甲醇和苯乙酮為起始原料,一鍋法反應得到2-(1,3-二氫異苯并呋喃)-1-苯乙酮,進而對底物進行拓展,得到標題化合物,并對反應條件進行優化。結果表明,以甲苯為溶劑、叔丁醇鉀為堿,鈷催化劑用量為10%mol,標題化合物的產率較好?;衔锝Y構經1HNMR13CNMR確證。該方法具有反應條件溫和、操作簡單、產率較高的特點。

    關鍵詞:鈷催化;鄰苯二甲醇;一鍋法;2-(1,3-二氫異苯并呋喃)-1-苯乙酮;合成

    中圖分類號O625.1      文獻標識碼:A      文章編號:0258-32832022

     

    Synthesis of 2-(1,3-Dihydroisobenzofuran)-1-acetophenone Derivatives ZHAO Mei-ling1,2, LIU Qian-qian2, ZHANG Cui-lan2, LONG Si-hui*1, LI Li*2, LIU E2 (1.Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan, 430205, China; 2. College of Chemical Engineering and Pharmacy,Jingchu University of Technology,Jingmen 448000,China), Huaxue shiji, 2022, 44(6)

    Abstract: 2-(1,3-dihydroisobenzofuran)-1-acetophenone was synthesized by one pot reaction of phthaloyl alcohol and acetophenone in cobalt catalyzed system. Then, 2-(1,3-dihydroisobenzofuran)- 1-acetophenone derivatives were obtained by expanding the substrates. The reaction conditions were optimized. The results showed that 2- (1,3-dihydroisobenzofuran) -1-acetophenone derivatives (3a3g) were obtained in good yield by using toluene as solvent, potassium tert butyl alcohol as base and 10% mol cobalt as catalyst. The structures of the compounds were confirmed by 1HNMR and 13CNMR. The method is characterized by mild reaction conditions, simple operation and high yield.

    Key words: cobalt catalysis; phthaloyl alcohol;one pot;2-(1,3-dihydroisobenzofuran)-1-acetophenone; synthesis

    引用本文趙美玲, 劉芊芊, 張翠蘭,等. 2-1,3-二氫異苯并呋喃)-1-苯乙酮類衍生物的合成[J]. 化學試劑,2022,44(6):926-930。

     

     

    吳茱萸次堿合成工藝改進

    陳仕云1,高永好4,吳宗好4,桂雙英2, 3,何勇* 4, 5

    1. 合肥學院 分析測試中心,安徽 合肥  230601;2. 藥物制劑技術與應用安徽省重點實驗室,安徽 合肥  230012;3. 安徽中醫藥大學 藥學院,安徽 合肥  230012;4. 合肥華方醫藥科技有限公司,安徽 合肥  230088;5. 合肥工業大學 化學與化工學院,安徽 合肥  230009)

     

    摘要:以靛紅、色胺為起始原料,縮合得到N-(2-氨基苯甲?;?/span>)色胺,在硫酸氫鈉存在下與原甲酸三乙酯經Pictet-Spengler反應合成了7,8,13b,14-四氫吲哚并[2',3':3,4]吡啶并[2,1-b]喹唑啉-5(7H)-酮,最后芳構化制備吳茱萸次堿,總產率55.8%。目標化合物結構經1HNMR、13CNMRESI-MS確證。該工藝反應條件溫和、操作簡單、原料易得、成本低廉、適用于工業化生產。

    關鍵詞:吳茱萸次堿;環合;Pictet-Spengler反應;合成;改進

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

     

    Improved Synthesis of Rutaecarpine CHEN Shi-yun1, GAO Yong-hao4, WU Zong-hao4, GUI Shuang-ying2,3, HE Yong*4,5 (1. Analytical & Testing Center, Hefei University, Hefei 230601, China; 2. Anhui Province Key Laboratory of Pharmaceutical Preparation Technology and Application, Hefei 230012, China; 3. Department of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012, China; 4. Hefei Huafang Pharmaceutical Technology Co., Ltd., Hefei 230088, China; 5. School of chemistry and chemical engineering, Hefei University of technology, Hefei 230009, China), Huaxue Shiji, 2022, 44(6),

    Abstract: N-(2-aminobenzoyl) tryptamine was firstly prepared using Indigo and tryptamine as the starting materials by condensation reaction. Then, 7, 8, 13b, 14-tetrahydroindolo [2',3':3,4] pyrido [2,1-b] quinazoline-5(7H)-one was synthesized using triethyl orthoformate in the presence of sodium bisulfate following the Pictet Spengler reaction. Finally, the rutaecarpine was prepared by aromatization with a total yield of 55.8%. The target compound has been confirmed by using 1HNMR、13CNMR and ESI-MS. Our improved processes have the merits of mild reaction conditions, simple operation, easy availability of raw materials, and low costs, which are suitable for industrial production.

    Key words: rutaecarpine; cyclization; pictet-spengler reaction; synthesis; improvement

    引用本文:陳仕云,高永好,吳宗好,等. 吳茱萸次堿合成工藝改進[J]. 化學試劑,2022, 44(6)931-935.

     

     

    硫酸苯肼的合成及分析方法

    祁鍇鈮1, 2,辜順林1, 2,劉建武1, 2,張 2,嚴生虎* 1, 2

    (1.常州大學 藥學院,江蘇 常州  213164;2.石油和化工行業連續流技術工程實驗室,江蘇 常州  213164)

     

    摘要:以苯胺、硫酸、亞硝酸鈉為原料,經過重氮化反應、還原反應、酸化反應合成了硫酸苯肼,探索了最佳合成工藝條件,在進行重氮化反應時,采用了連續流微通道反應器,大大縮短了時間,解決了重氮化反應過程中易飆溫失控的問題,極大的保證了人員安全,且降低能耗、節約成本,為硫酸苯肼工業化生產提供了參考。同時采用了HPLC對產品進行分析,峰形尖銳對稱,分離效果較好,為生產硫酸苯肼的純度分析提供一些參考。

    關鍵詞:硫酸苯肼;連續流;合成;高效液相色譜法;分析

    中圖分類號:TQ246.3          文獻標識碼:A          文章編號:0258-32832022

     

    Synthesis and Analysis Method of Phenylhydrazine Sulfate QI Kai-ni1,2, GU Shun-lin1,2, LIU Jian-wu1,2, ZHANG Yue 2, YAN Sheng-hu*1,2 (1. School of Pharmacy, Changzhou University, Changzhou 213164, China; 2. Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry, Changzhou 213164, China), Huaxue Shiji, 2022

    Abstract: Phenylhydrazine sulfate was synthesized through diazotization reaction, reduction reaction and acidification using aniline, sulfuric acid, and sodium nitrite as raw materials.  The optimal synthesis conditions were explored. A continuous flow microchannel reactor was introduced for the diazotization reaction, which greatly shortened the time and reduced the risk of thermal runaway caused by the strong exothermic diazotization process, therefore, it ensured the safety of personnel, reduced energy consumption, and saved cost. Our research results provide references for the industrial manufacture of phenylhydrazine sulfate. Besides, HPLC detection method was also established to analyze the product, the peak shape was sharp and symmetrical, indicating good separation effect, which provides reliable references for the purity analysis of phenylhydrazine sulfate.

    Key words: phenylhydrazine sulfate; continuous flow; synthesis; HPLC; analysis

    引用本文:祁鍇鈮,辜順林,劉建武,等. 硫酸苯肼的合成及分析方法[J]. 化學試劑,2022,446936-940.

     

    全文PDF :

    2022化學試劑第6期PDF文檔.pdf


    第200章厨房里征服美艳老师
  • <blockquote id="cw04w"><samp id="cw04w"></samp></blockquote>
  • <blockquote id="cw04w"></blockquote>