傅里叶变换红外光谱技术的应用及进展
周枫然1，韩桥1，张体强2，吴海2，曾武3，王德发*1
（1.中国计量科学研究院，北京 100029；2.国家气体产品质量监督检验中心，北京 100029；3.中计华量环境科技河北有限公司，河北 石家庄 050000）
摘要：傅里叶变换红外光谱技术（FTIR）具有扫描速度快、分辨率和灵敏度较高的优点，广泛应用于机理研究、性能表征、成分检测等研究领域。根据不同的检测需求，研究者们在使用傅里叶变换红外光谱技术时也作了相应的调整和优化。本文简单介绍了傅里叶变换红外光谱技术的原理，重点总结了近年来FTIR技术在各研究领域的应用现状。并指出与其他分析技术联用、建立数学模型以及标准化是除提升仪器自身精度外，提高FTIR测量准确度的发展趋势，这为FTIR在相关领域的研究和应用提供了参考。
关键词：FTIR；机理研究；性能表征；成分测量；联用技术；数学模型
中图分类号：O65 文献标识码：A 文章编号：0258-3283（2021）08
Application and Progress of Fourier Transform Infrared Spectroscopy Technology
ZHOU Feng-ran1,HAN Qiao1, ZHANG Ti-qiang2,WU Hai2, ZENG Wu3,WANG De-fa*1(1. NationalInstitute of Metrology, Beijing 100029, China;2.National Center for QualitySupervision and Inspection on Gas Products, Beijing 100029, China;3.Zhongjihualiang Environmental Technology Hebei Co., Ltd., Shijiazhuang 050000, China), Huaxue Shiji, 2021, 43(8),1001～1009
Abstract：Because of the advantages of high speed of scanning, high resolution and high sensitivity, Fourier transform infrared spectroscopy (FTIR) hasbeen widely used in various research fields such as mechanism research, performance characterization andcomposition measurement. According to different detection requirements, researchers have also made corresponding adjustments and optimizations when using Fourier transform infrared spectroscopy.This article briefly introduces the principle of Fourier transform infrared spectroscopy technology, focuses on the application status of FTIR technology in various research fields in recent years. It points out that, besides of optimizing the instrument system,combination with other analysis techniques, establishment of mathematical models as well as standardization are thedevelopmenttrend ofimproving the accuracy of the FTIR, which provides advance for the research and application of FTIR in related fields.
Key words：FTIR; mechanism research; performance characterization; composition measurement; technology combination; mathematical model
球磨制备C/CoPc复合材料电催化CO2还原反应
（宁波大学 材料科学与化学工程学院 化学合成与绿色应用研究所，浙江 宁波 315211）
摘要：电催化CO2还原（CO2RR）可以将大气中的CO2有效转化为CO或碳氢化合物等一系列增值化学品，可有效缓解温室效应导致的环境问题。酞菁钴（CoPc）因其优异的二氧化碳还原产物选择性，近年来被广泛应用于电催化CO2RR反应中，然而，CoPc自身的不良导电影响了其催化活性。为此，选用CoPc及简单易得的乙炔炭黑（C）通过简便球磨法制备得到乙炔炭黑包裹的CoPc催化剂（CoPc/C），将其置于DMF中进行搅拌处理来制备CoPc/Cs。在0.1 mol/L KHCO3中，CoPc/Cs表现出最好的电催化CO2还原性能，其过电位低至190 mV，在-0.6 ～ -0.9 V vs RHE的宽电势下CO的法拉第效率高于90%。该工作为简便制备高性能酞菁类催化剂提供了一种新思路。
关键词：电催化CO2还原；酞菁钴；复合材料；球磨
中图分类号：O643.3 文献标识码：A 文章编号：0258-3283（2021）--
Preparation of C/ CoPc Composites by Ball grinding for Electrocatalytic Reduction of CO2
ZHANG Li, LIU Lin-chang, ZHU Hong-lin* (Institute of Chemical Synthesis and Green Applications, College of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: Electrocatalytic reduction of CO2(CO2RR) can effectively convert atmospheric CO2 into a series of value-added chemicals such as CO or hydrocarbons, which can effectively alleviate environmental problems caused by the greenhouse effect. Cobalt phthalocyanine (CoPc) has been widely used in electrocatalytic CO2RR reaction in recent years due to its excellent selectivity of carbon dioxide reduction products. However, poor conductivity of CoPc itself affects its catalytic activity. To this end, we selected CoPc and easy to obtain acetylene carbon black (C) by simple ball milling method to prepare CoPc/C catalyst coated with acetylene carbon black (CoPc/C), and put the CoPc/C in DMF to prepare CoPc/Csby stirring treatment. In 0.1M KHCO3, CoPc/Cs showed good electrocatalytic performance of CO2 reduction, and its overpotential was as low as 190 mV, and the Faraday efficiency of CO was more than 90% at the wide potential of -0.6 ~ -0.9 V vs RHE. This work provides a new idea for the simple preparation of high performance phthalocyanine catalysts.
Keywords: electrocatalytic reduction of CO2; phthalocyanine cobalt; composite materials; ball milling
石墨毡原位生长TiN纳米棒及其作为钒电池电极的电化学性能研究
王新生*1，井明华*2，房大维2
（1. 河南省地质矿产勘查开发局第四地质矿产调查院， 河南` 郑州 450000；
2. 辽宁大学 化学院 稀散元素化学研究院，辽宁 沈阳 110036）
摘要：利用水热合成和高温退火方法，将氮化钛纳米棒原位生长在石墨毡表面，成功构建了兼具高催化活性和高导电性的碳纤维复合电极材料。用扫描电子显微镜对复合电极的表面形貌和结构进行了表征。利用接触角测试仪对电极表面的浸润性进行了考察。采用三电极体系并通过小幅电位阶跃法和循环伏安法对电极的电化学表面积和电化学性能进行了分析。最后，通过充放电测试对相应电池性能进行了考察。结果表明：以该复合材料为电极的电池在电流密度为200 mA/cm2下，能量效率达到了 80.23 %，比常规电池提升了约7.2 %，且电池表现出更优的倍率性能和能量密度。
关键词：钒电池；石墨毡；水热法；氮化钛纳米棒；复合电极材料
中图分类号：TQ 000 文献标识码：A 文章编号：0258-3283（2021）--
Construction and Electrochemical Performance of TiN/Graphite Felt Nanorods Electrode for Vanadium Redox Flow Battery
WANG Xin-sheng*1, JING Ming-hua*2, FANG Da-wei2 (1. Institute of Geological and Mineral Resources Survey of Henan, Zhengzhou 450000, China; 2. Institute of Rare and Scattered Elements, College of Chemistry, Liaoning University, Shenyang 110036, China), Huaxue Shiji, 2021, 43(8), ～
Abstract：TiN nanorods were grown in situ on the surface of graphite felt fibers by hydrothermal synthesis and high temperature annealing, and a carbon fibers composite electrode material with high catalytic activity and high electrical conductivity was successfully constructed. The surface morphology and structure of the composite electrode were characterized by scanning electron microscopy. The wettability of the electrode was investigated by contact angle test. The real electrochemical surface area and electrochemical performance of the prepared electrode were analyzed by small potential step method and cyclic voltammetry respectively in a common three-electrode system. Finally, the battery performance was investigated by charging and discharging tests. The results showed that the energy efficiency of the single cell using the composite material as electrodes reached 80.23 % at the current density of 200 mA/cm2, which was about 7.2 % higher than that of the conventional battery. Moreover, the single cell also showed better rate performance and energy density.
Key words：Vanadium battery; Graphite felt; Hydrothermal method; Titanium nitride nanorods; Composite electrode material
RhNi/Co3O4纳米材料催化氨硼烷水解产氢研究
张子豪，刘林昌，郭亚君，朱红林*
（宁波大学 材料科学与化学工程学院 化学合成与绿色应用研究所，浙江 宁波 315211）
摘要：金属氧化物被广泛应用于催化剂的载体，Co3O4作为一种金属氧化物具有弱磁性和氧化还原等特性，可被当做载体制备出高效同时高稳定性的催化剂。采用浸渍-还原法，通过改变Rh和Ni的物质的量之比制得了一系列Rh基及过渡金属Ni基负载在Co3O4载体上的催化剂，并对这些样品进行表征及氨硼烷（AB）水解产氢的测试。一系列表征结果证明RhNi合金已成功负载到Co3O4载体表面。催化剂活性测试表明，Rh1.5Ni0.5/Co3O4表现出最优异的氨硼烷水解产氢性能，转换频率（TOF）高达1178.85 min-1，相应的活化能（Ea）为66.65kJ/mol。
关键词：RhNi合金；Co3O4；纳米材料；氨硼烷（AB）；催化产氢
中图分类号：O612.8.3 文献标识码：A 文章编号：0258-3283（2021）--
Performance of RhNi/Co3O4 Nanomaterials for Hydrogen Generation from Catalytic Hydrolysis of Ammonia Borane
ZHANG Zi-hao, LIU Lin-chang, GUO Ya-jun, ZHU Hong-lin* (Institute of Chemical Synthesis and Green Applications, College of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: Metal oxides are widely used for the support of catalyst, and magnetic Co3O4 can be used as a carrier for the preparation of supported catalyst, which is highly efficient and stable. Herein, a series of the Rh-based and Ni-based supported on Co3O4 catalysts which were prepared via changing the molar ratio of Rh/Ni by the impregnation-reduction technology were characterized and tested for the hydrogen generationfrom hydrolysis of ammonia borane (AB). It was proved that RhNi alloys were supported on the surface of Co3O4carrier successfully. The activity test shows that Rh1.5Ni0.5/Co3O4exhibits extremely high catalytic activity for hydrolysis of AB with conversion frequency (TOF) as high as 1178.85min-1, and the corresponding activation energy (Ea) 66.65kJ/mol.
Keywords:RhNi alloys; Co3O4; nanomaterials; ammonia borane (AB); hydrolyticdehydrogenation
KMnO4改性汉麻废弃物对水体中Pb2+吸附工艺优化研究
张旭1,3，柏广宇2，高宝昌1，孙宇峰1，赵国栋3，田媛1，石雨1，崔宝玉1
（1. 黑龙江省科学院大庆分院，黑龙江 大庆 163000；2. 黑龙江省哈尔滨生态环境监测中心，黑龙江 哈尔滨 150050；3. 哈尔滨理工大学 材料科学与化学工程学院，黑龙江 哈尔滨 150050）
摘要：建立了汉麻废弃物KMnO4改性方法及其对水体中Pb2+吸附工艺优化方案，以汉麻废弃物为切入点，通过KMnO4预处理，制备成表面富含Mn-O基团吸附剂，达到吸附Pb2+净化水体的目的。通过单因素分析确立三因素三水平正交试验方案，确定了改性汉麻废弃物对水体中Pb2+吸附最佳工艺：溶液pH 4.5、吸附时间20 min、A/C（改性汉麻废弃物吸附剂投放量与Pb2+离子浓度比）值25条件下，改性汉麻废弃物吸附容量最大为40.25 mg/g。KMnO4改性汉麻废弃物Pb2+吸附剂具有易制备、环保、高效等优点。
关键词：KMnO4；汉麻废弃物；二价铅离子；吸附工艺优化
中图分类号：X131.2 文献标识码：A 文章编号：0258-3283(2021)--
KMnO4 Modified Hemp Waste to Pb2+ Adsorption Process Optimization In Water
ZHANG Xu1,3,BAI Guang-Yu2,GAO Bao-chang1,SUN Yu-feng1,ZHAO Guo-dong3,TIAN Yuan1,SHI Yu1,CUI Bao-yu1(1.Daqing Branch of Heilongjiang Academy of Sciences，Daqing 163000,China；2.Harbin Ecological Environment Monitoring Center of Heilongjiang Province，Harbin 150050,China；3.Harbin University of Science and Technology Materials Science and Chemical Engineering Academy，Harbin 150050,China), , Huaxue Shiji, 2021, 43(8), ～
Abstract: To establish KMnO4 modification method for hemp waste and optimize the adsorption process of Pb2+ in water, with hemp waste as the entry point, the adsorbent rich in Mn-O group on the surface was prepared by pretreatment with KMnO4 to achieve the purpose of adsorbing Pb2+ and purifying water. The best adsorption process of modified hamp waste to Pb2+ in water is established according to the analysis of the single factor and three factors and three levels orthogonal tests：Optimum adsorption process conditions are at pH4.5 solution、adsorption time 20 min and A/C（ratio of adsorbent dosage and Pb2+ concentration of modified hamp waste）value for 20 . In this way，the maximum adsorption capacity of modified hamp waste is 40.25 mg/g.KMnO4 modified hamp waste to Pb2+ adsorptiont has the advantages of easy preparation, environmental protection, high efficiency and so on.
Key words：KMnO4;hemp waste;divalent lead ions;adsorption process optimization
基于庆大霉素检测与分析应用的研究进展
刘里*，李林琴，汪帆
（曲靖师范学院 化学与环境科学学院，云南曲靖 655011）
摘要：庆大霉素是应用最广泛的氨基糖苷类抗生素之一，对人和家畜的革兰氏阴性和革兰氏阳性细菌感染均有广谱杀菌作用。动物源性食品中过多的庆大霉素会对人类健康产生不利影响，例如增加耳毒性和肾毒性的发生率。尽管存在肾毒性，氨基糖苷类抗生素庆大霉素仍被认为是一种重要的抗感染药物。庆大霉素残留的测定在很大程度上依赖于适当的分析技术。庆大霉素具有高度极性、不挥发，缺乏紫外线发色团等特性，这对药物的分析提出了很大的挑战。综述首先简要介绍了庆大霉素，然后对现有的分析技术进行了调研，阐述了不同分析方法用于检测庆大霉素所面临的挑战和机遇。综述了2000～2020年庆大霉素及其硫酸盐的测定方法及分析应用，已报道的方法分为分光光度法、荧光法、蒸发光散射法、液相色谱法、超高效液相色谱-串联质谱法、电化学法、比色法、化学发光法、微生物法、免疫层析法和表面等离子共振技术。根据应用方法和仪器对文献进行了分类，并对所有方法的分析参数制成表格，便于查阅和比较。
关键词：庆大霉素；检测；分析应用；光谱法；色谱法；
中图分类号：O657；R978.1文献标识码：A 文章编号：0258-3283(2021)--
Recent Advances on Determination Methods and Analytical Applications of Gentamicin
LIULi*，LI Lin-qin，WANG Fan(College of Chemistry and Environmental Environmental Science, Qujing Normal University，Qujing，Yunnan，655011）, Huaxue Shiji, 2021, 43(8), ～
Abstract：Gentamicin as one of the most widely used aminoglycoside antibiotics, exhibits broad-spectrum bactericidal action against both gram-negative and gram-positive bacterial infections in both humans and livestock. Excessive levels of gentamicin in food of animal origin can have adverse effects on human health such as increasing the incidences of ototoxicity and nephrotoxicity. Despite its nephrotoxic potential, the aminoglycoside antibiotic gentamicin is still considered to be an important agent against infections. However, determining gentamicin residues relies largely on adequate analytical techniques. Gentamicinis highly polar, non-volatile and lacks a UV chromophore. This poses a great challenge in the analysis of this drug. The present review begins with a brief introduction to gentamicin followed by a survey on the existing analytical techniques, and describes the challenges and opportunities faced by different analytical methods for the detection of gentamicin. This article reviews determination methods and analytical applications of gentamicin and its sulfatefrom 2000 to 2020. The reported methods are classified into seven types: spectrophotometry, spectrofluorimetry, scattering, liquidchromatography, ultra performance liquid chromatography-tandem mass spectrometry, electrochemical detection, colorimetry,chemiluminescence,microbial method,immunochromatographyand surface plasmon resonance technology. The literature is classified based on applied methodology and instrumentation, and the analytical parameters of all the reviewed methods were tabulated for easy access and comparison.
Keywords:gentamicin; determination; analytical applications; spectrophotometry; chromatography
酞菁钴（CoPc）基电极材料在电催化CO2还原反应中应用的研究进展
李忠义，马静静，郑岳青*
（宁波大学 材料科学与化学工程学院 化学合成与绿色应用研究所，浙江 宁波 315211）
摘要：温和条件下电催化还原CO2为高能量密度的碳基化学品及化学燃料实现碳中和提供了极具诱人的策略，然而阻碍其实际应用的关键仍是高性能电极材料的设计与可控构筑。目前用于电催化CO2还原反应（CO2RR）的众多电催化材料中，酞菁钴（CoPc）基催化剂因具有高CO选择性及高催化活性而备受青睐。就CoPc基电极材料在电催化CO2还原反应中应用的最新研究进展进行综述。首先重点介绍了提升负载型CoPc基催化剂电催化性能的策略，然后依次介绍了CoPc基催化剂在级联电催化CO2RR和CO2全分解中的应用、以及电催化CO2RR的反应机理，最后就该领域尚未解决的问题提出展望。
关键词：电极材料；电催化CO2还原；酞菁钴；负载型催化剂；催化机理
中图分类号：O643.36 文献标识码：A 文章编号：0258-3283（2021）--
Cobalt Phthalocyanine (CoPc) Based Electrode Materials for Electrocatalytic CO2 Reduction
LI Zhong-yi, MA Jing-jing, ZHENG Yue-qing* (Institute of Chemical Synthesis and Green Applications, College of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: Electrocatalytic reduction of CO2 to high energy carbon-based chemicals and fuels in mild conditions offers a seductive strategy for achieving carbon neutrality, but design controllable architecture of high performance electrode materials remains the key to hampering its practical applications. Among the numerous electrocatalytic materials currently used for electrocatalytic CO2 reduction reaction (CO2RR), cobalt phthalocyanine (CoPc) based catalysts are favored for their high CO selectivity and catalytic activity.This article reviews the latest research progress on the application of CoPc-based electrode materials in electrocatalytic CO2 reduction reactions. Firstly, we focus on the strategies for the performance boosting of supported CoPc-based catalysts, then the applications of CoPc-based catalysts in cascade electrocatalytic CO2RR, overall CO2splitting reaction and the reaction mechanism of electrocatalyticCO2RR are introduced, finally we present the outlook on the unresolved issues in this field.
Key words: electrode material; electrocatalytic CO2 reduction; CoPc; supported catalyst; catalytic mechanisms
姚培1，李树白1，张怿涵2，秦建国*3，张启蒙1，刘媛1，付博文1，顾子栋1，杨敏1
(1. 常州工程职业技术学院 化工与制药工程学院，江苏 常州 213164；2. 常州大学江苏省油气储运技术重点实验室，江苏 常州 213000；3. 上海沃凯生物技术有限公司，上海 201506)
摘要：离子液体（ILs）由于其独特的物理化学性质，如：对噻吩类硫化物较好的溶解性，低的蒸气压难挥发，对环境友好，不溶于燃油，可避免与油品的交叉污染，而被用于燃油的脱硫研究。离子液体由于价格高影响了离子液体的广泛应用，通过离子液体改性负载固体材料后，减少离子液体用量，促进离子液体的广泛应用。基于离子液体负载固体材料在脱硫中的应用发展，综述了离子液体负载固体材料的方法，离子液体种类，负载材料的种类以及几个方面对复合材料在燃料油脱硫的应用研究，最后对离子液体负载复合材料回收方法进行比较，并对离子液体负载材料脱硫的前景和发展进行了展望。
关键词：离子液体；脱硫；负载；复合材料；燃料油；
中图分类号：X712 文献标识码：A 文章编号：0258-3283（2021）--
The research of the deep desulfurization in fuel oil by ionic liquid load solid complex
YAO Pei1, LI Shu-bai1, ZHANG Yi-hang2, QIN Jian-guo3, ZHNG Qi-meng1, LIU Yuan1, FU Bo-wen1, GU Zi-dong1, YANG Min1 (1. College of Chemical and Pharmaceutical Engineering, Changzhou Vocational Institute of Engineering, Changzhou 213164, China; 2. School of Petroleum Engineering, Changzhou University, Changzhou 213000, China; 3. Shanghai OurChemBio-Technology Co., Ltd., Shanghai 201506, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: Due to their unique physical and chemical properties, Ionic liquids (ILs) were widely used in the fields of desulfurization in recent years. For example, high solubility to thiophene sulfides, low vapor pressure, difficult to volatilize, environment friendly, insoluble in fuel, which could avoid cross contamination with oil products.Due to the high price of ionic liquids, the wide application of ionic liquids was affected. The modification of solid materials by ionic liquids can reduce the amount of ionic liquid, which can promote the wide application of ionic liquids. Based on the application and development of solid materials supported by ionic liquids in desulfurization, the methods of supporting solid material by ionic liquids, the type of ionic liquids and the type of supporting materials for the application of composite materials in desulfurization of fuel oil were reviewed. Finally, the recovery methods of composites supported by ionic liquids were compared and the prospectsof the desulfurization for composites supported by ionic liquids were prospected.
Keywords: Ionic Liquid; desulfurization; modified;composites; fuel oil
四唑虫酰胺及其关键中间体的合成方法综述
党铭铭1，郭永艳1，田雁飞1，柳爱平2,3，刘卫东2,3，刘民华*2,3
(1. 湖南有色金属职业技术学院 资源环境系，湖南 株洲 412000；2. 湖南化工研究院有限公司 国家农药创制工程技术研究中心，湖南 长沙 410014；3. 农用化学品湖南省重点实验室，湖南 长沙 410014)
摘要：综述了由拜耳作物科学公司开发的新型双酰胺类杀虫剂四唑虫酰胺(Tetraniliprole)的合成方法，主要包括缩合法、胺解法和环化法等3种，且对这些方法所涉及的关键中间体的合成也进行了简要概述。其中，缩合法，特别是以关键中间体N,3-二甲基-2-氨基-5-氰基苯甲酰胺和1-(3-氯吡啶-2-基)-3-(5-三氟甲基-2H-四氮唑-2-亚甲基)吡唑-5-甲酸在碱和甲磺酰氯作用下直接合成四唑虫酰胺的合成路线，具有原料易得、产率高和易于操作等优点，可能是目前制备四唑虫酰胺的最佳合成工艺。
关键词：四唑虫酰胺；双酰胺类杀虫剂；鱼尼丁受体；合成方法
中图分类号：TQ450 文献标识码：A 文章编号：0258-3283（2021）--
A Review on Synthetic Methods of Tetraniliprole and Key Intermediates
DANG Ming-ming1, GUO Yong-yan1, TIAN Yan-fei1, LIU Ai-ping2,3, LIU Wei-dong2,3, LIU Min-hua*2,3 (1. Department of Resources and Environment, Hunan Nonferrous Metals Vocational and Technical College, Zhuzhou 412000, China; 2. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry Co., Ltd., Changsha 410014, China; 3. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China), Huaxue Shiji, 2021, 43(8), ～
Abstract:The synthetic methods for tetraniliprole discovered by Bayer CropScience as the novel diamide insecticide were reviewed. The syntthetic methods to tetraniliprole are divided into 3 kinds including condensation, ammonolysis and cyclization methods. The synthetic methods for all key intermediates involved in these methods were also briefly summarized. Among them, the condensation method, especially the route of the key intermediate 2-amino-5-cyano-N,3-dimethylbenzamide(2) and 1- (3-chloropyridin-2-yl) -3 - ((5-(trifluoromethyl)-2H-tetrazol-2-yl)methyl)-1H-pyrazole-5-carboxylic acid(3a) under base and methanesulfonyl chloride conditions might at present be the most efficient synthetic process due to its advantages such as starting materials easily obtained, the high yield and easy industrialization operation.
Key words: tetraniliprole; diamide insecticide; ryanodine receptor(RyR); synthetic method
超级细菌NDM-1及其检测方法的研究进展
赵雨佳1,2，廖湉毅1,3，范培蕾1，梁亮1，王晓阳1，赵海波*1
(1. 北京市计量检测科学研究院，北京 100024；2. 清华大学 药学院，北京 100084；3. 巴黎大学 科学学院，巴黎 75006)
摘要：抗生素滥用造成细菌的耐药性问题日益严重，对人类健康和卫生安全构成极大威胁。新德里金属β-内酰胺酶能水解碳青霉烯在内的绝大多数β-内酰胺类抗生素，导致产该酶的细菌仅对替加环素和多粘菌素敏感，因此也被称为超级细菌NDM-1。编码该酶的blaNDM-1基因大多定位在质粒上，能通过水平传播，加剧多重耐药菌的产生，由于缺乏特效抑制剂，导致临床抗生素的使用难度进一步增加。为满足临床实验室、应急检测和现场监测的需求，表型筛查、表型确证、快速筛查、基因确证和宏基因组测序等一系列方法被研发出来，用于监测和预防NDM-1的全球扩散。对超级细菌NDM-1的分子生物学特性、检测方法和流行情况等方面进行综述，为监测和预防NDM-1的全球大扩散提供参考。
关键词：超级细菌NDM-1；细菌耐药性；抗生素；金属β-内酰胺酶；检测方法
中图分类号：R185、Q933 文献标识码：A 文章编号： 0258-3283（2021）--
Perspectives on Superbacteria NDM-1 and Detection Methods
ZHAO Yu-jia1,2, LIAO Tian-yi1,3, FAN Pei-lei1, LIANG Liang1, WANG Xiao-yang1, ZHAO Hai-bo *1 (1. Beijing Institute of Metrology, Beijing 100024, China; 2. School of Pharmacy, Tsinghua University, Beijing 100084, China; 3. Science College，Paris University, Paris 75006, France), Huaxue Shiji, 2021, 43(8), ～
Abstract：The bacterial drug-resistance issue caused by antibiotics abuse is increasingly serious, which posed a great threat to human health and hygiene. New Delhi metal β-lactamase can hydrolyze most β-lactam antibiotics including carbapenems that makes the bacteria producing this enzyme to be only sensitive to tigecycline and polymyxin. Therefor it is also called superbacteria NDM-1. The gene coding this enzyme is mostly located on plasmids, which can aggravate the production of multi-drug resistant bacteria through horizontal spread. The lack of specific inhibitors has further increased the difficulty of using clinical antibiotics. To meet demands of clinical laboratories, emergency testing, and on-site monitoring, a series of methods including phenotypic screening, phenotypic confirmation, rapid screening, genetic confirmation and metagenomics sequencing have been developed to prevent the global spread of superbacteria NDM-1. This paper reviewed the molecular biological characteristics, detection methods and prevalence of superbacteria NDM-1, to provide references for monitoring and preventing the global spread of NDM-1.
Key words：superbacteria NDM-1; bacterial drug-resistance; antibiotic; mental β-lactamase; detection method
潜血手印检测及增强方法进展研究
任建新1，刘丛睿2，张晓梅*1
（1.中国刑事警察学院刑事科学技术学院，辽宁 沈阳 110035；
2. 中国刑事警察学院公安信息技术与情报学院，辽宁 沈阳 110035）
摘要：潜血手印是重大案件现场经常出现的一类痕迹物证，有关潜血手印的检测和增强技术一直以来都是法庭科学领域的重要研究内容。有效、合理的应用检测及增强方法对案件的侦破有着举足轻重的作用。本综述根据增强潜血手印所用原理的不同将增强方法划分为光学方法、化学方法和其他方法，并重点介绍了化学方法在潜血手印、潜血痕迹检测、增强中的应用。希望能为公安工作的实际应用以及血手印检测及增强技术的发展提供一定的参考依据。
关键词：法庭科学；潜血手印；潜血印痕；增强；进展研究
中图分类号：DF794.1 文献标识码：A 文章编号：0258-3283（2021）--
Methods for the Detection and Enhancement of Fingerprint in Blood
REN Jian-Xin1, LIU Cong-Rui2, ZHANG Xiao-Mei*1 (1. Department of Forensic Science, Criminal Investigation Police University of China, Shenyang 110035, China; 2. Department of Public Security Information Technology and Intelligence, Criminal Investigation Police University of China, Shenyang 110035, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: At serious crime scenes, bloody fingerprint is one of the most commonly encountered types of trace evidence. The detection and enhancement technology of bloody fingerprint has always been an important research content in the field of forensic science. Effective and reasonable application detection and enhancement methods play a pivotal role in the detection of criminal cases. In this review, the enhancement methods are divided into optical methods, chemical methods and other methods, and the application of chemical methods to detect and enhance bloody fingerprints is emphatically introduced. We hope to provide some references for the practical application of public security work and the development of blood fingerprints detection and enhancement technology through this review.
Key words: forensic science; bloody fingerprint; blood impression; enhancement; research progress
龙脑樟挥发油化学成分、抗烟草花叶病毒及抑菌活性研究
杨鹏飞1，卢慧1，王新峰2，陈芝飞3，席高磊3，万帅3，马飞2，王正伟*2
（1.郑州轻工业大学 食品与生物工程学院，河南 郑州 450002；2. 河南中烟工业有限责任公司许昌卷烟厂，河南 许昌 461000；3.河南中烟工业有限责任公司技术中心，河南 郑州 450000）
摘要：采用水蒸气蒸馏法从龙脑樟的叶和茎中提取挥发油，通过气相色谱-氢火焰离子化法(GC-FID)和气相色谱-质谱联用(GC-MS)技术对其化学成分进行鉴定，用归一化法测定挥发油中各组分的相对百分含量，并评价其抗烟草花叶病毒（TMV）和抗菌活性。从龙脑樟叶的挥发油中共分离鉴定了29种挥发性化合物，其中d-冰片含量最高，达到68.45%，其他主要成分为樟脑（14.22%）、异丁香烯（4.65%）和(E)-β-石竹烯（2.00%）等；茎挥发油分离鉴定了17种成分，主要成分是d-冰片（64.02%）、樟脑（17.60%）和异丁香烯（5.39%）等。龙脑樟挥发油对TMV有抑制作用，在100 μg/mL时抑制率达56.9%；对金黄色葡萄球菌、蜡状芽孢杆菌、大肠杆菌、烟曲霉和白色念珠菌均有较强的抑制作用，对烟曲霉的抑制能力最强，MIC值为31.3 μg/mL。
关键词：龙脑樟；挥发油；单萜；抗烟草花叶病毒；抗菌
中图分类号：R284.1 文献标识码：A 文章编号：0258-3283（2021）--
Chemical Composition, Anti-tobacco Mosaicvirus and Antimicrobial Activities of the Essentialoil ofCinnamomumCamphoraChvar. Borneol
YANG Peng-fei1, LU Hui1, WANG Xin-feng2,CHENZhi-fei3, XIGao-lei3, WAN Shuai3, MA Fei2, WANG Zheng-wei*2(1. College of Food and Biological Engineering, Zhengzhou University ofLight Industry, Zhengzhou450002, China; 2. Xuchang Cigarette Factory,China Tobacco Henan Industrial Co.,Ltd.,Xuchang461000,China; 3. Technology Centre, China Tobacco Henan Industrial Co., Ltd.,Zhengzhou450000, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: The essential oil was extracted from Cinnamomum camphor by steam distillation, and its chemical composition was identified byGC-FIDandGC-MS,the normalization method was used to determine the relative percentage of each component in the essential oil,and evaluated its anti-TMV and antibacterial activity.A total of 29 volatile compounds were isolated and identified from the essential oil of Cinnamomumcamphora leaves. Among them, the content of d-borneol was the highest, reaching 68.45%. The other main components were camphor (14.22%), isobutene (4.65%) and (E)-β-Caryophyllene (2.00%). The essential oil from the stems was separated and identified 17 components, the main components were d-borneol (64.02%), camphor (17.60%) and isobutene (5.39%).The essential oil ofCinnamomum camphor has an inhibitory effect on TMV, and the inhibition rate is 56.9%;It also has the inhibition effects on Staphylococcus aureus, Bacillus cereus, Escherichia coli, Aspergillusfumigatus and Candida albicans,which has thebestbacteriostaticeffectonAspergillusfumigatus,with MIC of 31.3μg/mL.
Keywords: Cinnamomumcamphora; essential oil; monoterpene; anti-TMV; antimicrobial
韩月颖1，张喜庆1，王琦2，魏菁3，刘继军4，高云航*1
（1. 吉林农业大学 动物科学技术学院，吉林长春 130118；2. 金普海关，辽宁大连 116600；3. 哈尔滨海关技术中心，黑龙江哈尔滨 150028；4. 中国农业大学 动物科学技术学院，北京 100083）
摘要：为探索一种最佳的漆酶酶活力测定反应体系条件，从而确定更为准确的酶活力测定方法，该研究以漆酶标品为研究对象，以2,2-联氮-二(3-乙基-苯并噻唑-6-磺酸)二铵盐(ABTS)为底物，采用分光光度法确定漆酶标品稀释倍数与ΔOD值之间的线性关系以及最佳酶促反应时间，选取酶活力测定反应体系中的缓冲液浓度、pH值以及ABTS浓度作为影响因素进行单因素优化，以所测定漆酶酶活力为响应值进行响应面优化与评估。结果表明，漆酶标品稀释倍数在30～80之间与吸光度变化值线性关系良好，酶促反应中最佳酶活力测定时间为起始3min。反应体系中当醋酸-醋酸钠缓冲液浓度为50 mmol/L、pH4.0、底物ABTS浓度为1 mmol/L时，所测得漆酶标品酶活力最为接近真实值，为1040.49 U/g。将优化好的反应条件应用于生产漆酶微生物的酶活力检测中，从而确定菌株的产酶性能，结果表明，所优化的方法在测定微生物产酶活性方面十分稳定，具有可行性。
关键词：漆酶；ABTS；反应条件；响应面优化；微生物应用
中国分类号：Q814.9 文献标识码：A 文章编号：0258-3283（2021）--
Optimize the Determination Method of Laccase with ABTS as Substrate and Its Application Based on Response Surface Method
HAN Yue-ying1, ZHANG Xi-qing1, WANG Qi2, WEI Jing3, LIU Ji-jun4, GAO Yun-hang*1(1.College of Animal Science and Technology, Jilin Agricultural University, Changchun130118, China; 2.JinpuCustoms, Dalian 116600, China; 3. Harbin Customs Technical Center, Harbin150028, China; 4.College of Animal Science and Technology, China Agricultural University, Beijing 100083, China), Huaxue Shiji, 2021, 43(8), ～
Abstract:In order to explore an optimal reaction system condition for the determination of laccase enzyme activity, and to determine a more accurate method for determination of enzyme activity, this study took the laccase standard product as the research object and used 2,2-diazepine-bis(3-Ethyl-benzothiazole-6-sulfonicacid) diammoniumsalt(ABTS) was used as the substrate. Spectrophotometric method was used to determine the linear relationship between the laccase standard dilution multiple and the ΔOD value and the optimal enzymatic reaction time. On the basis of single-factor pre-test, three variables, acetate-sodium acetate buffer concentration, pH value and ABTS concentration, were selected to carry out three-factor and three-level Box-Behnken design, and further optimization was made in response to the reaction conditions. The results showed that the dilution ratio of the laccase standard product was between 30 and 80 and the absorbance change value had a good linear relationship. The best enzyme activity determination time in the enzymatic reaction was the first 3 minutes. In the reaction system, when the concentration of ace-sodium acetate buffer was 50 mmol/L, pH 4.0, and the substrate ABTS concentration was 1 mmol/L, the enzyme activity of laccase marker was the closest to the real value, and the optimized reaction conditions were feasible.The optimized reaction conditions were applied to the enzyme activity detection of laccase-producing microorganisms to determine the enzyme-producing performance of the strain. The results showed that the optimized method was very stable and feasible in determining the enzyme-producing activity of microorganisms.
Keyword: laccase; ABTS; reaction conditions; response surface optimization; microbial application
高效液相色谱法准确定量微量植物体中的重要植物色素
陈燕秋，喻静兰，侯捷，高慧敏，李良君，徐仲杰，雷雯*
（上海化工研究院有限公司 国家同位素工程技术研究中心上海分中心
上海稳定性同位素工程技术研究中心，上海 200062）
摘要：建立了高效液相色谱法快速准确定量微量植物体中重要植物色素（叶绿素a、叶绿素b和叶黄素）的分析方法。微量植物叶片以95%乙醇匀浆超声提取色素4 h，过滤膜后直接分析。色谱分离选用COSMOSIL氰基柱（4.6 mm × 250 mm，5 μm），以甲醇-水洗脱进行洗脱，流速为1.0 mL/min，用二极管阵列检测器检测，可在15 min内完全植物中三种重要色素的快速分离分析。结果表明，三种色素在0.05～50 mg/L范围内线性关系良好（相关系数均为0.9999）；平均加标回收率为90%～110%；相对标准偏差（RSD）＜5%；日内及日间精密度均＜5%，满足定量要求。与目前检测植物色素的方法相比，该方法前处理简单快速，且采用简单的甲醇-水体系快速分离植物色素，结果可靠，重现性好，可为植物体的生理研究提供基础。
关键词：高效液相色谱；准确定量；叶绿素-a；叶绿素-b；叶黄素
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283(2021)—
Determination of important plant pigments in trace plants by High performance liquid chromatography
CHEN Yan-qiu, YU Jing-lan, HOU Jie, GAO Hui-min, LI Liang-jun, XU Zhong-jie, LEI Wen* (Shanghai Research Institute of Chemical Industry Co,Ltd, National Isotope Engineering Technology Research Center, Shanghai Engineering Research Center of Stable Isotope, Shanghai 200062, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: A high performance liquid chromatography (HPLC) method was established to determine the important plant pigments (chlorophyll-a, chlorophyll-b and lutein) in trace plant. The trace plants after extracted by 95% ethanol, and the sample was filtered for HPLC analysis. The separation was performed on an COSMOSIL Cyano column (4.6 mm × 250 mm, 5 μm) by elution with water and methanol as the mobile phases. Rapid separation was achieved within 15 min at a flow rate of 1.0 ml/min with detection by diode array detector. Under the optimized conditions, good linearity was obtained in the range of 0.05-50 mg/L with the correlation coefficient (R2) of about 0.9999. The average recovery was between 90% to 110% with the relative standard deviation (RSD) less than 5%. The intra-day and inter-day precisions were all below 5%. Compared with the current methods for detecting plant pigments, the method is simple and fast in pretreatment, and uses a simple methanol-water system to quickly separate plant pigments, with reliable results and good reproducibility, which can provide a basis for physiological studies of plants.
Key words:High performance liquid chromatography; accurate quantification; chlorophyll-a; chlorophyll-b; lutein
A2/O-MBR组合工艺去除有机氯农药残留的特性研究
吴春英*，白鹭，谷风，陆文龙，葛及
（吉林化工学院 资源与环境工程学院，吉林 吉林 132022）
摘要：以污水中16种有机氯农药（OCPs）残留为目标物，阐明其在厌氧/缺氧/好氧与MBR的组合工艺（A2/O-MBR）中的去除特性。结果表明，16种OCPs在该工艺中的进水浓度范围从50.5 ng/L（艾氏剂）到169.2 ng/L（六氯苯），出水中浓度范围从1.02 ng/L（杀螨酯）到80.1 ng/L（百菌清）。该工艺对大多数有机氯农药残留具有很强的去除能力，且去除率均在92%以上。去除途径主要分3种，以生物降解为主要去除途径、以生物降解和污泥吸附共同作用为去除途径、以污泥吸附为主要去除途径，同时还有少部分OCPs得不到有效去除。
关键词：有机氯农药；A2/O-MBR；去除率；污泥吸附；生物降解
中图分类号：X703 文献标识码：A 文章编号：0258-3283(2021)--
Removal characteristics of Organochlorine Pesticides Residues in Membrane Bioreactor Combined with Anaerobic-Anoxic-Aerobic Proces
WU Chun-ying，BAI Lu，GU Feng，LU Wen-long，GE Ji (School of resources and Environmental Engineering, Jilin Institute of Chemical Technology, Jilin City 132022), Huaxue Shiji, 2021, 43(8), ～
Abstract: The removal characteristics of 16 organochlorine pesticides (OCPs) in membrane bioreactor (MBR) combined with ana erobic-anoxic-aerobic (A2/O-MBR) process were investigated in a municipal treatment plant. The results showed that the influent concentration of 16 OCPs in this process ranged from 50.5 ng/L of aldrin to 169.2 of HCB ng/L, the effluent concentration range from 1.02 ng/L of acaractone to 80.1 ng/L. This process has a strong removal capacity for most organochlorine pesticide residues, and the removal rate is above 92%. There are three main ways to remove organochlorine pesticide residues in the process: biodegradation as the main removal route, biodegradation and sludge adsorption as the removal route, and sludge adsorption as the main removal route. And a few OCPs can not be effectively removed.
Key words: Organochlorine pesticide (OCPs); A2/O-MBR; Removal efficiency; Sludge adsorption; Biodegradation
超高效液相色谱-串联质谱法测定毛发中4种苯丙胺类兴奋剂含量的不确定度评估
胡骏杰*1,2，马文俊2，刘飞3，朱军1,2，张润生4
（1. 济宁医学院 司法鉴定中心，山东 济宁 272067；2. 济宁医学院 法医学与医学检验学院，山东 济宁 272067；3. 南京大学 化学化工学院，生命分析化学国家重点实验室，江苏 南京 210023；4. 上海市公安局 物证鉴定中心，上海 200083）
摘要：建立了毛发中4种苯丙胺类兴奋剂的超高效液相色谱-串联质谱外标定量检测方法，并对该方法进行了不确定度评估。通过分析整个实验过程，从标准溶液配制、样品配制、线性拟合、样品处理过程、基质效应等方面确定不确定度来源，量化各不确定度分量，并进行合成与扩展。结果表明，毛发中苯丙胺类兴奋剂测定结果不确定度最主要的来源为标准曲线拟合。基于司法鉴定工作需要，本文特别给出了毛发中4种苯丙胺类兴奋剂在成瘾认定含量阈值（0.2 ng/mg）处完整的不确定度报告，各物质扩展不确定度为0.0240～0.0356 ng/mg。该评估结果可为吸毒成瘾认定案件的法医鉴定工作提供有效参考信息。
关键词：超高效液相色谱-串联质谱；毛发；苯丙胺类兴奋剂；外标定量；不确定度；吸毒成瘾认定
中图分类号：O657.63 文献标识码：A 文章编号：0258-3283（2021）--
Uncertainty Evaluation for the Determination of Four Amphetamine-Type Stimulants in Hair by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
HU Jun-Jie*1,2, MA Wen-Jun2, LIU Fei3, ZHU Jun1,2, ZHANG Run-Sheng4 (1. Judicial Expertise Center, Jining Medical University, Jining 272067, China; 2. College of Forensic Medicine and Laboratory Medicine, Jining Medical University, Jining 272067, China; 3. State Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China; 4. Center for Evidence Authentication, Shanghai Municipal Public Security Bureau, Shanghai 200083, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: A method was developed for quantitative detection of four amphetamine-type stimulants (ATSs) in hair by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with the external standard, and the uncertainty of the method was evaluated. After comprehensively analyzing the entire experiment, uncertainty sources were confirmed from the processes of standard solution preparation, sample preparation, linear fitting, sample processing, matrix effect, etc. Each uncertainty component was quantified, and then the combined standard uncertainty and expanded uncertainty were respectively calculated. The results showed that the main source of uncertainty in the determination of ATSs in hair arose from the calibration curves. Based on practical needs of judicial expertise, this article specifically gave the complete uncertainty report of four ATSs in hair at the addiction threshold concentration of 0.2 ng/mg, and the expanded uncertainty of each compound was obtained to be 0.0240-0.0356 ng/mg. The evaluation results could provide effective reference information for forensic identification of drug addiction cases.
Key Words: ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); hair; amphetamine-type stimulants (ATSs); quantitative detection with the external standard; uncertainty; identification of drug addiction
陈晓梅，王丽英*，孙俊民，张永锋
（内蒙古工业大学化工学院呼和浩特煤炭转化与循环经济研究所，内蒙古呼和浩特市010051）
摘要：采用低成本、高活性胺基-双酚钴配合物调控的自由基聚合（CMRP）和催化链转移反应（CCT）对乙酸乙烯酯或丙烯酸叔丁酯与苯乙烯单体进行了共聚反应。以钴配合物为催化剂、偶氮二异丁腈（AIBN）为引发剂、聚乙烯吡咯烷酮（PVP）为分散剂，通过溶液聚合方法得到的聚乙酸乙烯酯和聚丙烯酸叔丁酯作为大分子引发剂，引发苯乙烯的分散聚合，从而获得具有较低分子量分布（～1.8）的丙烯酸叔丁酯和苯乙烯的共聚物及乙酸乙烯酯和苯乙烯的共聚物（PVAc-b-PS和PtBA-b-PS），数均分子量随单体转化率线性增加。运用凝胶渗透色谱、核磁共振波谱、扫描电子显微镜等测试手段对合成的嵌段共聚物进行了表征。
关键词：共聚；聚苯乙烯；乙酸乙烯酯；自由基聚合
中图分类号：TQ326.9文献标识码：A 文章编号：0258-3283(2021)--
Sequential Synthesis of Well-defined Poly(vinylacetate)-block-polystyrene Using Cobalt Complexes by Dispersion Polymerization
CHENXiao-mei, WANGLi ying*, SUNJun-min, ZHANG Yong-feng（School of Chemical Engineering, Inner Mongolia University of Technology; Institute of Coal Conversion and Cyclic Economy, Huhhot, 010051, China）, Huaxue Shiji, 2021, 43(8), ～
Abstract:The sequential syntheses of well-defined poly(vinyl acetate)-block-polystyrene copolymer (PVAc-b-PS) and poly(tert-Butyl acrylate)-block-polystyrene copolymer (PtBA-b-PS) were challenging due to inactive vinyl acetate (VAc) monomer and active styrene (St) monomer. In this paper, sequential syntheses of VAc and St monomer were carried out by organometallic mediated radical polymerization (OMRP) and catalytic chain transfer (CCT) by using low-cost, highly active and versatile amino-bis(phenolate) cobalt complex. PVAc and PtBA obtained via solution polymerization mediated by cobalt complex and initiated by azobisisobutyronitrile (AIBN), as macro-initiators, initiated dispersion polymerization of styrene to achieve PVAc-b-PS and PtBA-b-PS with lower polydispersity(~1.8) for the first time. Linear first-order kinetics with different feeding ratios of St and macro-initiator were obtained and the number-average molecular weight (Mn) increased linearly with monomer conversion. Synthesized block copolymers were characterized by Gel Permeation Chromatography, nuclear magnetic resonance spectroscopy, scanning electron microscopy, and Matrix-Assisted Laser Desorption/ Ionization Time of Flight Mass Spectrometry.
Key words:copolymerization; polystyrene; vinyl acetate; radical polymerization
苯并[d]咪唑基Zn(Ⅱ)配合物的晶体结构和热稳定性
赵明霞1，熊丽琴2，常进3，赵治巨4，齐传民*5
(1. 山西工程技术学院 矿业工程系，山西 阳泉 045000；2. 上海交通大学 生物医学工程学院，上海 200025；3.太原理工大学 生物医学工程学院，山西 太原，030000；4. 邢台学院 化学与化工学院，河北 邢台，054001；5. 北京师范大学 化学学院，北京 100875）
摘要：以3-（2-羧苯基）-7-甲基-2-丙基-3H-苯并[d]咪唑-5-羧酸（MZ）为配体，与六水合硫酸锌通过溶剂加热回流后常温静置挥发制备了化合物1（MZ?1.5H2O）和配合物2（{[Zn(MZ)2]?H2O}n），并利用元素分析、红外光谱和X-射线单晶衍射技术手段对其结构进行表征。X-射线单晶衍射结果表明，化合物1由一个MZ配体和1.5个水分子组成，通过氢键连接R33(10)单元（水分子与羰基间）形成一维锯齿链，进一步通过氢键连接C22(4)单元（水分子与咪唑环氮上氢原子间）形成二维结构，之后通过p-p堆积作用有序堆积形成三维网络结构；配合物2由两个独立的分子Zn1和Zn2组成，Zn1和Zn2均由一个Zn(II)原子，两个MZ配体分子和一个配位水分子组成，通过MZ配体连接中心Zn(II)原子形成了独特的二维结构，进一步通过氢键作用形成三维网络结构。此外，研究了化合物1和2的热稳定性。
关键词：苯并[d]咪唑；锌(Ⅱ)配合物；晶体结构；3D网络结构；热稳定性
中图分类号：O627 文献标识码：A 文章编号：0258-3283（2021）--
Crystal Structure and Thermal Stability of Zn(Ⅱ) Complex with Benzo[d]imidazole Ligand
ZHAO Ming-xia1, XIONG Li-qin2, CHANG Jin3, ZHAO Zhi-ju4, QI Chuan-min*5 (1. Department of mining engineering, Shanxi Institute of Technology, Yangquan 045000, China; 2. School of Biomedical Engineering, Shanghai Jiao Tong University, Shanghai 200025, China; 3. College of Biomedical Engineering, Taiyuan University of Technology, Taiyuan 030000, China; 4. College of Chemical Engineering and Biotechnology, Xingtai University, Xingtai 054001, China; 5. College of Chemistry, Beijing Normal University, Beijing 100875, China), Huaxue Shiji, 2021, 43(8), ～
Abstract：Compound 1 (MZ·1.5H2O) [MZ = 3-(2-carboxyphenyl)-7-methyl-2-propyl-3h-benzo[d]imidazole-5- carboxylic acid] and its coordination polymer 2 ({[Zn(MZ)2]·H2O}n were successfully prepared by solvent refluxing reaction and then volatilization at room temperature with the MZ ligand and zinc sulfate hexahydrate. The complexes were confirmed by elemental analysis, IR and X-ray single crystal diffraction. The x-ray single crystal diffraction results showed that compound 1 is composed of a MZ ligand and 1.5 water molecules. The R33(10) units (formed by hydrogen bond between water molecule and carbonyl oxygen atom) and water molecules though hydrogen bond connect 1 into a one-dimensional (1D) zigzag chain. Then a two-dimensional (2D) structure is formed though hydrogen bond between 1D zigzag chain and C22(4) units (formed by hydrogen bond between water molecule and NH of imidazole ring), and through π-π stacking, further form a three-dimensional (3D) network structure. Complex 2 is composed of two independent molecules Zn1 and Zn2, both of which are composed of one Zn(II) atom, two MZ ligand molecules and one coordination water molecule. A unique 2D structure is formed by connecting the central ZnII atoms with MZ ligands, and then formed a 3D network structure by hydrogen bonding interaction. In addition, the thermal stability of complexes 1 and 2 were studied in this paper.
Key words：benzo[d]imidazole; zinc (Ⅱ) complex; crystal structure; 3D network structure; thermal stability
用于溶酶体定位的比率型次氯酸根探针的构建及应用研究
马志伟*1，周诗瑾2，王川川1，陈晓培1，王建玲1，李爱勤1
（1. 河南牧业经济学院 理学部，河南 郑州 450046；2. 河南省实验中学，河南 郑州 450002）
摘要：以常见荧光团罗丹明和萘酰亚胺设计并合成了一例用于比率型识别次氯酸根的荧光探针。通过紫外吸收光谱和荧光光谱研究发现，探针能够对次氯酸根实现高效专一的比率型选择，能够克服其他分析物的干扰。溶液体系荧光发射强度比率值（F590 nm/F542 nm）在次氯酸钠浓度为0～1 μmol/L范围内呈现良好的线性，其对次氯酸根的最低检出限为1.3×10-8 mol/L。应用实验结果表明，探针可以定位于亚细胞器溶酶体中识别次氯酸根，并且能够应用于自来水等实际样品中检测次氯酸根。
关键词：荧光；探针；比率型；次氯酸根；溶酶体；定位
中图分类号：O625 文献标识码：A 文章编号：0258-3283（2021）--
Construction and application of ratio hypochlorite probe for lysosome localization
MA Zhi-wei*,1, ZHOU Shi-jin2, WANG Chuan-chuan1, CHEN Xiao-pei1, WANG Jian-ling1, LI Ai-qin1 (1. Faculty of Science, Henan University of Animal Husbandry and Economy, Zhengzhou, 450046, China; 2. Henan Experimental High School, Zhengzhou, 450002), Huaxue Shiji, 2021, 43(8), ～
Abstract：A fluorescent probe 1 for the ratiometric recognition of hypochlorite was designed and synthesized from rhodamine and naphthalimide. The results of UV absorption and fluorescence spectra showed that probe 1 could achieve high-efficiency and specific ratiometric selection for hypochlorite, and could overcome the interference of other analytes. The fluorescence emission intensity ratio (F590 nm/F542 nm) showed good linearity with the concentration of NaOCl in the range of 0～1 μmol/L. The detection limit of hypochlorite was 1.3×10-8 mol/L. The application results showed that probe 1 can be located in the lysosomes to recognize hypochlorite, and can also be used to detect hypochlorite in real water samples.
Key words：fluorescence; probe; ratiometric; OCl-; lysosome; location
响应面优化微波辅助提取花椒叶山椒素及其生物活性研究
苟鼎*，张腊梅，黄红琴，李敏
（达州中医药职业学院，四川达州，635000）
摘要：以花椒叶为原料，乙醇作为溶媒，研究花椒叶山椒素微波辅助提取工艺条件，采用响应面法对工艺进行优化。以清除铁还原力、羟基自由基(?OH)能力及2,2’-联氨-双-（3-乙基苯并噻唑啉-6-磺酸）二胺盐（ABTS）能力来评价体外抗氧化能力和α-淀粉酶活抑制率来评价其降血糖能力。结果表明，花椒叶山椒素最佳提取工艺条件为微波温度25℃、微波时间10 min、微波功率400W、料液比1：30（g/mL）、乙醇浓度58%、在此条件下花椒叶山椒素最高提取率为5.98 mg/g。花椒叶山椒素具有较强的抗氧化活性和降血糖能力，铁还原力、清除?OH自由基能力、清除ABTS自由基能力和α-淀粉酶抑制率均表现出一定的质量浓度依赖性；花椒叶山椒素铁还原力、清除清除?OH、清除ABTS自由基能力和α-淀粉酶抑制率半数有效质量浓度(IC50)分别为37.67、56.09、34.49和4.96μg/mL。花椒叶山椒素可以作为一种天然食源性抗氧化和降血糖剂。
关键词：花椒叶；山椒素；微波辅助提取；抗氧化；降血糖
中图分类号：R284 文献标识码: A 文章编号：0258-3283(2021)--
Response Surface Methodology for Optimization of Microwave Extraction of Sanshool from Zanthoxylum bungeanum Leaves and Its Bioactivity
GOU Ding*,ZHANG La-mei, HUANG Hong-qin, LI Min(Dazhou vocational college of chinese medcine, Dazhou635000, China) , Huaxue Shiji, 2021, 43(8), ～
Abstract：Taking Zanthoxylum bungeanum leaves as raw material and ethanol as solvent, the microwave-assisted extraction conditions of sanshool were studied. The process was optimized by response surface methodology.The antioxidant activity was evaluated by the ability to hydroxyl radical, 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) radical and 2,2'-Hydrazinebis-(3-ethylbenzothiazoline-6-sulfonic acid) diamine salt (ABTS) andantihyperglycemic activity was evaluated by the inhibition rate ofα-amylase.The results showed that the optimum extraction conditions of sanshool from Zanthoxylum bungeanumleaves were microwave temperature of 25 ℃, microwave treatment of 10 min, microwave power of 400W, solid-liquid ratio of 1:30 (g: mL),ethanol concentration of 58%, under these conditions, the yield of sanshool was 5.98mg/g. The sanshool from Zanthoxylum bungeanum leaves had strong antioxidant and antihyperglycemic activity. The iron reduction ability, ?OH radical scavenging ability, ABTS free radical scavenging ability and inhibition rate ofα-amylase showed the certain mass concentration dependence;The IC50 of iron reducing power,?OH radical scavenging ability, ABTS free radical scavenging ability and inhibition rate ofα-amylase were 37.67μg/mL、56.09μg/mL、34.49μg/mL和4.96μg/mL, respectively.Sanshool from Zanthoxylum bungeanum leaves could be used as a natural antioxidant and hypoglycemic agent.
Key words:Zanthoxylum bungeanum leaves; sanshool; microwave-assisted extraction ; antiglycation; hypoglycemic activity
内生菌Aspergillus terreus PC-038次生代谢产物中
抗菌化学成分研究
雷丹丹1,2，刘俊1,3，龙星美1，陈广桂1，廖尚高1,2，徐国波*1,2
（1. 贵州医科大学 药学院，贵州 贵安 550025；2. 国家苗药工程技术中心及民族药与中药开发应用教育部工程研究中心，贵州 贵阳 550004；3. 湖南省华容县人民医院，湖南 华容 414200）
摘要：研究内生菌Aspergillus terreus PC-038次生代谢物中抗菌活性成分。采用现代分离技术对A. terreus次生代谢物中活性组分进行分离纯化，利用现代质谱和核磁等波谱技术鉴定其结构，采用96孔板二倍稀释法测试单体化合物的抗菌作用。从A. terreus代谢物的活性组分中分离得到17个化合物。化合物3～7和10～14均为从内生菌A. terreus代谢物中首次分离，其中烟曲霉酸为主要成分。抗菌结果显示化合物8和烟曲霉酸对Staphylococcus aureus ATCC25923有显著的抑制作用，MIC分别为8 μg/mL和4 μg/mL。本研究丰富了A. terreus次生代谢物的化合物库，明确了化合物8和烟曲霉酸为A. terreus PC-038的抗菌主要活性成分，为新型抗生素的研发奠定了基础。
关键词：Aspergillus terreus；次生代谢产物；分离纯化；结构鉴定；抗菌
中图分类号：O629.9 文献标识码：A 文章编号：0258-3283（2021）
Study on Antibacterial Chemical Components of Secondary Metabolites from Endophytic Fungus Aspergillus terreus PC-038
LEI Dan-dan1,2, LIU Jun1,3, LONG Xing-mei1, CHEN Guang-gui1, LIAO Shang-gao1,2, XU Guo-bo*1,2 (1. School of Pharmacy, Guizhou Medical University, Guian 550025, China; 2. National Engineering Research Center of Miao‘s Medicines & Engineering Research Center for the Development and Application of Ethnic Medicine and TCM, Ministry of Education,, Guiyang 550004, China; 3. The People’s Hospital of Huarong County, Huarong 414200, China), Huaxue Shiji, 2021, 43(8)
Abstract: To investigate the antimicrobial constituents ofAspergillusterreusPC-038.The active components of A.terreus were isolated and purified by modern separation techniques on the basis of bioassay-guided method. Their structures were identified by spectroscopic methods including MS and NMR analysis. The antibacterial activity was tested on a 96-well plate with double dilution method. Seventeen compounds were isolated from the extracted metabolites of A.terreus. Compounds 3-7 and 10-14 were isolated from metabolites of A.terreusfor the first time, and compound 9 was the main component. The MICs of 1,2-Dihydrohelvolic acid (8) andHelvolic acid(9) against Staphylococcus aureus ATCC25923were 8μg/mL and 4 μg/mL, respectively. They are the main active ingredient of A.terreusPC-038. This study enriched the chemical constitutes data of A.terreus and laid the foundation for the discovery of new antibiotics.
Key words: Aspergillus terreus; secondary metabolites; isolation and purification; structure identification; antibacterial
石墨烯改性的涂料用水性聚氨酯乳液的制备和表征
郑舒文1，杨长龙1，许超1，马元生1，王大众1，多俊龙1，徐立功*2
（1. 国网辽宁省电力有限公司沈阳供电公司 辽宁 沈阳110811；2. 华东理工大学 体育科学与工程学院 上海 200237）
摘要：利用石墨烯掺杂改性提高水性聚氨酯乳液成膜性能；将经氮丙啶基团功能化的氧化石墨烯均匀分散在多官能氮丙啶齐聚物中，配制成石墨烯重量份为10%的氮丙啶交联剂，按照不同比例将其添加在自制的羧酸基阴离子型水性聚氨酯乳液中，利用羧基同氮丙啶基团的开环交联反应制备一系列水性聚氨酯膜。并采用傅里叶红外光谱（FTIR）、原子力显微镜（AFM）、热失重分析（TGA）、水接触角测试仪及万能试验机对样品进行了表征和测试；随石墨烯含量的增加，涂膜的耐热性、疏水性、拉伸强度和表面硬度均有明显提高，而微观相分离程度和断裂伸长率则呈下降趋势。较未改性乳液，经石墨烯掺杂的水性聚氨酯更适用于输电杆塔防腐。
关键词：氮丙啶；氧化石墨烯；水接触角；开环反应；水性聚氨酯
中图分类号：TQ317.4文献标识码：A 文章编号：0258-3283（2021）--
Preparation and characterization of graphene-modified waterborne polyurethane emulsions for coatings
ZHENG Shu-Wen1, YANG Chang-Long1, XU Chao1, MA Yuan-Sheng1, WANG Da-Zhong1, DUO Jun-Long1, XU Li-Gong*2 (1. Shenyang Power Supply Company of State Grid Liaoning Electric Power Co. LTD Shenyang 110811, China; 2. School of Sports Science and Engineering, East China University of Science and Technology, Shanghai 200237, China), Huaxue Shiji, 2021, 43(8), ～
Abstract:Improve the waterborne polyurethane membrane properties by graphene doping modification. Aziridine-modified oxidized graphene was evenly dispersed in polyfunctional aziridine oligomers to prepare aziridine crosslinker with certain concentration. Depending on the ring-opening crosslinking reaction of carboxyl groups with azalidine groups, a series of different graphene content waterborne PU membranes were prepared by adding the above, different proportions aziridine crosslinker containing graphene to the homemade carboxyl anionic waterborne PU emulsions. FTIR, AFM, TGA, water contact angel tester and universal tester were used to characterize and test PU samples. With the increasing of graphene, the heat-resistance, surface water resistance, mechanical properties and hardness had a significant improvement. And at the same time, the microphase separation degree and elongation at break showed a decreasing trend. Compared with unmodified emulsion, graphene-doped waterborne polyurethane is more suitable for transmission tower anticorrosion.
Key words: aziridine, oxidized graphene, water contact angel, ring opening react,waterborne polyurethane
2-溴-1,4,5-三甲氧基萘的简便合成
李成林，洪伟*
（北方民族大学 化学与化学工程学院，宁夏银川 750021）
摘要：目标化合物是合成具有抗癌、抗菌作用化合物的中间体，将通过简单易行的方法合成。以1,5-二羟基萘为起始原料，通过与乙酸酐进行酰化反应，得到1,5-二乙酰氧基萘，再与N-溴代丁二酰亚胺、乙酸进行溴代、氧化反应得到2-溴5-乙酰氧基-1,4-萘醌，最后与连二硫酸钠、氢氧化钾和硫酸二甲酯进行还原、水解和甲基化的“一步法”反应得到目标化合物，3步反应总产率为62%，中间体及目标化合物的结构均经IR、1HNMR、13CNMR和HRMS表征。
关键词：2-溴-1,4,5-三甲氧基萘；乙酰化；溴化；还原；有机合成
中图分类号：O629 文献标识码：A 文章编号：0258-3283（2021）--
Facile Synthesis of 2-Bromo-1,4,5-trimethoxynaphthalene
LI Cheng-lin, HONG Wei*(School of Chemistry and Chemical Engineering, North Minzu University, Yinchuan 750021, China), Huaxue Shiji, 2021, 43(8), ～
Abstract: The target compound is an key intermediate in the synthesis of compounds with anti-cancer and anti-bacterial effects, which was synthesized successfully useing a simple and easy method. 1,5-Diacetoxynaphthalene was produced by acetylation reaction of 1,5-dihydroxynaphthalene with acetic anhydride. Subsequently, bromination and oxidation reaction of 1,5-diacetoxynaphthalene,N-bromosuccinimide amine and acetic acid led to intermediate 5-acetoxy-2-bromo-1,4-naphthoquinone. Finally, the target compound was obtained via reduction hydrolysis and methylation reaction of sodium dithionate, potassium hydroxide and dimethyl sulfate with 5-acetoxy-2-bromo-1,4-naphthoquinone. The total yield of this synthetic route was 62%. The structures of intermediates and target compound were characterized by IR, 1HNMR, 13CNMR and HRMS.
Key words:2-bromo-1,4,5-trimethoxynaphthalene;acetylation;bromination; reduction; organic synthesis
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