挥发性有机物催化氧化技术及催化剂研究进展
黄青斌
(中国人民解放军92196部队，山东 青岛 266011)
摘要：近年来，随着生态环境的逐渐恶化，挥发性有机物的污染治理越来越受到社会各界专家和学者的广泛重视。挥发性有机物的治理技术主要包括吸附技术等回收技术和催化氧化技术等破坏技术，催化氧化是处理挥发性有机物一种较为彻底的技术，有着能耗低、无二次污染、安全性好和适用范围广等优点。通过对挥发性有机物处理技术，催化氧化机理和挥发性有机物氧化催化剂等几个方面的介绍，旨在推动挥发性有机物治理特别是催化氧化技术的进展。
关键词：挥发性有机物；消除技术；催化剂
中图分类号：TK91 文献标识码：A 文章编号：0258-3283（2019）--
Research progress in catalytic oxidation technology and catalysts for volatile organic compounds HUANG Qing-bin* (Troops 92196 of People's Liberation Army, Shandong 266011, China) Huaxue Shiji, 2019, 41(2), ～
Abstract：In recent years, with the gradual deterioration of the ecological environment, the pollution control of volatile organic compounds has received more and more attention from experts and scholars from all walks of life. The treatment technology of volatile organic compounds mainly includes recovery technologies such as adsorption technology and catalytic technologies such as catalytic oxidation technology. Catalytic oxidation is a more thorough technique for the treatment of volatile organic compounds. It has the advantages of low energy consumption, no secondary pollution, good safety and wide application range. The introduction of volatile organic compounds treatment technology, catalytic oxidation mechanism and volatile organic oxidation catalysts is aimed at promoting the development of volatile organic compounds, especially catalytic oxidation technology.
Key words：volatile organic compounds; elimination technology; catalyst
基于石墨烯纳米复合材料的重金属离子电化学传感器研究
王新星*，高健，刘广茂，朱旭，崔久英，孙琪琪
(青岛科技大学 化学与分子工程学院 生态化工国家重点实验室培育基地 光电传感与生命分析教育部重点实验室 山东省生化分析重点实验室，山东 青岛 266042)
摘要：近年来，工业快速发展使得我国水污染现象日趋严重，其中，重金属离子含量超标是造成水污染的重要原因。因此，发展简便、快速、灵敏的重金属离子检测技术非常重要。电化学检测方法具有操作简单、制备成本低、灵敏度高和易于微型化等优点，在重金属离子检测中具有重要应用价值。基于热还原氧化石墨烯（TrGNO）-金纳米颗粒（AuNPs）复合材料构筑高性能电化学传感器平台，采用电化学方法实现对铜离子（Cu2+）的简便、快速、灵敏检测。文中采用透射电子显微镜和各种电化学技术对纳米复合材料及其修饰电极进行了形貌表征和电化学测试，并对材料制备和测试条件进行了优化。结果表明，通过TrGNO与AuNPs的有效复合，所制备的纳米复合材料具有增大的电极表面积和优异的导电性，有利于提高对Cu2+的电化学检测灵敏度。线性检测范围为1.0×10-6 ～ 5.0×10-4 mol/L，检测限可达8.5×10-7 mol/L。
关键词：热还原氧化石墨烯；金纳米颗粒；电化学传感器；重金属离子；铜离子
中图分类号：O657.1 文献标识码：A 文章编号：0258-3283（2019）--
Research on Graphene-based Electrochemical Sensor for the Detection of Heavy Metal Ions Wang Xin-xing*, Gao Jian, Liu Guang-mao, Zhu Xu, Cui Jiu-ying, Sun Qi-qi (Shandong Key Laboratory of Biochemical Analysis, Key Laboratory of Optic-electric Sensing and Analytical Chemistry for Life Science, Key Laboratory of Eco-chemical Engineering, Ministry of Education, College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042) Huaxue Shiji, 2019, 41(2), ～
Abstract: With the rapid development of industry, water pollution in our country is becoming more and more serious, and heavy metal ions are important pollutants. Therefore, it is an urgent demand to develop a simple, rapid and sensitive method for heavy metal ions detection. The electrochemical method shows great potential in this respect with the advantages of simple operation, low cost, high sensitivity and miniaturization. A thermally reduced graphene oxide (TrGNO) – Au nanoparticles (AuNPs) nanocomposite was fabricated and applied to the construction of electrochemical sensing platform for the detection of Cu2+. The morphology and electrochemical properties of the TrGNO –AuNPs nanocomposite were investigated by transmission electron microscopy and various electrochemical techniques. The results indicated that the electrode surface area and electrical conductivity were obviously improved by the synergistic effect of TrGNO and AuNPs, which are beneficial to improve the sensitivity of electrochemical detection of Cu2+. The electrochemical sensor showed good linear relationship with the concentration of Cu2+ in the range of 1.0×10-6 ～ 5.0×10-4 mol/L, and the detection limit is 8.5×10-7 mol/L.
Key words: thermally reduced graphene oxide; gold nanoparticles; electrochemical sensor; heavy metal ions; copper ion
锰酸锂电池正极材料高温包覆改性研究
姚年春*1，何玉林1, 2
（1. 江苏财经职业技术学院 机械电子与信息工程学院，江苏 淮安 223003；2.上海大学 材料科学与工程学院，上海 200072）
摘要：对尖晶石 LiMn2O4 材料进行表面修饰能够在一定程度上减少电极材料和电解液的直接接触，抑制锰元素溶解。通过Pechini法制备了不同包覆量（1、1.5和2 wt%）的锂镧锆氧固态电解质/锰酸锂复合材料。当包覆量为1.5 wt%时，复合正极材料首次放电容量达到112.5 mAh/g，在0.5C循环100次后容量损失率仅为8.6%。尖晶石晶粒表面形成了独特的网络状包覆层，减少了活性物质和有机电解液之间的直接接触却不影响锂离子扩散，显著提升了锰酸锂的高温电化学性能。
关键词：锂镧锆氧；锰酸锂；包覆
中图分类号: TQ152 文献标识码: A 文章编号:0258-3283(2019)--
Study on modification of anode material of manganic acid lithium battery coated at high temperature YAO Nian-Chun*1, HE Yu-Lin1, 2 (1. School of mechanical electronics and Information Engineering, Jiangsu Polytechnic of Finance and Economics, Huaian 223003, China; 2. School of Materials Science and Engineering, Shanghai University, Shanghai 200072, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: LiMn1.95Ni0.05O3.98F0.02/Li7La3Zr2O12 Composite anode materials are prepared by the Pechini method. The morphology of the coating layer varies as the weight percentage increases from 1.0 to 2.0. LiMn1.95Ni0.05O3.98F0.02 coated with 1.5 wt% Li-La-Zr-O solid electrolyte exhibits an initial discharge capacity of 112.7 mAh/g at 0.5C-rate and a capacity loss of only 8.6% after 100 cycles at 55 °C, while the coating material exists as distinct reticulation covering the surface. This improvement is caused by the presence of Li-La-Zr-O coating layer that can inhibit manganese dissolution without blocking Li+ migration. The morphology of coating materials has been controlled by adjusting the temperature of heat treatment during the coating process.
Key words: Li7La3Zr2O12; LiMn1.95Ni0.05O3.98F0.02; coating
抗炎药物分子诱导铁羰基化合物释放一氧化碳研究
冯勇，郑叶，方佳玲，赵娟，庞倩倩，姜秀娟*
(嘉兴学院 生物与化学工程学院，浙江 嘉兴 314001)
摘要:通过Fe3(CO)12和1-巯基甘油反应合成了一种二铁羰基化合物[Fe2{m-SCH2CH(OH)CH2(OH)}2(CO)6]。进一步通过红外光谱技术研究了该化合物在抗炎药物分子作用下的一氧化碳释放性能，结果表明含羧基抗炎药物可以作为有效的取代试剂与铁羰基化合物作用，诱导其分解释放一氧化碳（CO），可以作为潜在的一氧化碳释放分子（CORMs）。对一氧化碳释放反应进行动力学分析表明该过程符合准一级反应动力学，而且反应速率与抗炎药物的结构密切相关。
关键词：一氧化碳释放剂；二铁羰基化合物；羧基；抗炎药物
中图分类号：O614.8 文献标识码：A 文章编号：0258-3283（2019）--
The Study of Anti-inflammatory Drugs Initiation Carbon Monoxide releasing from Iron Carbonyl Complex FENG Yong, ZHENG Ye, FANG Jia-ling, ZHAO Juan, PANG Qian-qian, JIANG Xiu-juan* (College of Biological, Chemical Sciences and Engineering, Jiaxing University, Jiaxing 314001) Huaxue Shiji, 2019, 41(2), ～
Abstract: One diiron carbonyl complex [Fe2{m-SCH2CH(OH)CH2(OH)}2(CO)6] has been synthesized by the reaction of Fe3(CO)12 and 1-thioglycerol. Its carbon monoxide releasing ability was further investigated under the initiation of anti-inflammatory drugs by IR. The results indicate that the anti-inflammatory drugs with carbonylic group can serve as effective substitutive reagent to initiate the decomposition of the complex to release carbon monoxide (CO), which can serve as CO-releasing molecule. Kinetic analysis indicates that the CO-releasing progress is one-order kinetic reaction, and the CO-releasing rate is structural dependent on the anti-inflammatory drugs.
Key words: CO-releasing molecule; diiron carbonyl complex; carboxylic; anti-inflammatory drugs
油酸酰胺聚氧乙烯醚（7EO）磺基琥珀酸单酯二钠盐
的合成及性能研究
顾佳运，朱国华*，华平，喻红梅，陈衡，刘海涛，孙杰
（南通大学 化学化工学院，江苏 南通 226019）
摘要：以油酸酰胺聚氧乙烯醚（7EO）和顺丁烯二酸酐为原料、亚硫酸钠为磺化剂合成了油酸酰胺聚氧乙烯醚（7EO）磺基琥珀酸单酯二钠盐（OAPESS）。最佳合成工艺条件：n(聚醚）:n(顺酐）= 1:1.05，酯化温度130 ℃，时间为2.0 h，n（顺酐）:n(亚硫酸钠）= 1:1.05，磺化温度80 ℃，时间3.0 h，整个反应在氮气保护下进行。通过红外光谱、核磁共振氢谱确定了产品的结构，并考察了产品的性能。OAPESS的临界表面张力为33.09 mN/m，OAPESS溶液的消泡速率为0.02 cm/min，乳化时间为15 min，渗透性为14 s，钙皂分散性为20%，去污力为66.22%，増溶性为50 L/mol。上述的结果表明OAPESS具有良好的表面活性、润湿渗透性和泡沫稳定性。
关键词：磺基琥珀酸单酯二钠盐；合成；性能
中图分类号：TQ423.3 文献标识码：A 文章编号：0258-3283（2019）
Synthesis and Properties of Disodium Oleamide Polyoxyethlene Ether(7) Sulfosuccinate GU Jia-yun，ZHU Guo-hua*，HUA Ping，YU Hong-mei, CHEN Heng, LIU Hai-tao, SUN Jie (School of Chemistry and Chemical Engineering, Nantong University, Nantong 226019, China), Huaxue Shiji, 2019, 41(1),
Abstract: Disodium oleamide polyoxyethlene ether(7) sulfosuccinate（OAPESS）was synthesized from oleamide polyoxyethylene ether (7), maleic anhydride and sodium sulfite as sulfonating agent.The optimum conditions were as follows:The molar ratio of polyoxyethylene ether oleate (7) to maleic anhydride was 1:1.05,the reaction temperature and the reaction time were 130℃ and 2 h, respectively. The molar ratio of maleic anhydride to sodium sulfite was 1:1.05 ,the reaction temperature and the reaction time were 80℃ and 3 hours, respectively.This reaction was protected by nitrogen.The structure of the OAPESS was confirmed by FTIR and 1HNMR. The γcmc of OAPESS is 33.09 mN/m,the defoaming rate of solution OAPESS is 0.5px/min,the emulsifying time is 15 min,the infiltration time is 14 s, and the dispersibility LSDP is 20%, the detergency was 66.22 %,the solubility was 50 L/mol.The results indicated that OAPESS has good surface activity, wetting ability and stable performance.
Key words: sulfosuccinate; synthesis; performance
六硝基六氮杂异伍兹烷降感技术研究进展
屈晨曦，葛忠学*，张敏，许诚，毕福强，丁可伟
（西安近代化学研究所，陕西 西安 710065）
摘要：六硝基六氮杂异伍兹烷（HNIW，CL-20）是一种高能量密度新型含能材料，在单质炸药、混合炸药以及推进剂等方面有着广泛的应用前景。但是CL-20感度较高的特点限制了其进一步推广应用，对CL-20晶体进行晶体修饰处理可以有效地降低其感度。概述国内外CL-20晶体修饰降低感度技术研究进展，总结了共结晶和核壳结构包覆两种主要的晶体修饰降感方法，并对不同方法降感机理进行分析。对共结晶和核壳结构包覆这两种降感方法的研究现状进行梳理并对降感效果进行了总结和对比，最后分析该领域的研究趋势。
关键词：CL-20；晶体修饰；降感技术；核壳结构
中图分类号：O69 文献标识码：A 文章编号：0258-3283(2019)--
Reasearch Progress on Sensitivity Decrease Methods of Hexanitro-hexaazaisowurtzitane QU Chen-xi, GE Zhong-xue*, ZHANG Min, XU Cheng, BI Fu-qiang, DING Ke-wei (Xi’an Modern Chemistry Research Institute, Xi’an 710065, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: Hexanitrohexaazoisowurtziane (HNIW, CL-20) is a new energetic material with high energy density. It has broad application in explosive, mixed explosive and propellant. However, high sensitivity of CL-20 limits its further application. Crystal modification of CL-20 crystal can effectively reduce its sensitivity. The research progress of CL-20 crystal modification and sensitization reduction technology domestic and foreign is summarized. Main crystal modification methods are discussed, which are modification of cocrystal method and construction core-shell structure method. The mechanism of sensitization reduction by different methods is analyzed. Two different methods of decreasing sensitivity were introduced and effects of these different crystal methods in sensitivity decrease are compared. Finally, tendency of the research filed is pointed out.
Key words: CL-20, crystal modification, sensitivity decrease method, core-shell structure
临床应用含磷药物结构特点的综述
姚秋丽*，任林静，冉茂刚，何佳芯，向丹
(遵义医学院 药学院，贵州 遵义 563000)
摘要：临床上使用的含磷药物结构丰富、活性各异，但目前极少有文献或参考书籍针对含磷药物的结构特征和由于含磷基团的引入而对临床使用特点产生影响进行综述，这无疑为进一步探索具有潜在生物活性的含磷化合物的设计和合成带来诸多不便。针对该情况，将临床中使用的含磷药物按照其结构特点进行分类，阐述含磷基团的引入对药物活性的影响，为含磷新药物的研发提供思路。
关键词：含磷药物；前药；磷酸盐；膦酸盐
中图分类号：R914.4 文献标识码：A 文章编号：0258-3283（2019）--
Review on the Structures of Phosphorus-containing Drugs Used in Clinical Practice YAO Qiu-li*, REN Lin-jing, RAN Mao-gang, HE Jia-xin, XIANG Dan (School of Pharmacy, Zunyi Medical University, Zunyi 563000, China) Huaxue Shiji, 2019, 41(2), ～
Abstract：Phosphorus-containing drugs have various structures and show diverse clinical activities. Only few literatures had ever reviewed the structural features and the corresponding characteristics of clinical activities. This undoubtely makes inconvenience in the design and synthesis of phosphorus-containing compounds with potential biological acitivities. Phosphorus-containing drugs according to their characteristics of structures were categorized, and the differences of acitivities were further elaborated.The introduction of the phosphorus motieties, hoping to provide solutions for the design of new phosphorus-containing drugs.
Key words：phosphorus-containing drugs; prodrugs; phosphates; phosphonates
Gemini型双季铵盐阳离子表面活性剂的合成及应用研究进展
张萍1，臧凯2，袁彩彩2，石贤财2，章亚东*1
（1. 郑州大学 化工与能源学院，河南 郑州 450001；2.郑州大学 济源研究院，河南 济源 459000）
（2.
摘要：双子（Gemini）型双季铵盐阳离子表面活性剂以其独特的结构而具有良好的表面活性、较低的临界胶束浓度（CMC）等优良的物理性能。以间隔基团的不同综述了Gemini型双季铵盐阳离子表面活性剂的合成路线，并简要的介绍了Gemini型双季铵盐阳离子表面活性剂在杀菌、金属缓蚀、煤沥青润湿、乳化及作为基因和药物载体方面的应用，为Gemini型双季铵盐阳离子表面活性剂的后续研究提供了参考。并指出要重视其合成条件的优化，以降低生产成本，扩大Gemini型双季铵盐阳离子表面活性剂的应用范围。
关键词：Gemini型双季铵盐阳离子表面活性剂；合成；应用研究
中图分类号：TQ423.12 文献标识码：A 文章编号：0258-3283(2019)—
Progress in Synthesis and Application of Gemini double quaternary ammonium Cationic Surfactants ZHANG Ping1, ZANG Kai2, YUAN Cai-cai2, SHI Xian-cai2, ZHANG Ya-dong*1 (1. Chemical and Energy Institute, Zhengzhou University, Zhengzhou 450001, China; 2. Jiyuan Research Institute, Zhengzhou University, Jiyuan 459000, China) Huaxue Shiji, 2019, 41(2), ～
Abstract: Gemini-type double quaternary ammonium cationic surfactant has excellent physical properties such as good surface activity and low CMC. The synthetic routes of Gemini-type double quaternary ammonium cationic surfactant are reviewed in terms of spacer groups. Gemini-type double quaternary ammonium cationic surfactant was briefly described for sterilization, metal corrosion inhibition, and coal bitumen wetting. Emulsification and its application as a gene and drug carrier provide a reference for subsequent investigation of Gemini-type double quaternary ammonium cationic surfactant. It also pointed out that it is necessary to pay attention to the optimization of the synthesis conditions, and to reduce the production cost. It is possible to use Gemini-type double quaternary ammonium cationic surfactant in real life.
Key words: Gemini-type double quaternary ammonium cationic surfactant; synthesis; applied research
水溶性阳离子柱[5]芳烃还原石墨烯复合物在荧光检测左旋肉碱中的应用研究
谭晓平*1，石洪凡2，朱乾华1，罗莎莎1，张庭璎1，杨阳1
（1. 长江师范学院 化学化工学院，重庆 涪陵 408100；2.云南省食品药品监督检验研究院，云南 昆明 650000）
摘要: 采用湿化学还原法，在还原氧化石墨烯表面引入水溶性大环主体超分子柱[5]芳烃（CP5），形成复合物CP5-RGO。采用FTIR、XPS对复合物CP5-RGO进行表征。使用罗丹明123（R123）作为探针分子，CP5-RGO作为受体来构建荧光传感器，以此来检测左旋肉碱，其线性范围为0.1 ～ 2.0 μmol/L和2.0 ～ 25.0 μmol/L，检出限为0.034 μmol/L。以牛奶为实际样品，采用加标回收方法探讨了R123@CP5-RGO传感器的实用性，其回收率为91.0 % ～ 100.2 %，相对标准偏差为2.0 % ～ 2.6 %。所构建的荧光传感平台R123@CP5-RGO具有快速、灵敏、简便等优点，有望应用于实际样品的检测。
关键词：水溶性阳离子柱[5]芳烃；还原氧化石墨烯；罗丹明123；左旋肉碱
中图分类号：O652.7 文献标识码：A 文章编号：0258-3283(2019)--
Application Research on the Fluorescence Detection of L-carnitine by Water-soluble Cationic Pillar[5]arene-Reduce Graphene composite TAN Xiao-Ping*1, SHI Hong-Fan2, ZHU Qian-Hua1, LUO Sha-Sha1, ZHANG Ting-Ying1, YANG Yang1 (1. School of Chemistry and Chemical Engineering, Yangtze Normal University, Fuling 408100, China; 2. Yun Nan Institute for Food and Drug Supervision and Inspection, Kunming 650000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: A wet-chemistry reduction method was used to introduce a water-soluble cationic pillar[5]arene (CP5) onto the graphene surface to form composite CP5-RGO. The CP5-RGO was characterized by FTIR and XPS. A novel competitive fluorescence sensing platform towards L-carnitine was developed based on the receptor CP5-RGO and probe R123. Low detection limit of 0.034 μmol/L (S/N ＝ 3) and linear response ranges of 0.1 ～ 2.0 μmol/L and 2.0 ～ 25.0 μmol/L for L-carnitine were obtained. It was successfully utilized to detect L-carnitine in milk samples and the recoveries were in the range of 91.0 ～ 100.2% and RSDs were in the range of 2.0 ～ 2.6%. The fluorescent sensor platform based on R123@CP5-RGO holds the advantages of rapidness, simplicity, and high sensitivity, which is expected for the detection of practical samples.
Key words: water-soluble cationic pillar[5]arene; reduce grapheme oxide; R123; L-carnitine
羧化碳纳米管修饰电极同时测定邻、对苯二酚
常凤霞*，王宇，刘思麟，张熠佳
(西南民族大学 化学与环境保护工程学院，四川 成都 610041)
摘要：采用滴涂法将羧化多壁碳纳米管（c-MWCNT）修饰于玻碳电极表面，以此修饰电极采用循环伏安法对邻苯二酚和对苯二酚进行测定，二者的氧化峰和还原峰峰电位差均超过100 mV，可实现对邻、对苯二酚的同时测定。对测定条件，包括底液pH、c-MWCNT修饰量进行了优化，研究了峰电流与扫描速度的关系。在优化的实验条件下，氧化峰电流与邻苯二酚和对苯二酚浓度在5.00×10-5 ～ 5.00×10-3mol/L范围内呈现良好的线性关系，检出 限（S/N ＝ 3）分别为4.30×10-6 mol/L和3.80×10-6 mol/L，检测了加标自来水样和湖水样的回收率，获得了满意的结果。
关键词：羧化碳纳米管；邻苯二酚；对苯二酚；同时测定
中图分类号：O657.1 文献标识码：A 文章编号：0258-3283(2019)--
Simultaneous Detectionof Catechol and Hydroquinone by Carboxylated Carbon Nanotubes Modified Electrode CHANG Feng-xia*, WANG Yu, LIU Si-lin, ZHANG Yi-jia (College of Chemistry and Environmental Protection Engineering, Southwest Minzu University, Chengdu 610041, China) Huaxue Shiji, 2019, 41(2), ～
Abstract:The electrochemical behavior and detection conditions of catechol and hydroquinone were explored by cyclic voltammetry. The results showed that both of the oxidation and reduction peak potential differences between catechol and hydroquinone exceeded 100 mV, which was sufficient to distinguish the two isomers. And the cathodic and anodic peak currents were proportional to the square root of scan rates, indicating that the electrochemical processes were diffusion controlled. In the phosphate buffer solution (pH 7.38), the peak currents showed good linear relationships with concentrations of catechol and hydroquinone in the range of 5.00×10-5 ～ 5.00×10-3 mol/L with detection limits of 4.30×10-6 mol/L and 3.80×10-6 mol/L (S/N＝3), respectively. And the recovery rates of the spiked tap water and lake water were also in satisfied range. The method was facile, easy-operated and low-cost, and may be applied to detect catechol and hydroquinone in the polluted water.
Key words: carboxylated carbon nanotubes; catechol; hydroquinone;simultaneous detection
超高效液相色谱-四极杆-飞行时间质谱法检测茶叶中玉米赤霉烯酮
王丹a，姚婷*a，甘卓亭b，汪勇a，张婷a，刘玉娟a
（黄山学院 a.分析测试中心，b.旅游学院，安徽 黄山 245041）
摘要：为探索检测茶叶中玉米赤霉烯酮的较佳方法，建立了发酵黑茶中玉米赤霉烯酮的超高效液相色谱串联四极杆飞行时间质谱（UPLC-Q-TOF-MS）检测方法。用甲醇水溶液(V（甲醇）︰V（水） = 7︰3)提取玉米赤霉烯酮，以乙腈-水溶液为流动相，采用负模式，借助UPLC-Q-TOF-MS进行测定分析。玉米赤霉烯酮的质量浓度为0.02 ～ 5.0 μg/mL时，浓度与峰面积呈良好的线性关系；方法检出限（LOD，S/N≥3）为2 μg/kg，定量限（LOQ≥10）为6.6 μg/kg，相对标准偏差（RSD）为1.3 % ～ 6.8 %；同时，不同茶叶样品的3个加标水平下，玉米赤霉烯酮的平均回收率为86.9 % ～ 105.5 %。利用该方法检测32个黑茶样品中的玉米赤霉烯酮，结果显示，32个黑茶样品中的玉米赤霉烯酮的含量均低于国家标准，该方法操作简单、选择性好、灵敏度高，满足茶叶中玉米赤霉烯酮的测定要求。
关键词：玉米赤霉烯酮；超高效液相色谱串联四极杆飞行时间质谱；黑茶；残留分析
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283（2019）--
Determination of Zearalenone in fermented dark tea by Ultra Performance Liquid Chromatography-Quadrurpole-Flight Time Mass Spectrometry Wang Dana, Yao Ting*a, Gan Zhuo-tingb, Wang Yonga, Zhang Tinga, Liu Yu-juana (a. Analysis and Testing Center; b. School of Tourism, Huangshan University, Huangshan 245041, China) Huaxue Shiji,2019,41(2), ～
Abstract: For a better way to detect zearalenone in fermented dark tea, a method with ultra performance liquid chromatography - MS quard-flight time mass spectrometry (UPLC-Q-TOF-MS) for detecting zearalenone in fermented dark tea was established. Zearalenone was extracted by using the solution of V(methanol):V(water) ＝7: 3, which was determined and analyzed using UPLC-Q-TOF-MS with acetonitrile and water as mobile phase and the negative model. The good linear relation between the peak area and the concentration was presented when the mass concentration range of zearalenone is 0.02 ～ 5.0 μg/mL. The detecting limit (LOD, S/N≥3) is 2 μg/kg, the quantitative limit (LOQ≥10) is 6.6 μg/kg, and the relative standard deviation (RSD) of 1.3 % ～ 6.8 %. At the same time, the method was used to detect the zearalenone in 32 dark tea samples, the average recovery rate of the zearalenone in different samples is 86.9 % ～ 105.5 %. The results showed that the contents of zearalenone in 32 dark tea samples were below the national standard. This method is suitable for the requirements of determination of zearalenone in dark teas due to simple operation, good selection and high sensitivity.
Key words: zearalenone; high performance liquid chromatography-tandem mass spectrometry; dark tea; residue analysis
顶空-气相色谱/质谱分析水果味电子烟烟气粒相物
挥发性成分
邹艳1a，郭鹏1b，张博2，张文洁2，朱远洋2，郑美玲2，彭周舟2，冯银龙*3
（1. 红塔辽宁烟草有限责任公司 a.沈阳卷烟厂，b.技术中心，辽宁 沈阳 110000；2.郑州轻工业学院 食品与生物工程学院，河南 郑州 450002；3.河南中烟工业有限责任公司 技术中心，河南 郑州 450000)
摘要：为分析电子烟烟气粒相物挥发性成分，建立了一种顶空（HS）-气相色谱质谱联用（GC/MS）方法，测定了3种水果味电子烟烟气粒相物挥发性成分。研究表明，顶空平衡温度120 ℃，平衡时间20 min时的捕集效率最佳；3种电子烟中分别鉴定出26、23、20种烟气粒相物挥发性成分，其中相对含量较高的是丙二醇，均占每种总含量的80％以上；5次重复实验的组分峰面积的RSD为3.64%，方法重复性良好；电子烟烟气中主要的致香成分为2, 3-丁二酮、乙酸乙酯、乙酸甲酯、反-3-己烯醇、3-甲基-2-戊醇、2-庚醇。实验方法操作简便、重复性好、无溶剂残留，适于电子烟烟气粒相物挥发性成分的分析。
关键词：电子烟；粒相物；挥发性成分；顶空法；气相色谱质谱联用
中图分类号：O0657.7 文献标识码：A 文章编号：0258-3283(2019)--
Analysis of Particulates Volatile Components from Fruit-flavored E-cigarette Smoke by Headspace-gas Chromatography-mass Spectrometry ZOU Yan1a，GUO Peng1b，ZHANG Bo2，ZHANG Wen-Jie2，ZHU Yuan-Yang2，ZHENG Mei-Ling2，PENG Zhou-Zhou2，FENG Yin-Long*3 (1a.Shenyang Cigarette Factory, 1b.Technology Center, Hongta Liaoning Tobacco Industry Co., Ltd., Shenyang 110000, China；2.School of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450002, China；3. Technology Center, China tobacco Henan Industrial Co., Ltd., Zhengzhou 450000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract:In order to analyze the volatile component of the E-cigarette smoke particulates, a headspace (HS)-gas chromatography-mass spectrometry (GC/MS) method was established to determine the volatile component of three fruit-flavored E-cigarette smoke particulates. The results showed that the capture efficiency with the headspace equilibrium temperature of 120 °C and the equilibrium time of 20 min was the best. 1# ～ 3# E-cigarette smoke particulates identified 26, 23, 20 volatile components, respectively, of which the higher content is propylene glycol accounting for more than 80% of its total content. RSD of the component peak area of the five repeated tests was 3.64%, and the method was good repeatability. The main aroma components in electronic cigarette smoke were 2, 3-butanedione, ethyl acetate, methyl acetate, trans-3-hexenol, 3-methyl-2-pentanol, 2-heptanol. The experimental method was simple in operation, good in repeatability and solvent-free, and was suitable for analysis of volatile components of E-cigarette smoke particulates.
Key words: E-cigarette; particulates; volatile components; headspace; gas chromatography-mass spectrometry
硫酸奎宁荧光探针在Fe3+检测中的应用
李敏*1, 2，敬小莉1，谈文林1
（1. 达州职业技术学院 基础教育部， 四川 达州 635000；2.四川文理学院 化学化工学院, 四川 达州 635000）
摘要：硫酸奎宁作为荧光试剂，最大激发波长为350 nm，最大发射峰位于450 nm处。硫酸奎宁与不同浓度的Fe3+混合后，发生荧光猝灭，lg（I0/I）与c（Fe3+）呈良好的线性关系，基于此建立了硫酸奎宁荧光探针检测Fe3+的新方法。研究表明，该方法检测Fe3+浓度的线性范围为0.7 ～ 400 μmol/L，相关系数为R ＝ 0.9995，检测限为140 nmol/L。在实际样品分析中，当分别加入4、10和70 μmol/L Fe3+时，回收率为99.4% ～ 100.4%，RSD为0.8% ～ 2.1%。该方法操作简便、反应速度快、灵敏度高，能用于实际样品中Fe3+的检测分析。
关键词：硫酸奎宁；荧光探针；猝灭；Fe3+
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283(2019)--
Application of Quinine Sulfate fluorescence probe in the Detection of Fe3+ Ion LI Min*1, 2, JING Xiao-li1, TAN Wen-lin1 (1.Department of Basic Education, Dazhou Vocational and Technical College, Dazhou 635000, China; 2. Department of Chemistry and Chemical Engineering, Sichuan University of Arts and Science, Dazhou 635000, China), Huaxue Shiji, 2019,41(2), ～
Abstract: As a fluorescent reagent, quinine sulfate has a maximum excitation wavelength of 350 nm and a maximum emission peak of 450 nm. When quinine sulfate was mixed with different concentrations of Fe3+, the fluorescence of quinine sulfate was quenched. It was found that lg(I0/I) showed a good linear relationship with the concentration of c(Fe3+). Based on this, a new method was developed for the detection of Fe3+ by quinine sulfate as a fluorescent probe. The linear range of Fe3+ concentration was 0.7 ～ 400 mmol/L with a correlation coefficient of 0.9995. The limit of detection was140 nmol/L. When 4, 10, 70 mmol/L Fe3+ were added to the real samples, the recovery ranges 99.4% ～ 100.4% and the relative standard deviation (RSD) ranges 0.8% ～ 2.1%. This method was simple, rapid and sensitive and can be used for the detection of Fe3+ in real samples.
Key words: Quinine sulfate; fluorescent probe; quenched; Fe3+
奶粉中金黄色葡萄球菌标准样品的均匀性和稳定性研究
李妍1，罗超1，李兰英1，颜娟2，范一灵3，杨燕3，刘刚*1
（1. 上海市计量测试技术研究院 化学与电离辐射所，上海201203；2.上海海洋大学 食品学院，上海 201306；3.上海市食品药品检验所，上海201203）
摘要：人工制备的奶粉中金黄色葡萄球菌标准样品，进行均匀性和不同储存条件下稳定性的实验研究。奶粉中高密度菌体和低密度菌体标准样品的均匀性统计学结果变异小，均匀性良好；两种密度菌体在-80 ℃保存半年后，活菌数没有显著变化，符合稳定性统计学要求，提高保存温度之后，低密度菌体标准样品可以在-20 ℃下保存半年以上，而高密度标准样品的活菌数在-20 ℃下保存40 d后开始下降，直到70 d后达到稳定，继续提高保存温度，高密度菌体标准样品在4 ℃下保存稳定性较差，而低密度菌体标准样品在4 ℃可以稳定7 d。综上所述，得出低密度菌体的奶粉中金黄色葡萄球菌标准样品可以满足实验室质量控制和方法验证的基本需求，保障量值准确统一，保证检测结果的有效性、可比性及国际国内互认度。
关键词：金黄色葡萄球菌；标准样品；均匀性；稳定性
中图分类号：Q819 文献标识码：A 文章编号： 0258-3283(2019)--
Homogeneity and Stability Study on Standard Reference Materials of Staphylococcus aureus in Milk Powder LI Yan1, LUO Chao1, LI Lan-Ying1, YAN Juan2, FAN Yi-Ling3, YANG Yan3, LIU Gang*1 (1. Division of Chemistry and Ionizing Radiation Measurement Technology, Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China; 2. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China; 3. Shanghai Institute for Food and Drug Control, Shanghai 201203, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: A group of reference material (RM) candidates of high and low-level of staphylococcus aureus in milk powder was developed for the quality control and method validation in laboratory. The homogeneity and stability of the RM candidates were investigated. The homogeneity statistical results of small variation demonstrated good uniformity of both high and low-level bacteria SRM candidates. The long-term stability investigation results showed that the numbers of living bacteria of both high and low-level were stable over 6 months under -80 °C, and if the storage temperature was increased to -20 °C, the low-level RM could keep stable for 6 months, but the high-level bacteria RM’s living number declined from 40 days and reached a plateau at 70 days. Then, if the storage temperature was further increased to 4 °C, the living number of the high-level RM decreased dramatically in 2 days while the low-level RM could keep stable for 7 days which is adequate for the sample delivery by using cold chain transportation. In conclusion, the low-level RM of staphylococcusaureusin milk powder SRM candidate would be used in laboratory quality control and method validation for the promotion of the validity and comparability of the test results, and the domestic and international mutual recognition.
Key words: Staphylococcus aureus; standard reference material; homogeneity; stability
基于壳聚糖衍生物的Al3+荧光探针的设计合成
林锦斌a，徐宏达a，叶伟a，傅琼瑶a，陈瑞a，曾莉芳a，张军*a, b
（海南医学院a. 热带医学与检验医学院环境监测实验室，b. 国际教育学院，海南 海口 571199）
摘要：人体摄入过量的Al3+会导致多种疾病，因此Al3+的检测具有重要的意义。荧光探针法在目标物质检测中具有选择性好、灵敏度高等优点，已成为重要的检测手段。以2-羟基-1-萘甲醛和羧甲基壳聚糖为原料，在乙醇溶液中回流反应8 h，高产率得到一种高选择性Al3+荧光探针P。在常见的金属离子和阴离子中，该荧光探针对Al3+呈现出较好的选择性和较高的灵敏度。在V（乙醇）∶V(水） ＝ 4:1、pH 6.0、50 mmol/L HEPES溶液中，该探针对Al3+的线性响应范围为4.0×10−5 ～ 1.0×10−4 mol/L，检出限为1.3×10-5 mol/L。
关键词：壳聚糖；荧光探针；Al3+
中图分类号：O022.7 文献标识码：A 文章编号：0258-3283(2019)--
Design and Synthesis of Al3+-Selective Fluorescent Probe Based on Chitosan Derivative LIN Jin-bina, XU Hong-daa, YE Weia, FU Qiong-yaoa, CHEN Ruia, ZENG Li-fanga, ZHANG Jun*a, b (1. Laboratory of Environment Monitoring, School of Tropical and Laboratory Medicine, 2．School of International Education, Hainan Medical University, Haikou 571199, China) Huaxue Shiji, 2019, 41(2), ～
Abstract：Overtake of Al3+ causes various diseases. Thus, the detection of Al3+ is of great importance. Among the detection methods, fluorescent probe method has many advantages, such as good selectivity and high sensitivity. Al3+-Selective fluorescent probe P was synthesized using 2-hydroxy-1-naphthaldehydes and carboxymethyl chitosan as raw materials. Probe P showed good selectivity to Al3+ compared to other tested metal ions and anions. The proposed probe P showed a wide linear range of 4.0×10−7 ～ 1.0×10−4 mol/L with detection limit of 1.3×10-5 mol/L Al3+ in water-ethanol solution (V(ethanol)∶V(water) ＝ 4∶1, pH6.0, 50 mmol/L HEPES).
Key words：chitosan; fluorescent probe; Al3+
以三苯胺衍生物为识别基的共轭聚合物荧光探针的合成及性能
陈珍娥*1, 2，张海1, 2
（遵义师范学院1. 化学化工学院；2. 黔北特色资源应用研究实验室，贵州 遵义 563002）
摘要：以三苯胺衍生物为识别基，通过Suzuki偶联反应，成功设计和合成了1种新的共轭聚合物，利用核磁共振谱、红外光谱、凝胶渗透色谱对合成的目标产物进行了结构表征，并研究了探针在DMF溶液中的紫外吸收和荧光性质。研究表明，探针能选择性识别Ag+，在3. 00× 10-6～7.00× 10-6 mol /L Ag+浓度范围内线性关系良好, I0/I ＝ 1.03 + 0.026 c[Ag+]（×10-6），线性相关系数R ＝ 0.997。
关键词：三苯胺衍生物；芴；Ag+；荧光探针
中图分类号：O621.3 文献标识码：A 文章编码：0258-3283(2019)—
Synthesis and Properties of Conjugated Polymer with Triphenylamine Derivatives as Recognition Units CHEN Zhen-e*1, 2, ZHANG Hai1, 2 (a.School of Chemistry and Chemical Engineering; b. Qianbei Featured Resources Applied Research Laboratory, Zunyi Normal College, Zunyi 563002, China), Huaxue Shiji, 2019,41(1), ～
Abstract: A novel conjugated polymer was synthesized by Suzuki coupling reaction with triphenylamine derivatives as recognition units. The structure was confirmed by NMR, IR and GPC. The properties of polymer were investigated by UV-Vis and fluorescence spectroscopy in DMF/H2O solution. The results revealed that polymer showed the selective fluorescence quenching in the presence of Ag+ as compared to other metal cations(Na+, K+,Mg2+,Ba2+, Al3+,Zn2+, Fe3+,Pb2+, Cu2+, Hg2+,Co2+,Cr2+, Cd2+, Ni2+ and Mn2+). The concentration of Ag+ was in the range of 3. 00× 10-6～7.00× 10-6 mol/L with linear equation as I0/I ＝ 1.03 + 0.026[Ag+] and the correlation coefficient of R = 0. 997．
Key words: triphenylamine derivatives; fluorine; Ag+; fluorescent probe
恩诺沙星–d5的合成
梁大伟*，王悦秋，谭琳
(雅安职业技术学院 药学与检验系，四川 雅安 625000)
摘要：以乙醇-d6为原料，与碘反应得到碘乙烷-d5，进一步与1-Boc-哌嗪经过两步反应得到中间体1-乙基哌嗪-d5，然后与1-环丙基-7-氯-6-氟-1,4-二氢-4-氧代喹啉-3-羧酸乙酯发生Buchwald-Hartwig偶联反应得到1-环丙基-6-氟-1,4-二氢-4-氧-7-(4-乙基-1-哌嗪基)-3-喹啉羧酸乙酯–d5，最后经碱水解后得到标题化合物，5步总收率为52%，其结构经1HNMR、13CNMR、IR与MS表征，化学纯度为99.5%，同位素丰度为99.3%，可作为食品安全领域检测用稳定同位素内标试剂。
关键词：氘代标记；恩诺沙星；合成
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283(2019)--
Synthesis of Enrofloxacin-d5 LIANG Da-wei*, WANG Yue-qiu, TAN Lin (Department of Pharmacy & Inspection, Ya’an Polytechnic College, Ya’an, 625000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract：The synthesis of enrofloxacin–d5 has been achieved in five steps as follows: iodination of CD3CD2OD with I2 to yield CD3CD2I, which was used to ethylation of 1-Boc-piperazine in 2 steps provided 1 –ethylpiperazine –d5. The key ethyl 1 -cyclopropyl- 7-(4-ethylpiperazin-1-yl) -6-fluoro-4-oxo- 1, 4-dihydroquinoline -3-carboxylate–d5 was constructed from 1-ethylpiperazine–d5 and ethyl 7-chloro-1- cyclopropyl-6- fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylate via a Buchwald–Hartwig coupling reaction. The final step was a hydrolyzation by alkaline. The total yield was 52%, and the structure was confirmed by 1HNMR, 13CNMR, IR and MS. The purity was 99.5% and isotopic enrichment of D was 99.3%. It could be used as an internal standard in the field of food safety detection.
Key words：deuterium labeled; enrofloxacin; synthesis
固定化酶解法合成7-ACA的方法研究
张宏*1，王艳戎2，罗兰1
（1.四川化工职业技术学院 化学工程系，四川 泸州 646099；
2.泸州职业技术学院 科技产业处，四川 泸州 646000）
摘要：天然类头孢菌素C通过化学或酶解法可制得半合成头孢菌素的重要母核7-氨基头孢烷酸（7-ACA）。主要研究头孢菌素C在自制固定化CA-Co-Fe/KIT-6催化下，通过一步裂解制备7-ACA的方法，先自行合成负载Co-Fe活性组分的KIT-6载体，再将头孢菌素脱酰酶通过物理吸附固定在Co-Fe/KIT-6上。经正交实验，优化了7-ACA的制备条件为：温度28 ℃，pH 8.0，底物浓度4%，固定化CA酶用量0.3 g，时间40 min，反应液中7-ACA浓度93.5%，收率84.3%。第5次使用经离心回收的固定化CA-Co-Fe/KIT-6，其相对酶活性为87.6%，7-ACA收率为78.4%。
关键词：头孢菌素C；头孢菌素脱酰酶；7-ACA
中图分类号：TQ45 文献标识码：A 文章编号：0258-3282(2019)--
Researching on Synthesis of 7-ACA by Immobilized Enzymatic Hydrolysis ZHANG Hong*1, WANG Yan-rong2, LUO Lan1 (1. Department of Chemical Engineering, Sichuan Vocational College of Chemical Industry, Luzhou 646099, China; 2. Department of Science and Technology Industry, Luzhou Vocational and Technical College, Luzhou 646000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: The cephalosporin antibiotic is a broad-spectrum antibiotic with high antibacterial activity and low irritation of β-lactone amine, and is a very important anti-infective drug. Semi-synthetic cephalosporin is superior to natural cephalosporin in terms of antibacterial activity, antibacterial range, pharmacokinetics, etc., and its clinical application is developing rapidly. The natural cephalosporin C can produce the important parent nucleus 7-aminocephalosporanic acid (7-ACA) of semi-synthetic cephalosporin by chemical or enzymatic hydrolysis. The cephalosporin C is catalyzed by self-immobilized CA-Co-Fe/KIT-6 to produce 7-ACA by one-step pyrolysis. The KIT-6 carrier carrying the Co-Fe active component is synthesized by itself, and the cephalosporin is deacylated. The enzyme was immobilized on Co-Fe/KIT-6 by physical adsorption; the immobilized cephalosporin deacylase cleavage cephalosporin C was determined by orthogonal experiment to obtain the optimal reaction conditions for the preparation of 7-ACA: temperature 28 ℃, pH 8.0, substrate concentration 4%, immobilized CA enzyme dosage 0.3 g, reaction time 40 min, 7-ACA concentration 93.5%, and yield 84.3%. For the 5th time, the immobilized CA-Co-Fe/KIT-6 recovered by centrifugation was used, and its relative enzyme activity was 87.6%, and the 7-ACA yield was 78.4%.
Key words: cephalosporin C; cephalosporin deacylase; 7-ACA
2-芳基取代的吡啶并[2,3-d]嘧啶衍生物的合成
刘娥*，李立威，姚明，张冕
(荆楚理工学院 化工与药学院，湖北 荆门 448000）
摘要：以2-氨基-3-氰基吡啶为起始原料，先制备得到3-氨甲基吡啶-2-胺，在氯化亚铜、三乙烯二胺和2,2,6,6-四甲基-1-哌啶氧催化体系下，得到几种2-芳基取代的吡啶并[2,3-d]嘧啶衍生物。同时考察了反应温度、反应溶剂、反应时间对反应收率的影响。该方法具有操作简便，后处理简单、反应收率高的特点。目标化合物结构经1HNMR、13CNMR和LC-MS确证。
关键词：2-芳基；吡啶并[2,3-d]嘧啶；合成
中图分类号：O626 文献标识码：A 文章编号：0258-3283（2019）
Synthesis of 2-Aryl substituted pyridio[2,3-d]pyrimidine Derivatives LIU E*，LI Li-wei，YAO Ming，ZHANG Mian （College of Chemical Engineering and Pharmacy，Jingchu University of Technology，Jingmen 448000, China）, Huaxue Shiji, 2019, 41(1),
Abstract: Using 2-amino-3-cyanylpyridine as starting material, the 3-aminomethylene-2-amine was first prepared. Several 2-aryl substituted pyridio[2,3-d]pyrimidine derivatives were designed and synthesized , by using CuCl/DABCO/TEMPO as the catalysts. The effects of reaction temperature, solvent and time on reaction yield were also investigated. This method has the advantages of simple operation, simple post-treatment and high reaction rate. The structure of the compound was confirmed by 1HNMR、13CNMR and LC-MS.
Key words: 2-aryl; pyridio[2,3-d]pyrimidine; synthesis
铜催化合成艾拉莫德中间体杂质
刘巧云*1，王宏义1，秦海芳1，杨怡1，高雨琼1，陈剑2，赵金亮2
（1.常州工程职业技术学院，江苏 常州 213164；2.常州佳德医药科技有限公司，江苏 常州 213164）
摘要：3-甲磺酰胺基-4-苯氧基苯甲醚是合成抗风湿新药艾拉莫德的关键中间体，但在制备过程中生成了一种双取代产物的工艺杂质，且分离困难。开发一种高效制备艾拉莫德中间体的工艺杂质3-(N,N-二甲磺酰基)胺基-4-苯氧基苯甲醚的新方法，即由5-甲氧基-2-苯氧基苯胺经桑德迈尔反应碘代、再经铜催化反应制得。考察了铜催化反应的催化剂、缚酸剂、反应温度、溶剂对反应的影响。结果表明：Cu(OAc)2·H2O/1,10-菲罗啉为催化剂和配体、碳酸钾为缚酸剂、DMSO为溶剂，100 ℃反应8 h能够以良好的反应收率得到产物。其结构经1HNMR、13CNMR、DEPT谱和质谱确证。该方法具有步骤简单、收率高等特点，为艾拉莫德及中间体的杂质研究和质量控制提供了帮助。
关键词：铜催化；艾拉莫德中间体；杂质研究；合成
中图分类号：R971 文献标识码：A 文章编号：0258-3283（2019）
Synthesis of Iguratimod Intermediate Impurity via Copper Catalysis LIU Qiao-yun*1, WANG Hong-yi1, QIN Hai-fang1, YANG Yi1, GAO Yu-qiong1, CHEN Jian2, ZHAO Jin-liang2 (1.Changzhou Institute of Engineering Technology, Changzhou 213164, China；2.Changzhou Jiade Pharmaceutical Technology Co., Ltd, Changzhou 213164, China), Huaxue Shiji, 2019, 41(1),
Abstract: 3-Methylsulfonamido-4phenoxyanisole is a key intermediate for synthesizing the anti-rheumatic new drug Iguratimod. However, a process-related impurity of disubstituted product of which formed during the preparation process and was difficult for separation. In this work, a novel effective procedure for preparing 3-(N,N-dimethylsulfonyl) amido-4-phenoxyanisole, the Iguratimod intermediate impurity, was developed. It was prepared by Iodination of 5-methoxy-2-phenoxyaniline via Sandmeyer reaction, and then by copper-catalyzed reaction. The influences of catalyst, deacid reagent, temperature and solvent of the copper-catalyzed reaction were investigated. The results indicated that the procedure proceeds smoothly to give the corresponding products in good yield by using Cu(OAc)2·H2O/1,10-phenanthroline as catalyst/ligand, with K2CO3 and DMSO for 8 h at 100 ℃. The structure was confirmed by 1HNMR, 13CNMR, DEPT and MS. This reaction method has advantages of simple procedure and high yield, and is helpful for impurity research and quality control of Iguratimod and its intermediates.
Key words: copper-catalysis; Iguratimod intermediate; impurity study; synthesis
