基于WO3-纳米棒复合石墨烯薄膜修饰玻碳电极的DNA传感平台
郑德论*1，张锐龙1，陈键侨1，王呈文1，张彩云1，陈学武1，汪庆祥2，高凤2
(1.汕头职业技术学院 自然科学系, 广东 汕头 515041; 2. 闽南师范大学 化学与环境科学院，福建 漳州 363000)
摘要：以棒状WO3纳米粒子（rWO3）、石墨烯（GR）和壳聚糖（CTS）形成的纳米复合材料修饰玻碳电极（GCE）为平台，制备了一种新型电化学DNA生物传感器。电化学实验表明，复合膜层中WO3纳米粒子和GR的协同效应增大了电极表面积，导致其电化学响应信号明显增强。通过CTS-WO3-GR杂化膜层丰富的氨基官能团和引入双功能手臂分子对苯二甲醛（TPA），将探针ssDNA稳固组装于传感界面。该DNA生物传感器集合了复合膜材料的许多优点，如：CTS良好的生物相容性和成膜能力，rWO3纳米粒子和GR优异的电子转移能力等。在最佳条件下，以亚甲基蓝（MB）为电化学信号分子，采用差分脉冲伏安法（DPV）检测特异性ssDNA序列的浓度范围为1.0×10-14 ～1.0×10-8 mol/L，并获得较低的检测限值2.7×10-15 mol/L（3σ）。该生物传感器对单碱基和三碱基错配的ssDNA序列也表现出良好的稳定性和识别能力。
关键词：棒状WO3；石墨烯；复合膜层；对苯二甲醛；DNA 生物传感器
中图分类号: 0621.2 文献标识码: A 文章编号：0258-3283（2019）
Novel DNA Sensing Platform Based on Glassy Carbon Electrode Modified with WO3-Nanorod Composite Graphene Film ZHENG De-lun*1, ZHANG Rui-long1, CHEN Jiang-qiao1, WANG Cheng-wen1, ZHANG Cai-yun1, CHEN Xue-wu 1, WANG Qing-xiang 2, GAO Feng2 (1. Department of Natural Sciences, Shantou Polytechnic, Shantou 515078, China; 2. Department of Chemistry and Environmental Sciences, Minnan Normal University, Zhangzhou 363000, China), Huaxue Shiji, 2019, 41(3)
Abstract: A new electrochemical DNA biosensor was fabricated by using a rod-like WO3 (rWO3), graphene (GR) and chitosan (CTS) nanocomposite materials modified glassy carbon electrode (GCE) as the platform. The basal electrode of CTS-WO3–GR/GCE was applied to the electrochemical experiments and the obtained data indicated that the synergistic effect of nano-WO3 and GR increased the surface area of the electrode and resulted in the corresponding increase of the electrochemical responses. The CTS-WO3–GR hybrid film with rich amino groups was further employed as functional matrix for probe ssDNA immobilization using terephthalaldehyde (TPA) as a bifunctional arm-linker. The DNA biosensor has the advantages such as the good biocompatibility and film-forming ability of CTS, the excellent electron transfer ability of rWO3 or GR. Under the optimal conditions, differential pulse voltammetry (DPV) was used to record the electrochemical response of MB and the specific ssDNA sequence could be detected in the concentration range from 1.0×10−14 to 1.0×10−8 mol/L with a low detection limit of 2.7×10−15 mol/L (3σ). The biosensor also showed good stability and discrimination ability to the one-base and three-base mismatched ssDNA sequence.
Key words：rod-like WO3; graphene (GR); composite film; terephthalaldehyde; DNA biosensor
稀土Ce掺杂ZnO微纳米材料的制备及应用研究
鲁雅，梁刚锋，吴林欣，方识耘，胡添添，袁建锋*
(浙江师范大学 行知学院，浙江 兰溪 314100)
摘要：随着现代化工业的发展，许多有毒或者无法直接进行生物降解的有机污染物产生，其对环境及人类健康造成严重的问题，因此，开发高效、经济、简单、快速的有机染料污染处理方法，一直深受各界关注。半导体光催化剂具有独特的性能，是处理有机污染物的有效材料之一。目前，半导体光催化材料普遍存在催化效率低、响应范围窄、回收再利用困难等问题。因此，以宽禁带光催化剂ZnO为研究主体，对其进行稀土元素Ce掺杂，旨在提升ZnO的催化性能，为开发高效光催化剂奠定基础。最终确定最佳掺杂量为2%，最佳pH为8，氙灯输出电流为21 A，催化剂用量以15 mg为宜，具有较好的稳定性，循环重复利用4次后，其催化活性基本不变。综上所述，该微纳米催化剂具有工业应用的前景。
关键词：稀土元素；ZnO；微纳米结构；光催化
中图分类号：TB383 文献标识码：A 文章编号：0258-3283（2019）
Preparation and Application of Ce Doped ZnO Micro/nano-materials LU Ya, LIANG Gang-feng, WU Lin-xin, FANG Shi-yun, HU Tian-tian, YUAN Jian-feng* (Xingzhi College, Zhejiang Normal University, Lanxi 314100, China), Huaxue Shiji, 2019, 41(3)
Abstract: With the development of modern industry, lots of organic pollutants that are toxic or cannot be directly bio-degraded cause the serious problems to environment and human health. Therefore, the development of efficient, economical, simple and rapid organic dye pollution treatment methods has been well payed attention. Photocatalysts have unique properties and are one of the effective materials for handling organic pollutants. At present, photocatalytic materials generally have problems of low catalytic efficiency, narrow light-response range, and difficulty in recycling. Therefore, in this work, the wide band gap photocatalyst ZnO is used as the research subject, and the element Ce doping is carried out to improve the catalytic performance of ZnO. Finally, the optimum Ce doping amount is 2%, the optimum pH is 8, the xenon lamp output current is 21A, the catalyst dosage is 15 mg, and the cycle can be reused 4 times, which has the prospect of industrial application.
Key words: rare-earth element; ZnO; micro/nano structure; photocatalysis
5α, 8α-过氧化甾腙衍生物的合成及抗肿瘤活性评价
卜明*1a，由丹2，张嵩1b，陈哲1c
(1.齐齐哈尔医学院 a.药学院，b. 基础医学院，c. 医药科学研究院，黑龙江 齐齐哈尔 161006；
2.齐齐哈尔第一医院，黑龙江 齐齐哈尔 161006)
摘要：以脱氢表雄酮为原料，经多步反应合成5个侧链具有不同吲哚结构的过氧化甾腙衍生物。所有合成化合物都通过MS、1HNMR和13CNMR进行结构表征。另外，分别选用人肝癌细胞（HepG2）、人乳腺癌细胞（MCF-7）和人正常肾上皮细胞（293T）对化合物的抗增殖活性进行评价，结果表明，3β-羟基-5α,8α-过氧化雄甾-6-烯-17-(5-氟-吲哚)腙和3β-羟基-5α,8α-过氧化雄甾-6-烯-17-(5-氯-吲哚)腙对所测试的肿瘤细胞株具有显著的抑制活性。
关键词：脱氢表雄酮；甾体；过氧化物；吲哚；抗肿瘤活性
中图分类号：O626 文献标识码：A 文章编号：0258-3283（2019）
Synthesis and Antitumor Activity of 5α, 8α-Peroxide Steroid Derivatives Containing Dihydrazone Unit BU Ming*1a，YOU Dan2，ZHANG Song1b, CHEN Zhe1c(1a. School of Pharmacy, 1b.Basic Medical Science College, 1c. Research Institute of Medicine & Pharmacy, Qiqihar Medical University, Qiqihar 161006, China; 2. The First Hospital of Qiqihar, Qiqihar 161006, China), Huaxue Shiji, 2019, 41(3)
Abstract：Using dehydroepiandrosterone (DHEA) as staring material, five steroidal endoperoxide detivatives with different indole-sidechain structures had been synthesized, and the structures were confirmed by MS, 1HNMR and 13CNMR. The antiproliferative activity was evaluated against human liver carcinoma cells (HepG2), human breast cervical cancer cells (MCF-7) and normal kidney epithelial cells (293T). The results showed that 5α, 8α-epidioxy-17-(5-fluoro-indol-3-ylmethylene)hydrazonoandrostan-3β-ol and 5α, 8α-epidioxy-17-(5-chloro-indol-3-ylmethylene)hydrazonoandrostan-3β-ol have significant inhibitory activity to the tested cancer cells.
Key words：dehydroepiandrosterone; sterol; endoperoxide; indole; antitumor activity
新型6-巯基嘌呤衍生物的合成及其生物活性研究
田静*，盛观星，包婷雯，张盼盼，卢永昌，林鹏程
（青海民族大学 药学院 青海省青藏高原植物化学重点实验室，青海 西宁 810000）
摘要：以6-氯嘌呤为原料，设计并合成了新型6-巯基嘌呤衍生物，通过IR、1HNMR 和HPLC-MS等方法对所合成化合物的结构进行了解析，并测试了其抗菌以及抗肿瘤活性。生物活性测试结果表明，目标化合物N'-(2-氨基乙基)马来酰亚胺基-6-甲巯基嘌呤-9-己酰胺具有较高的抗菌活性和抗肿瘤活性。抗菌活性测试结果显示，对所测试的10个菌种均有较好的抗菌活性。体外抗肿瘤细胞活性测试中，对6种肿瘤细胞株的IC50值在1.35 μmol/L和1.76 μmol/L之间，相比对照药物6-巯基嘌呤（IC50=1.97~4.53 μmol/L）表现出更好的抗肿瘤活性。
关键词：6-巯基嘌呤衍生物；合成；生物活性
中图分类号： 文献标识码：A 文章编号：0258-3283（2019）
Synthesis and Biological Activity of Novel 6- Mercaptopurine Derivative TIAN Jing*, SHENG Guan-xing, BAO Ting-wen, ZHANG Pan-pan, LU Yong-chang, LIN Peng-cheng (Key Laboratory for Tibet Plateau Phytochemistry of Qinghai Province, College of Pharmacy, Qinghai University for Nationalities, Xining 810007, China), Huaxue Shiji, 2019, 41(3)
Abstract: With 6-chloropurine as starting material, a novel 6- mercaptopurine derivative was synthesized. The structure of the compound was confirmed by IR, 1HNMR and HPLC-MS. The compound was screened based on antibacterial and anticancer activities. The results showed that the target compound exhibited high antibacterial activities against 10 strains. And it also exhibited high antitumor activities against 6 tumor cell lines with IC50 between 1.35 μmol/L and 1.76 μmol/L, 6- mercaptopurine (IC50=1.97~4.53 μmol/L) as control.
Key words: 6- mercaptopurine derivative; synthesis; biological activity
（R）-BINOL制备的手性磷酸在不对称Mannich反应中的应用
杨翠凤，徐泽刚，陈涛，李秉擘，宁斌科*
（西安近代化学研究所 氟氮化工资源高效开发与利用国家重点实验室，陕西 西安 710065）
摘要：手性磷酸是本世纪初发展起来的一种新型有机小分子催化剂，其拥有一个Brønsted acid酸性位点及Lewis base碱性位点，由于其酸性位点适宜的酸性，可向一些反应分子提供质子或与其形成氢键的弱相互作用，而碱性位点的磷氧双键可以提供孤对电子，因此手性磷酸具有双功能催化剂的优点，促使其在有机不对称反应中显示出独特的催化活性以及较高的对映选择性，特别在催化亚胺的反应中，更显示出特别高的催化效能。针对手性磷酸在不对称Mannich反应中的应用进展及其不对称催化作用机理进行评述，并对该类应用的未来发展方向做了一定的预测与展望。
关键词：Mannich反应；手性磷酸；对映选择性；Brønsted acid；亚胺
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283（2019）--
Applications of the （R）-BINOL Phosphoric Acid in Asymmetric Mannich Reactions YANG Cui-feng, XU Ze-gang, CHEN Tao, LI Bing-bo, NING Bin-ke* (State Key Laboratory of Fluorine & Nitrogen Chemicals, Xi’an Modern Chemistry Research Institute, Xi’an 710065, China), Huaxue Shiji, 2019, 41(3), ～
Abstract:Chiral phosphoric acid is a novel organic small molecule catalyst developed at the beginning of this century. It has a Brønsted acid acidic site and a Lewis base basic site. It can provide protons to some reactive molecules due to its acidic acidity. Or a weak interaction with hydrogen bonds, and the phosphorus-oxygen double bond at the basic site can provide a lone pair of electrons. Therefore, chiral phosphoric acid has the advantage of a bifunctional catalyst, which promotes its unique catalysis in organic asymmetric reactions. The activity and higher enantioselectivity, especially in the reaction of the catalytic imine, show a particularly high catalytic efficiency. The application progress of chiral phosphoric acid in asymmetric Mannich reaction and its asymmetric catalytic mechanism are reviewed, and the future development direction of this kind of application is predicted and forecasted.
Key words: Mannich Reactions; Chiral phosphoric acid; Enantioselectivity; Brønsted acid; imines
锌酞菁水溶性衍生物的合成与光动力学性能研究进展
卢小鸾1，鲍艺1，张潇潇1，彭黔荣*2，孙晓霞 1，杨敏*1
(1.贵州大学 药学院，贵州 贵阳 550025；2.贵州中烟工业有限责任公司技术中心，贵州 贵阳 550009)
摘要：锌酞菁（ZnPc）是高效的第二代光敏剂，在光动力疗法中对恶性肿瘤细胞具有显著的光生物活性和强烈的细胞毒性。然而，由于共轭分子间的π-π作用力，ZnPc溶解性差、结晶趋势强，阻碍了其临床研究。因此，改善ZnPc水溶性和分散性的研究一直在进行。对近五年ZnPc水溶性衍生物（离子型与非离子型）的合成与光动力学性能的相关研究进行综述。
关键词：锌酞菁；光敏剂；光动力疗法；溶解性；光动力学性能
中图分类号：O62 文献标识码：A 文章编号：2058-3283（2019）
Progress on Synthesis and Photodynamic Properties of Zinc Phthalocyanine Water-Soluble Derivatives LU Xiao-luan 1, BAO Yi1, ZHANG Xiao-xiao1, PENG Qian-rong*2, SUN Xiao-xia1, YANG Min *1 (1.School of Medicine, Guizhou University, Guiyang 550025, China; 2.Technology Center of China Tobacco Guizhou Industrial Co., Ltd., Guiyang 550009, China), Huaxue Shiji, 2019, 41(3)
Abstract: Zinc phthalocyanine is a highly efficient second-generation photosensitizer with significant photobioactivity and strong cytotoxicity against malignant cells in photodynamic therapy. However, due to the π-π interaction between conjugated molecules, ZnPc has poor solubility and strong crystallization tendency, which hinders its clinical research. Therefore, how to improve the water solubility and dispersibility of ZnPc have been investigated. This work aims to review the progress on the synthesis and photodynamic properties of ZnPc water-soluble derivatives (ionic and nonionic) in the past five years.
Key words: zinc phthalocyanine; photosensitizer;photodynamic therapy;solubility; photodynamic properties
地高辛在不同溶剂中的溶解度测定及关联
刘兰云1，孙永跃*1，李国兵2，全灿3
(1.天津理工大学 化学化工学院，天津 300384；2.天津大学 化工学院，天津 300072；3.中国计量科学研究院 化学计量与分析科学研究所，北京 100029)
摘要：在278.15 ～ 323.15 K下采用静态平衡法测定了地高辛在乙醇、甲醇、异丙醇、甲醇-水体系（甲醇体积分数为80%）及乙醇-水体系（乙醇体积分数为80%、60%、40%、20%）中的溶解度数据，采用Apelblat方程、多项式方程和λh方程对地高辛的溶解度进行关联。实验结果表明，8种溶剂中，地高辛的溶解度均随温度的升高而增加，在80%乙醇水混合溶剂中溶解度最大，在20%乙醇水中溶解度最小，几种热力学模型对地高辛的关联效果也很好。经热力学理论分析，计算溶解焓与溶解熵可知地高辛的溶解过程为吸热过程。地高辛溶解度的测定及关联为其工业化纯化溶剂的选择提供重要理论依据。
关键词：地高辛；溶解度；静态平衡法；关联
中图分类号：O645.12 文献标识码：A 文章编号：0258-3283(2019)--
Determination and Correlation of Solubility of Digoxin in Different Solvents LIU Lan-yun1, SUN Yong-yue*1, LI Guo-bing2, QUAN Can3 (1.School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384, China; 2.School of Chemical Engineering and technology, Tianjin University, Tianjin 300072, China; 3.Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: The solubility of digoxin in methanol, ethanol, isopropanol and binary system of ethanol-water solvent were measured by an equilibrium method at 278.15 ～ 323.15 K. The modified Apelblat equation, empirical equation and the λh equation were selected to correlate the experimental data. The results showed that the solubility of digoxin in eight organic solvents all increased with temperature increasing. Digoxin has the highest solubility in 80% ethanol and the lowest in 20% ethanol. The solubilities of calculated values were in good agreement with the experimental results. Based on the thermodynamic theory analysis, the dissolution process and the dissolution entropy were calculated to know that the dissolution process of digoxin is an exothermic process. The determination and correlation of the solubility of digoxin provides an important theoretical basis for the selection of industrial purification solvents.
Key words：Digoxin; solubility; static equilibrium method; coorelation
不同产地多花黄精的电化学指纹图谱研究
王元媛，李欢欢，雷林玉，程旺兴*
(安徽中医药大学 药学院 安徽中医药大学现代中药安徽省工程技术研究中心，安徽 合肥 230012)
摘要:通过Belousov-Zhabotinski（B-Z）振荡反应研究不同产地多花黄精的鉴别，将多花黄精粉末加入以丙二酸为耗散物的BrO3-+H++Ce4++ CH2(COOH)2振荡体系，用电化学工作站记录数据，并考查不同条件对B-Z振荡图谱的影响。确定本实验最佳实验条件为：温度310 K、转速500 r/min、多花黄精粉末加入量0.100 0 g。对不同产地多花黄精电化学指纹图谱进行研究，结果发现不同产地多花黄精的指纹图谱主要参数有较大差异。该方法简单、迅速，电化学指纹图谱特征性强、直观，可用于不同产地多花黄精的区分和鉴别。
关键词: 多花黄精；电化学指纹图谱；B-Z 振荡；鉴别
中图分类号：O 657.33；R 282.5 文献标识码：A 文章编号：0258-3283（2019）
Electrochemical Fingerprints of Polygonatum cyrtonema Hua from Different Origins WANG Yuan-yuan, LI Huan-huan, LEI Lin-yu, CHENG Wang-xing* (School of Pharmacy, Anhui Engineering Technology Research Center of Modern Chinese Medicine, Anhui University of Chinese Medicine, Anhui 230012, China), Huaxue Shiji, 2019, 41(3)
Abstract：The technique of Belousov-Zhabotinski (B-Z) oscillating reaction was used to add Polygonatum cyrtonema Hua powder into BrO3-+H++Ce4++CH2(COOH)2 oscillating system with malonic acid as dissipipative material. The electrochemical workstation was used to record the data. The influence of different conditions on the B-Z oscillation pattern was examined. The optimized experimental conditions are as fellows: temperature 310 K, speed 500 r/min, the amount of medicine added 0.100 0 g. The electrochemical fingerprints of Polygonatum cyrtonema Hua from different regions were obtained. The electrochemical fingerprints of Polygonatum cyrtonema Hua from different places showed significantly different characteristics. Electrochemical fingerprinting is simple, rapid, and intuitive, and it can be conveniently used for distinguishing Polygonatum cyrtonema Hua from different origins.
Key words: Polygonatum cyrtonema Hua; electrochemical fingerprinting; B-Z oscillation; identification
高效液相色谱法测定鲁米诺试剂稳定性研究
谭文渊*，周良芹，陈雨琴，付大友，王竹青
（四川理工学院 化学工程学院 四川 自贡 643000）
摘要:建立了鲁米诺试剂体系的高效液相色谱分析方法，并用该方法测试了鲁米诺体系中鲁米诺的稳定性。结果表明，实验条件下，鲁米诺的保留时间为4.3 min，出峰效果较好，标准溶液在0.1 ～ 4 mmol/L范围内呈现良好的线性关系，平均加标回收率为90.31 % ～ 99.05 %，相对标准偏差RSD≤2.93 %。在10周内鲁米诺试剂没有明显变化，色谱峰面积偏差为2.19 %，稳定性良好，该方法具有操作简便、结果准确、精密度良好的优点，可用于对鲁米诺试剂进行检测分析。
关键词: 高效液相色谱；鲁米诺；稳定性
中图分类号: O652.1 文献标识码: A 文章编号: 0258-3283(2019)—
Research on Stability Determination of Luminol by High Performance Liquid Chromatography TAN Wen-Yuan*, ZHOU Liang-Qin, CHEN Yu-Qin, FU Da-You, WANG Zhu-Qing (College of Chemical Engineering, Sichuan University of Science and Engineering, Zigong 643000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract： HPLC Method for the determination of luminol reagent system has been established, and the stability of luminol has been tested. The results showed that the retention time of luminol was 4.3 min. Strong linear relationship was observed from the calibration curve of luminol in the concentration of 0.1 ～ 4mmol/L, the average recovery was 90.31% ～ 99.05% with RSD≤2.93%. No significant change was observed within 10 weeks for luminol reagent. The chromatographic peak was stable, and peak area deviation of the luminol reagent was 2.19%. The established chromotography is convenient, accurate and suitable for application of detection and analysis of luminol reagent.
Key words: HPLC; luminol; stability
猪肉中磺胺类兽药残留基体标准物质高准确度定值方法
段嫚雷，李兰英*，李杰，闻艳丽，孟娇然，王乐乐，丁敏，刘刚
（上海市计量测试技术研究院，上海 201203）
摘要：建立了猪肉中磺胺类兽药残留基体标准物质高准确度定值方法，优化了提取溶剂、提取次数、添加内标试剂后的平衡时间和过滤膜的选择等样品前处理条件。猪肉样品中加入同位素标记物，乙腈提取3次，上清液过无水硫酸钠柱，提取物经50 ℃水浴旋转蒸发至干，正己烷饱和的流动相定容溶解，正己烷脱脂净化，然后正离子多反应监测测定，最后采用外标法定量。结果表明，磺胺嘧啶和磺胺二甲嘧啶在 10.0 ～ 200.0 ng/mL浓度范围内呈良好的线性关系，线性相关系数均大于0.999，方法的检出限和定量限分别为0.5、2.0 mg/kg，在低、中、高3个添加水平范围内的回收率为95.7% ～ 104.8%，相对标准偏差＜5%（n ＝ 6），可用于猪肉中磺胺类兽药残留基体标准物质均匀性检验、稳定性监测和定值。
关键词：磺胺；兽药残留；基体标准物质；高准确度
中图分类号：O65 文献标识码：A 文章编号：0258-3283（2019）--
High Accuracy Certifying Value Method of Matrix Reference Materials for Sulfonamides Residues in Pork DUAN Man-lei, LI Lan-ying*, LI Jie, WEN Yan-li, Meng Jiao-ran, WANG Le-le, DING Min, LIU Gang (Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China), Huaxue Shiji, 2019, 41(3)
Abstract：A highly accurate quantification method was established for the determination of sulfonamides residues in pork for a matrix reference material. Several key issues during the sample pretreatment were optimized including extraction solvent, times of sample extraction, equilibration time after the addition of internal standards, the selection of filter membrane. Internal standards were added into the sample, and then the sample was extracted 3 times by acetonitrile and centrifugation. The supernatant was then treated with a home-made separation column filled with anhydrous sodium sulfate. The extract was evaporated and dried by rotary evaporator at the temperature of 50 °C. The residue was dissolved by mobile phase saturated with n-hexane, and it was defatted and purified by n-hexane. The analysis was performed under the positive mode using multiple reaction monitoring (MRM) and quantified by external standard method. A good linearity was obtained in the range from 10.0 to 200.0 ng/mL for sulfadiazine and sulfadimidine, while the correlation coefficients were more than 0.999. The limits of detection (LODs) and the limits of quantitation (LOQs) were 0.5 mg/kg and 2.0 mg/kg respectively. The recovery rates at the three spiked levels were between 95.7%~104.8% with relative standard deviations (RSDs, n=6) less than 5%. The method was suitable for the homogeneity inspection, stability monitoring and certify value of the matrix reference materials for sulfonamides residues in pork.
Key words：sulfonamides; residues; matrix reference material; high accuracy
环境标准样品的选择与使用研究
宁远英，刘涛*，孙自杰
（环境保护部标准样品研究所 国家环境保护污染物计量和标准样品研究重点实验室，北京 100029）
摘要：环境监测数据是客观评价环境质量状况、反映污染治理成效、实施环境管理与决策的基本依据，我国高度重视环境监测数据质量。环境标准样品是确保环境监测数据质量的重要工具，广泛应用于我国环境监测活动中，为监测数据的一致性、可比性和准确性提供了重要的技术支撑。简要介绍了环境标准样品的定义、分类、特性及特性值，探讨了环境标准样品的选择，并根据环境标准样品的应用，对环境标准样品在待测环境样品赋值、测量方法/程序的确认、环境监测质量控制等方面的使用进行了综述，为环境监测机构正确选择和使用环境标准样品提出相关建议。
关键词：环境标准样品；环境监测；选择；使用
中图分类号： X-651 文献标识码：A 文章编号：0258-3283（2019）--
Study on Selection and Use of Environmental Reference Material NING Yuan-ying, LIU Tao, SUN Zi-jie (Reference Materials Institute of MEE, State Environmental Protection Key Laboratory of Environmental Pollutant Metrology and Reference Materials, Beijing 100029, China) Huaxue Shiji, 2019, 41(2), ～
Abstract: Environmental monitoring data is the basic basis for objectively evaluating environmental quality, which reflected the effectiveness of pollution control, and implemented environmental management and decision-making. China attaches great importance to the quality of environmental monitoring data. Environmental Reference Material is important tool to ensure the quality of environmental monitoring data, and widely used in environmental monitoring in China. It provides important technical support for the consistency, comparability and accuracy of monitoring data. The definition, classification, characteristics and characteristic values of Environmental Reference Material was introduced, and the selection of environmental standard samples was discussed. Based on the application of Environmental Reference Material, the use of Environmental Reference Material were studied, such as calibration of environmental monitoring instruments, assign values to the Environmental Reference Material, confirmation of measurement method/procedure, and quality control for environmental monitoring. And put forward some suggestions on selection and use of Environmental Reference Material by environmental monitoring agency.
Key words: Environmental Reference Material; Environmental monitoring; selection; use
3-芳胺基丁-2-烯酸酯和酰胺的无溶剂合成与表征
鲁赟1，崔亮2，孙志明3，雷珺宇2，义建军2，肖勇1，胥明亮1，庄俊鹏1，郝海军*1
（1. 北京化工大学 理学院，北京 100029；2. 中国石油天然气股份有限公司 石油化工研究院合成树脂重点实验室，北京102206；3. 中国石油天然气股份有限公司 抚顺石化分公司，辽宁 抚顺 113008）
摘要: -酮基丁酸酯和N-芳基取代的 -酮基丁酰胺通过双乙烯酮与ROH（R ＝ 烷基或芳基）或N-甲基苯胺的反应以及乙酰乙酸乙酯的芳胺解反应制备得到。两类化合物与2 ～ 3倍物质的量的芳香胺在无溶剂条件下于室温下以质子酸为催化剂反应，以中高收率得到一系列的目标化合物，并对它们进行了1HNMR、13CNMR、IR和ESI-MS的光谱表征。其中两个还通过X-射线单晶衍射测定了其分子结构。实现了此类化合物的无溶剂无金属催化条件下的简单合成。
关键词:无溶剂反应; 酸催化；-二羰基化合物；[N, O]配体；缩合反应；双乙烯酮
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283(2019)--
Synthesis and Characterization of Esters and Amides of 3-Arylaminobut-2-enoic Acid via Solvent-free Condensation LU Yun, CUI Liang2, SUN Zhi-ming3, LEI Jun-yu2, YI Jian-jun2, XIAO Yong1, XU Ming-liang1, ZHUANG Jun-peng1, HAO Hai-jun*1 (1. Beijing University of Chemical Technology, Beijing 100029, China; 2. Key Laboratory of Synthetic Resin, Petrochemical Research Institute, PetroChina Company Limited, Beijing 102206, China; 3. Fushun Petrochemical Company, PetroChina Company Limited, Fushun 113008, China), Huaxue Shiji, 2019, 41(3)
Abstract: Acetylacetic esters and N-aryl acetylacetamides were synthsized by the reaction of diketene with alcohols or N-methylaniline and by treatment of ethyl acetylacetate with arylamines, respectively. The title compounds were obtained in moderate to high yield by facial condensation of acetylacetic esters and N-aryl acethlacetamide with 2-3 folds of various arylamines catalyzed by concentrate HCl at room temperature and in solvent-free condition. The samples were readily purified by recrystallization or by column chromatolography, and were confirmed by 1HNMR, 13CNMR, IR and ESI-MS. The crystal structures of two compounds were determined by X-ray single crystal diffraction analysis. A simple synthesis method of such compounds under solvent-free and metal-free catalysis is achieved.
Key words: solvent-free reaction; β-dicarbonyl compounds; [N, O] ligand; acid catalytic; condensation; diketene
一个基于半刚性苯并三氮唑配体的Ag(Ⅰ)配合物的合成、晶体结构及荧光性质
张倩*，叶英杰，陈垒
（河南工程学院 材料与化学工程学院，河南 郑州 450007）
摘要: 合成并表征一个以苯并三氮唑为端基的半刚性配体——1, 4-二（苯并三氮唑-1-亚甲基）苯，将其与三氟乙酸银在溶液条件下组装得到了一个新的Ag(Ⅰ)配合物，通过元素分析、X-射线单晶衍射及X-射线粉末衍射对其结构进行了表征。结果表明，此配合物的中心原子Ag(Ⅰ)与两个配体苯并三氮唑端基3位上的N原子配位形成一维无限链，一维无限链之间通过苯并三氮唑基团的π…π堆积作用形成二维网络。并对这个Ag(Ⅰ)配合物固体荧光性质进行了测定。结果表明，配合物和配体显示相似的荧光光谱，可以归属为配体内的π-π*跃迁。
关键词：Ag(Ⅰ)配合物；苯并三氮唑配体；一维链状结构；荧光性质
中图分类号：O614.7 文献标识码：A 文章编号：0258-3283(2019)--
Synthesis, Crystal Structure and Luminescent Property of Ag(Ⅰ) Complex Based on Semi-rigid Benzotriazole Ligand ZHANG Qian*, YE Ying-jie, CHEN Lei (School of Materials and Chemical Engineering, Henan University of Engineering, Zhengzhou 450007,China), Huaxue Shiji, 2019, 41(3)
Abstract：A semi-rigid ligand with benzotriazole end group, 1,4-bis(benzotriazole-1-ylmethyl)benzene (L) was synthesized and confirmed, and a new Ag(Ⅰ) complex were obtained by the ligand reacting with AgCF3CO2 under solution condition. The complex structure was confirmed by elemental analysis, X-ray crystal diffraction and X-ray powder diffraction. The center Ag(Ⅰ) atoms were bridged by two 3-position N atoms from benzotriazole end group of ligands to generate 1D chain structure. Furthermore, the 1D Ag(Ⅰ) chains were linked to each other by π-π stacking interactions of benzotriazole rings to resulting in 2D network structure. In addition, luminescent property of Ag(Ⅰ) complex was also investigated.The result indicate that complex show similar photoluminescent spectra with the ligand, which can be assigned to the π-π* transition in ligand.
Key words: Ag(Ⅰ) complex; benzotriazole ligand; 1D chain structure; luminescent property
渗透性客体上汗潜手印与金属遗留印迹联合显现方法研究
邢卓1，杨敦舜1，周红2，杨瑞琴*1，刘文斌*3，刘先博1
（1.中国人民公安大学 刑事科学技术学院，北京 100038；2.公安部物证鉴定中心，北京 100038；3.上海市现场物证重点实验室，上海 200020）
摘要：通过考察茚二酮手印显现法与金属遗留印迹显现法之间的相互影响以及两种方法对纸张上汗潜手印与金属遗留印迹显现效果的影响，建立汗潜手印与金属遗留印迹的联合显现方法。实验结果表明，经茚二酮手印显现法与金属工具遗留印迹显现法显出的印迹在颜色和细节特征反映上均互不干扰，且先显现汗潜手印、后显现金属遗留印迹是复合印迹联合显现的最佳顺序。该联合显现方法的建立不仅弥补了渗透性客体上金属遗留印迹显现中手印反映不完整的缺点，而且还使手印中微量金属信息得以利用，从而为证明犯罪嫌疑人与金属工具之间关联性提供了更强有力的证据。
关键词：金属遗留印迹；汗潜手印；渗透性客体；联合显现方法
中图分类号：O641.4 文献标识码：A 文章编号：0258-3283(2019)
Integrated Detection of Latent Fingerprints and Imprints Left by Metallic Tools on Porous Substrates XING Zhuo1, YANG Dun-shun1, ZHOU Hong2, YANG Rui-qin*1, LIU Wen-bin*3, LIU Xian-bo1(1. School of Forensic Science, People’s Public Security University of China, Beijing 100038, China; 2. Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China; 3. Shanghai Key Laboratory of Crime Scene Evidence, Shanghai 200083, China), Huaxue Shiji, 2019, 41(3)
Abstract: A novel method of integrated detection of latent fingerprints and imprints left by metallic tools on porous substrates was established by investigating the mutual influence between the 1,2-indanedione latent fingerprint detection technique and the trace metal detection test (TMDT) and the effect of these two techniques on the quality of latent imprints and imprints left by metallic tools. The results show that fingerprints visualized by 1,2-indanedione and imprints visualized by the TMDT do not interfere with each other with respect to the colour and detailed features. In addition, the best sequence for the integrated detection method is using 1,2-indanedione latent fingerprint detection technique before the TMDT. This integrated method not only can overcome the limitation that incomplete fingerprints are often obtained using the TMDT, but also can exploit the clue in trace metal in fingerprints, which provides more powerful evidences for demonstrating the relationship between suspects and suspected metallic tools.
Key words: imprints left by metallic tools; latent fingerprints; porous substrates; integrated detection method
各金属客体对手掌面铁器遗留印迹显现的干扰研究
王丽婷*1，张春阳2
(1.宁夏大学 ，宁夏 银川 750021；2.宁夏省公安厅，宁夏 银川 750001)
摘要：应用2,4,6-三(2’-吡啶基)-1,3,5-三嗪试剂配方，并结合紫外分光光度法，在考察手掌面铜质、铝质、镍合金金属客体遗留印迹的显色效果的基础上，研究了各金属客体对手掌面铁器遗留印迹的显现干扰。结果发现，2,4,6-三(2’-吡啶基)-1,3,5-三嗪配方显现和手掌接触20 min的印迹时，铜质客体遗留印迹能够被轻微显现，铝质、镍合金金属客体遗留印迹则无法显出，铜会干扰铁质客体遗留印迹的显现，此干扰可使用2%（W/V）的硫脲消除。
关键词：2,4,6-三(2’-吡啶基)-1,3,5-三嗪；手掌；铁
中图分类号：D918 文献标识码：A 文章编号：0258-3283（2019）--
Study on Interference of Metal Objects to the Imprints Left by Iron on Palm WANG Li-ting*1, ZHANG Chun-yang2 (1.Ningxia University, Yinchuan 750021, China; 2.Public Security Department of Ningxia Province, Yinchuan 750001, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: With the reagent of 2, 4, 6-tri-(2’-pyridyl)-1, 3, 5-triazine, combined with ultraviolet spectrophotometry, the detection effect of imprint on palm surface left by copper, nickel and aluminum alloy, as well as their visible interference to the iron imprint on palm surface were investigated. The results showed that using 2, 4, 6-tri-(2’-pyridyl)-1, 3, 5-triazine to detect the hand imprint left by copper, aluminum, nickel alloy with contact time over 20 min, only imprint of copper could be detected. Besides, the copper could interfere with the detection of iron imprint on hands, however, 2% (w / v) thiourea can be used to eliminate.
Key words: 2, 4, 6-tri-(2’-pyridyl)-1, 3, 5-triazine; palm; iron
一种有机-无机杂化冠醚型超分子化合物的合成、晶体结构和介电性质
秦刘磊，刘洋*，郑晓媛，吕美霞，朱春立，刘尊奇*
（新疆农业大学 化学工程学院，新疆 乌鲁木齐 830052）
摘要：4-溴苯胺、18-冠醚-6、高碘酸以一定的配比反应，成功合成了一种新型的超分子化合物(4-BrC6H4NH3)+(18-crown-6)(IO4)-，并通过X-射线单晶衍射、红外光谱（IR）、XRD、热重分析(TG)、变温介电测试等对其进行表征。单晶结构解析表明：低温（128 K）和室温（296 K）时，化合物空间群为Pnma，均为正交晶系。4-溴苯胺分子中的溴原子与相邻的-NH3+基团形成N-H…Br氢键，穿过18-crown-6分子的空腔，在b轴方向形成一维氢键链状结构。在100 ～ 310 K，500 Hz ～ 1 MHz范围内对晶体的介电性能进行测试，在223 K附近出现明显的介电响应。
关键词：有机-无机杂化；冠醚；晶体结构；介电性质
中图分类号：O646 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis, Crystal structure and Dielectric Properties of a Novel Organic-Inorganic Hybrid Supramolecular Compound based on Crown Ethers QIN Liu-lei, LIU Yang*, ZHENG Xiao-yuan, LV Mei-Xia, ZHU Chun-li, LIU Zun-qi* (Chemical Engineering College, Xinjiang Agricultural University, Urumqi 830052, China) Huaxue Shiji, 2019, 41(2), ～
Abstract：One new supramolecular complex (4-BrC6H4NH3)+(18-crown-6)(IO4)- has been successfully obtained by the reaction of 4-bromoaniline, 18-crown-6 and HIO4. The complex was characterized by X-ray single-crystal diffraction, IR, powder XRD, thermogravimetric analysis and variable-temperature dielectric measurement. X-ray single-crystal analysis reveals that complex belongs to orthorhombic system, space group Pnma at low temperature and room temperature. N-H…Br hydrogen bonds exist between the bromine atom and -NH3+ group in the adjacent 4-bromoaniline interaction through 18-crown-6. This formed one dimensional hydrogen-bond chain structure. The temperature dependence of dielectric measurement was taken from 100 ～ 310 K at 500 Hz ～ 1 M Hz. The results show distinct dielectric responses at ca. 223 K.
Key words：organic-inorganic hybrid; crown ether; crystal structure; dielectric properties
氢化松香GMA酯化物的合成与表征
许建本a, b，何春玲c，罗佩莉a，农克良*a, b
(广西民族师范学院 a.化学化工学院；b.广西高校桂西南特色植物资源化学重点实验室培育基地；c.文学与传媒学院，广西 崇左532200)
摘要：以氢化松香（HR）和甲基丙烯酸缩水甘油酯（GMA）为原料，三乙胺为催化剂，对苯二酚为阻聚剂，通过溶剂法合成了氢化松香GMA酯化物（HG），采用单因素和正交实验对酯化反应条件进行优化。探讨了单体配比（n（HR）：n（GMA））、催化剂用量、反应温度和时间对酯化物酸值和酯化率的影响。利用红外光谱对HG进行结构表征，热重分析对HG进行热稳定性测试。结果表明，成功合成了HG，且HG热稳定性较好，较佳工艺条件为n（HR）：n（GMA） ＝ 1：1.2，催化剂三乙胺用量为氢化松香的0.5 wt%，110℃反应4 h，HG酯化率达到95.8%。在引发剂、交联剂和分散剂存在条件下，HG可与苯乙烯反应生成聚合物微球，得到的微球球形较好，且带有羟基基团。
关键词：氢化松香；甲基丙烯酸缩水甘油酯；酯化物；微球
中图分类号：TQ35 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis and Characterization of Ester of Hydrogenated Rosin and GMA XU Jian-bena, b, HE Chun-lingc, LUO Pei-lia, NONG Ke-liang*a,b (a.College of Chemistry and Chemical Engineering; b.Guangxi Colleges and Universities Key Laboratory Breeding Base of Chemistry of Guangxi Southwest Plant Resources; c.College of Literature and Media, Guangxi Normal University for Nationalities, Chongzuo 532200, China), Huaxue Shiji, 2019, 41(3)
Abstract: By using hydrogenated rosin and glycidyl methacrylate as raw materials, triethylamine as catalyst, and hydroquinone as polymerization inhibitor, a hydrogenated rosin derived GMA ester (HG) was prepared by solvent method. Single-factor test and orthogonal experiment were used to determine the effects of monomer ratio, catalyst dosage, reaction temperature, and reaction time on the acidic value and esterification rate and to optimize the reaction process. The structure and thermal stability of HG was characterized by FT-IR and Thermal Gravimetric analysis (TGA), respectively. HG with good thermal stability was successfully prepared. The optimum conditions for the reaction were as following: molar ratio of HR and GMA of 1:1.2, triethylamine mass of 0.5% (based on HR weight), reaction temperature of 120 ℃, and reaction time of 4 h. Under these conditions, the esterification rate of the HG was up to 95.8%. Furthermore, polymer microspheres with a good spherical shape and contain hydroxyl groups were prepared with HG and styrene under the conditions of initiator, crosslinking agent and dispersing agent.
Key words: hydrogenated rosin; glycidyl methacrylate; ester; microspheres
高效除草剂环酯草醚的合成工艺优化
周裕林，李鑫，岳家委，徐德锋*
（常州大学 制药与生命科学学院，江苏 常州 213164）
摘要：环酯草醚是高效水稻苗后广谱除草剂，为解决生产过程中环境污染问题，以硫代乙酸钾为硫代试剂，本文以2-乙酰基-6-硝基苯甲酸为原料，经硼氢化钠还原、硫代、还原和亲核取代合成目标化合物。考察了各步反应溶剂、反应温度、反应时间和原料配比等因素对反应收率的影响，并通过合成工艺优化和正交试验得到目标化合物最佳合成工艺条件。反应总收率达71.3%，产品纯度为99.1%，其结构经1HNMR、13CNMR、熔点和HR-MS(ESI)确证。该工艺路线安全、简便、适合于工业化生产。
关键词：环酯草醚；2-乙酰基-6-硝基苯甲酸；3-甲基-7-硝基苯酞；3-甲基7-巯基苯酞；工艺优化
中图分类号：TQ457.2 文献标识码：A 文章编号：0258-3283(2019) --
Synthetic Process Optimization of High-efficiency Herbicide Pyriftalid ZHOU Yu-lin, LI Xin, YUE Jia-wei, XU De-feng* (School of Parmaceutical Engineering & Life Science, Changzhou University, Changzhou 213164, China) Huaxue Shiji, 2019, 41(2), ～
Abstract: Pyriftalidisa is high-efficiency rice seedling broad-spectrum herbicide. Potassium thioacetate was used as a thio reagent to solve the environmental pollution in the production process. Using 2-acetyl-6-nitrobenzoic acid as a raw material, pyriftalid was obtained via the successive reaction of borohydride reduction, thio reaction, borohydride reduction, nucleophilic substitution. The effect of yield for each step was investigated such as the reaction solvent, reaction temperature, reaction time and the ratio of raw materials and other factors. Synthetic process optimization and orthogonal experiments were used to screen the optimal synthesis conditions of pyriftalid. The total reaction yield and the product purity were 71.3% and 99.1% respectively.The structure of pyriftalid was confirmed by 1HNMR, 13CNMR, melting point and MS. The new technology is safe, simple and suitable for industrial production.
Key words: Pyriftalid; 2-acetyl-6-nitrobenzoic acid; 3-methyl-7-nitrophalide; 3-methyl-7-mercaptophalid; optimal reaction
N-苯磺酰咔啉的合成
胡珊珊，付玉轩，李佳佳，李小娟*
(新疆师范大学 化学化工学院，新疆 乌鲁木齐 830000)
摘要：描述了碱性条件下咔啉类化合物的苯磺酰胺化反应。在NaH作用下，具有两亲结构的β-或γ-咔啉与N-氟代双苯磺酰胺反应生成不同种类的目标化合物，实现咔啉苯磺酰胺的简便合成，收率良好。机理研究表明，在反应中间体咔啉氮负离子的影响下，N-氟代双苯磺酰胺的N―S键断裂提供苯磺酰基，这是商品化试剂N-氟代双苯磺酰胺作为亲电氟化、自由基氟化和胺化试剂之后新的应用。
关键词：β-咔啉；γ-咔啉；N-氟代双苯磺酰胺；N-苯磺酰咔啉
中图分类号： 文献标识码： 文章编号：0258-3283(2019)--
Synthesis of Carboline Sulfonamide HU Shan-shan, FU Yu-xuan, LI Jia-jia, LI Xiao-juan* (College of Chemistry and Chemical Engineering, Xinjiang Normal University, Urumqi 830000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: A convenient synthesis of carboline sulfonamide was achieved via sulfonamidation under alkaline conditions. The reactions between β- or γ-carbolines and N-fluorobenzenesulfonamide were investigated in the presence of NaH. With N-fluorobenzenesulfonamide as sulfonylation reagent, β- and γ-carboline benzene sulfonamide derivatives were obtained in good yields. These reactions provide a new pathway for carboline sulfonamide derivatives.
Key words: β-carboline; γ-carboline; N-fluorobenzenesulfonamide; carboline sulfonamide
离子膜电解法制备高锰酸钾
李勇，赖俐超，张丰如，唐春保*，刘燕，冯发达
（嘉应学院 化学与环境学院，广东 梅州 514015）
摘要：以锰酸钾为原料，采用离子膜电解槽制备高锰酸钾。研究了锰酸钾浓度、电解电流、温度、时间和电解槽内填充材料对电解效果的影响，确定了膜法电解制备高锰酸钾的工艺条件。结果表明，恒定电流下电解，随着电解时间的延长，转化率在增大，但电流效率在下降；阶梯电流下电解，整个电解过程，电流效率维持在70%以上。在多于5倍电解槽容积的电解液、79.63 g/L锰酸钾、65 ～ 68 ℃、4级阶梯电流条件下电解120 min，锰酸钾转化率为78.73%，电流效率为71.85%，电流效率较传统工艺大幅提高。
关键词：高锰酸钾；离子膜电解法；阶梯电流；电流效率；制备
中图分类号：TF803.27 文献标识码：A 文章编号：0258-3283（2019）--
Preparation of Potassium Permanganate by Ion-exchange Membrane Electrolysis LI Yong, LAI Li-chao, ZHANG Feng-ru, TANG Chun-bao*, LIU Yan, FENG Fa-da (School of Chemistry and Environment, Jiaying University, Meizhou 514015, China), Huaxue Shiji, 2019, 41(3), ～
Abstract: Potassium manganate as raw material, potassium permanganate was prepared using ion-exchange membrane electrolyzer . The effects of potassium manganate concentration, electrolytic current, temperature, time and filling material on the electrolysis efficiency were investigated. The preparation conditions of potassium permanganate were determined. The results showed that，Electrolysis at constant current, with the increase of electrolysis time, the conversion rate is increasing, but the current efficiency is decreasing. Electrolysis under step current, the current efficiency is maintained above 70% during the entire electrolysis process. On the conditions of 5 times the electrolyte volume of the electrolytic cell， the concentration of 79.63g/L K2MnO4，65~68℃, four step current and electrolysis time of 120min，the conversion rate of potassium manganate was 78.73% and the current efficiency was 71.85%. Compared with the traditional methods, the current efficiency was greatly improved.
Key words： potassium permanganate； ion-exchange membrane electrolysis；step current；current efficiency；preparation
几种新型二噁英半抗原的合成
杨夕强*，苏鹏辰，王冠蕾，曹克广
（承德石油高等专科学校 化学工程系，承德 河北 067000）
摘要：酶联免疫分析（ELISA）技术具有灵敏度高、操作简单以及耗时少等特点，应用于二噁英类化合物的检测，可以解决目前通用的色谱/质谱联用法检测费用高、样品前处理繁琐、检测周期长等问题。相关研究表明，ELISA技术的关键是设计与目标分子在大小、形状（立体结构）和电子性能上尽量相似的半抗原分子。因此，设计并合成包含二苯并-对-二噁英类结构的二噁英半抗原是提高其灵敏度和准确性的关键。基于“二噁英半抗原中间体的合成研究”，继续完成了二噁英成环关键步骤的反应条件探索，经水解最终得到4个未见报道的二噁英半抗原，并对5个重要中间体、4个最终产物进行了核磁验证。
关键词: 酶联免疫分析；二噁英；半抗原
中图分类号：O626 文献标识码：A 文章编号：0258-3283(2019)--
Synthesis of Several New Dioxin Haptens YANG Xi-qiang*, SU Peng-chen, WANG Guan-lei, CAO Ke-guang (Department of Chemical Engineering, Chengde Petroleum College, Chengde 067000, China), Huaxue Shiji, 2019, 41(2), ～
Abstract: Due to high sensitivity, simple operation and less time consuming, enzyme-linked immunoassay (ELISA) technique can be applied to the detection of dioxin compounds, which can overcome the disadvantages, such as the hightest cost, tedious pretreatment and long detection cycle of chromatography/mass spectrometry. The key of ELISA technology is to design the hapten molecules that are as similar as the target molecules in size, shape (stereoscopic structure) and electronic properties. Therefore, designing and synthesizing dioxin hapten containing two benzo - dioxins is the key to improve its sensitivity and accuracy of ELISA. The optimum reaction conditions of the cyclization reaction of dioxin were explored and then four unreported dioxin haptens were obtained by hydrolysis, and five important intermediates. The four final products were confirmed by NMR.
Key words: enzyme-linked immunoassay (ELISA); dioxin; hapten
