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《锻压技术》2013年（第38卷）第1期 目次
（全国中文核心期刊）
-------------------------------
特别提示：作为参考文献引用时举例：
[1] 童敏杰，王长文，雷d，等. 电沉积法制备的超细晶薄铜板拉伸及表面层效应[J]. 锻压技术, ): 16-19.
-----------------------------------------
《锻压技术》2013年（第38卷）第2期 目次
（全国中文核心期刊）
基于伺服压力机的板料成形研究现状与发展趋势
夏敏，向华，庄新村，等(1-5)
矩形直齿轮热锻工艺有限元模拟
只悦胜， 胡成亮 ， 赵震 ，等(6-9)
前轴垂直整形工艺模拟与模具开发
曾琦，蒋鹏(10-13)
13B型货车钩尾框框体锻造工艺模拟及优化王凯，王皓，唐振英，等(14-16)
396柴油机连杆模锻成形工艺研究李志广，安文忠，刘振杰(17-20)
深腔类盒形件充液成形技术研究郎利辉，许
诺，王永铭，等(21-25)
汽车B柱加强板拉延筋优化设计朱取才，王成勇 ，田植诚，等(26-30)
半圆筋循环载荷作用下的板材变形特征研究李群，李娜，郭宝峰，等(31-33)
板料渐进成形极限图测试方法研究王进，姜虎森，陶龙，等(34-36)
基于拉伸试验的板料成形性能研究丁华，薛松，张东，等(37-39)
小口径厚壁球形封头的冷拉深成形蒋起臣，王永生，杨一平，等(40-42)
带凸缘锥形零件拉延成形工艺研究韩来福， 杨智刚， 尚志全，等(43-46)
碳纤维连接结构钛合金铆钉电磁铆接试验研究 崔俊佳，孙立强，孟令博，等(47-52)
SUSXM7含铜不锈钢冲压成形性能研究张艳梅，程永奇，黎文灿，等(53-56)大比例三通接头成形工艺研究及质量控制王玲，付冬雪，郎利辉，等(57-60)
正在加载中，请稍后...中国分析测试协会
《化学试剂》2016年4月第38卷第4期中英文摘要
文章来源：《化学试剂》编辑部
纳米粒子在肿瘤成像/治疗中的研究进展
谭桂珍，徐勤飞，王兵毅，郝志峰*
（广东工业大学 轻工化工学院，广东 广州& 510006）
摘要：纳米粒子（20 ～ 400 nm）颗粒小，可通过血管的渗透增强和滞留效果而积累在肿瘤细胞中，避免被肾脏所清除，从而使其在血管中有更长的血液循环时间；纳米粒子比表面积大，可以携带大量的化疗药物用于药物的传递；纳米粒子表面经过改造后可以结合不同的靶向基团，并利用共价键结合到细胞表面受体，从而可将药物运输到特定的部位。近年来，越来越多的科研工作者致力于研究纳米颗粒与一些生物分子之间的关系，以此来开发更有效和特异性的抗癌药物。引用了近10年的参考文献，主要介绍了纳米粒子在肿瘤成像及治疗中的应用。
关键词：纳米粒子；表面改造；肿瘤成像和治疗
中图分类号：O6&&&&&&& 文献标识码：A&&&&&&& 文章编号：（2016）
Progress of Nano-particles in Tumor Image and Treatment
TAN Gui-zhen, XU Qin-fei, WANG
Bing-yi, HAO Zhi-feng* (School of Chemical Engineering and Light Industry, Guangdong University of Technology, Guangzhou 510006, China), Huaxue Shiji, )
Abstract: The size of nano-particles (20 ～ 400 nm) makes it can accumulate in the tumors by the effect of enhancing permeability and retention effect. It can avoid renal filtration and has a long blood circulation times. In the same time, the surface of nano-particles is big enough for drug delivery, it can conjugate to different chains after surface modification and conjugate to the surface of tumor by the receptors. Thus, it can transfer the drug to the especial position. In recent years, more and more scientists devote to research the relation between nano-particles and biomaterials in order to develop more efficient and specificity anti-cancer drug. In this work, an overview of the use of nano-particles in tumors diagnose and treatment is provided.
Key words: nano- surfa tumors image and treatment.
&-环糊精基氧化钨毛细管电色谱整体柱的制备及应用
李英杰，张馨予，高立娣*，吕仁江，董艳丽，陈男
（齐齐哈尔大学 化学与化学工程学院，黑龙江 齐齐哈尔& 161006）
摘要：采用一步键合法合成了&-环糊精基氧化钨毛细管电色谱整体柱，考察了制备整体柱的主要影响因素，获得最佳制柱条件为：功能单体双（6-O-丁烯二酸单酯）-&-环糊精（CPD-&-CD）与EDMA物质的量比为0.12 : 0.08，修饰纳米氧化钨的质量0.30 g，水浴温度40 ℃，聚合时间13 h。同时对整体柱进行了表征和评价，制备的整体柱有较均匀孔径的网状结构，固定相中修饰纳米氧化钨的含量达到16.6%，整体柱有良好的重现性和稳定性，同时具备较好的手性拆分能力。在最佳电色谱条件下，应用整体柱对美托洛尔、阿替洛尔和索他洛尔对映体进行拆分，均达到基线分离。
关键词：&-环糊精衍生物；纳米氧化钨；电色谱整体柱；洛尔类药物；手性拆分
中图分类号：&&&&&&&&&&& 文献标识码：A&&&&&&&&& 文章编号：（2016）
Preparation and Application of Electrochromatographic Column Based on &-cyclodextrin Derivatives and Tungsten Oxide
&LI Ying-jie, ZHANG Xin-yu, GAO Li-di*, LV Ren-jiang, DONG Yan-li, CHEN Nan (College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China), Huaxue Shiji, )
Abstract： In this work, the electrochromatography monolithic&column of &-cyclodextrin derivatives and tungsten oxide was prepared by one-step reaction, at the same time, the main influencing factors of prepared column were investigated. The optimum conditions of prepared column were listed as follows: the molar ratio of CPD-&-CD and EDMA is 0.12 : 0.08, the modified nanometer tungsten oxide of 0.30 g, and the reaction time of 13 h at 40 ℃ water bath. Characterization and evaluation of the monolithic column were also carried out. The results show that the obtained monolithic column has a mesh structure with uniform pore size, and the content of tungsten oxide in stationary phase was about 16.6%. The monolithic column has good reproducibility and stability，and the better ability of chiral separation. Under the optimum electrochromatographic conditions, the baseline separation of chiral drugs including metoprolol, atenolol and sotalol were obtained by the prepared monolithic column．
Key words: &-cyclodextrin derivatives；nanometer tungsten oxide；electrochromatography monolithic&column；Lol 药物drug；chiral separation
meso-5-对甲氧基苯基-10, 15, 20-三（对氯苯基）卟啉的合成及理论研究
韩久利1，佘远斌*1, 2
（1. 北京工业大学 绿色催化与分离北京市重点实验室，北京& . 浙江工业大学 化学工程学院，浙江 杭州& 310014）
摘要：在19种溶剂体系下合成了A3B型不对称卟啉化合物meso-5-对甲氧基苯基-10, 15, 20-三（对氯苯基）卟啉，并用密度泛函理论对其进行了结构优化，得到了稳定结构。研究发现溶剂粘度、极性等性质对产物的收率具有重要影响，其中在N, N-二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)等体系下无法得到产物，因其作为Lewis碱削弱了体系的酸性，阻碍反应的进行。在乙酸为溶剂的体系下，目标产物在总的卟啉化合物中的分布最高28.8%。在丙酸与乙酸混合溶剂体系下，卟啉的总收率最高达32.4%，目标产物收率也达到最高6.6%。
关键词：A3B型卟啉；溶剂性质；结构表征
中图分类号： O621.3&&&&&&&&&文献标识码：A&&&&&&&&文章编号：（2016）
Synthesis and Theoretical Investigation of 5, 10, 15-tri(p-chlorophenyl)-20-(p-methoxy)phenyl Porphyrin
HAN Jiu-li1, SHE Yuan-bin*1, 2 （1. Beijing Key Laboratory for Green Catalysis and Separation, Beijing University of Technology, Beijing 100124, C 2. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China）, Huaxue Shiji, 2016, 38(4)
Abstract: 5, 10, 15-Tri(p-chlorophenyl)-20-(p-methoxy)phenyl porphyrin was synthesized in 19 kinds of solvents and its structure was optimized by density functional theory (DFT) to obtain the stable structure. The research found that the characters of solvents have great effect on this reaction and the distribution of individual porphyrin products. As Lewis base, N, N-dimethyl formamide, dimethyl sulfoxide and so on can not obtain porphyrins. In the system of acetic acid, 5, 10, 15-tri(p-chlorophenyl)-20-(p-methoxy)phenyl porphyrin have the maximum distribution (28.8%) in the total porphyrins. In the mixture of acetic and proponic acid, the overall yield of porphyrins and the yield of the target porphyin arrived up to 32.4% and 6.6%, respectively.
Key words：A3B- structure characterization
稳定同位素15N标记2-甲基-5-硝基咪唑的合成与表征
王伟，徐建飞，杜晓宁，王雪婷，宋明鸣，雷雯，侯捷
(上海化工研究院 上海稳定性同位素工程技术研究中心，上海& 200062)
摘要：以15NH3和H15NO3作为同位素原料，经两步反应得到目标产物15N标记2-甲基-5-硝基咪唑。收率以15NH3计，为58%，经液相色谱（HPLC）、质谱（MS）、气体同位素质谱计（MAT-271）等对其纯度和丰度进行表征，纯度＞99.5%，丰度＞99%，可作为制备15N标记硝基咪唑类药物内标检测试剂的合成前体。
关键词：内标试剂；2-甲基-5-硝基咪唑；硝基咪唑；稳定同位素标记
中图分类号：O628.2&&&&&&&&&文献标识码：A&&&&&&&&&&文章编号： （2016）&&&&&& &
Synthesis and Characterization of Stable Isotope 15N Labeled 2-Methyl-5-nitroimidazole
WANG Wei, XU Jian-fei, DU Xiao-ning, WANG Xue-ting, SONG Ming-ming, LEI Wen, HOU Jie (Shanghai Engineering Research Center of Stable Isotope，Shanghai Research Institute of Chemical Industry，Shanghai 200062，China), Huaxue Shiji, 2016, 38(4)
Abstract: An efficient synthesis was established to prepare the stable isotope 15N labeled 2-methyl-5-nitroimidazole with 15NH3 and H15NO3 as the raw material. The total yield was 58% based on 15NH3 consumed. The target compound was confirmed by HPLC，MS and MAT-271. The chemical purity is 99.5% and deuterium isotopic enrichment is 99.0 atom%15N. The compound could be used as the synthetic precursor for prepare 15N labeled nitroimidazole.
Key words: isot 2-methyl-5- stable isotope labeling
基于灰色关联法高温堵剂性能评价
曲占庆1，刘晓强*1，齐宁1，雷锡岳1，苏程2，常琨2
（1. 中国石油大学（华东） 石油工程学院，山东 青岛& 266580；
2. 中国石化华北油气分公司采油一厂，甘肃 庆阳& 745000）
摘要：研发出了新型耐高温调剖堵水试剂磺化改性落叶松栲胶，其典型配方为：6.0 wt%磺化改性落叶松栲胶、2.5 wt%~ 3.0 wt%醛类交联剂、1.0 wt% ~ 1.5 wt%酚类促进剂P-1，其他为水，用氢氧化钠将pH调节至8 ~ 10。通过实验对改性落叶松栲胶性能进行测试。试验表明，堵剂胶凝时间4 ~ 10 h可控，满足pH在4 ~ 10的范围内使用，能用于100000 mg/L的较高矿化度地层，所成凝胶强度高。采用灰色关联法对温度、矿化度、组分浓度、pH等影响因素进行分析，各因素对磺化改性落叶松栲胶成胶时间和成胶强度的影响程度从大到小依次为温度、pH、栲胶浓度、矿化度。
关键词：改性栲胶；高温调剖堵水剂；室内试验；灰色关联分析
中图分类号：TE357.1&&&& 文献标识码：A&&&&&&&&文章编号：（2015）
Analysis of Influence Factors of High Temperature Plugging Agent Based on Gray Correlation Theory
QU Zhan-qing1, LIU Xiao-qiang1, QI Ning1, LEI Xi-yue1, SU Cheng2, CHANG Kun2 (1.College of Petroleum Engineering, China University of Petroleum, Qingdao 266580, C 2. First Gas Production Factory, Huabei Oilfield Branch, Sinopec, Qingyang 745000, China), Huaxue Shiji, 2016, 38(4)
Abstract: A new profile modifying and water shutoff agent is developed for western high temperature, low permeable oil reservoir. Its basis recipe is composed of 6.0% modified larch tannin extract, 2.5% ~ 3.0% formaldehyde, 1.0% ~ 1.5% phenolic crosslinking promoter P-1 in water solution with pH value of 8 ~ 10. Properties of the modified tannin extract are tested by laboratory experiment. Based on the testing results, the agent is of a controllable profile of colloiding time of 4 ~ 10 h. It can be used at the pH range of 4 ~ 10, standing as high as 100000 mg/L salinity with a high strength. Gray correlation theory is taken to analysis influence factors such as temperature, pH value, degree of mineralization and component concentration. Based on the calculation result, the gel time and the gel strength are affected by the following factors in a descending order: temperature, pH value, concentration of modified larch tannin extract and degree of mineralization.
Key words: modified
high te laboratory experimentation, gray correlation analysis
稳定同位素标记硼氘化钠的合成
谭树波，杨维成，罗勇*
（上海化工研究院 上海稳定同位素工程技术研究中心，上海 200062）
摘要：通过对硼氢化钠的合成方法研究，确定了同位素标记硼氘化钠的制备方法：以硼砂、金属钠、氘气为原料，搅拌条件下将反应釜升温至450 ℃，反应0.5 h，得含硼氘化钠产品的粗砂，采用索氏提取法处理粗砂，得目标产物硼氘化钠产品，产品纯度99.2 %，同位素丰度99.9atom% D。
关键词：硼砂；硼氘化钠；同位素标记；合成
中图分类号：O611&&&&&& 文献标识码：A&&&& 文章编号：（2016）
Synthesis of Isotope-labeled Sodium Borohydride-D4
TAN Shu-bo, YANG Wei-cheng, LUO Yong* (Shanghai Research Institute of Chemical Industry, Shanghai Engineering Research Center of Stable Isotope, Shanghai 200062, China) , Huaxue Shiji, 2016, 38(4)
Abstract: The synthesis procedure of isotope-labeledsodium borohydride-D4 was investigated via changing different parameters and established finally. The reaction system which had been added sodium tetraborate, sodium and deuterium gas was firstly heated up to 450 ℃ with stirring and kept for 0.5 h. The raw product was then extracted with soxhlet extractor, the purity of the target product was 93.7%, and D abundance of sodium borohydride-D4 was 99.9 atom% D.
Key Words:
sodium borohydride-D4; isotope- synthesis
微波辐射下离子化合物的合成及在Hantzsch反应中的应用
裴学海，黄克俊，陈林艳，陈治明*
（贵州师范大学 化学与材料科学学院 贵州省功能材料化学重点实验室，贵州& 贵阳&& 550001）
摘要：采用微波合成法得到四种离子化合物，反应在3 ~ 6 min内结束，并将四种离子化合物应用于催化Hantzsch二氢吡啶及Dilantin的合成，其中[n-C4H9Dmap]Br催化 Hantzsch二氢吡啶，得到87%的较高收率。离子化合物可反复使用7次，且催化活性并未降低。反应具有操作简单、条件温和、产率高等特点。
关键词: 微波合成；Hantzsch；Dilantin；离子化合物
中图分类号：O626 &&&&&&&文献标识码：A&&&&&&文章编号：（2016）
Synthesis of Ion Compounds under Microwave Irradiation and Application in the Hantzsch Reaction
PEI Xue-hai, HUANG Ke-jun, CHEN Lin-yan, CHEN Zhi-ming* (Key Laboratory of Functional Materials Chemistry of Guizhou Province, School of Chemistry and Materials Science, Guizhou Normal University, Guiyang 550001,China), Huaxue Shiji, 2016, 38(4)
Abstract：Four kinds of ionic compounds were obtained by microwave synthesis, the reaction was end in 3 to 6 minutes. And the four kinds of ionic compounds were applied to the synthesis of Hantzsch and Dilantin via catalyzed by [C4H9Dmap]Br and can be reused 7 times. The yield reached 87%. The catalytic activity is not reduced and the characteristics of simple operation, mild conditions, high production.
Key word: H D ionic compound
基于炔肟成环的5-取代异噁唑-3-羧酸酯类化合物的合成
靳清贤*1，张永霞2，田君梅1，李争光1，余洛洛 1，孙伟1
(1.郑州轻工业学院 材料与化学工程学院 河南省表界面科学重点实验室，河南 郑州& 450001；
2. 河南交通职业技术学院 公共基础教学部，河南 郑州& 450005)
摘要：异噁唑结构普遍存在于药物结构中，同时也在许多天然活性产物结构中存在，而5-取代异噁唑-3-羧酸酯类化合物是异噁唑化合物中研究较为广泛的一类。总结了炔肟成环制备5-取代异噁唑-3-羧酸酯类的合成方法和研究进展，详细归纳和报道各代表性例子，并对其加以对比分析。
关键词：炔肟；异噁唑；合成
中图分类号：O626&&&&&&&&文献标识码：A & & & &&文章编号: （2016）
Key Words: Alkyne- synthesis
毛细管电泳在线富集技术在黄酮类化合物分析中的应用
&&&&&&&&&&&&&&&&& 赵有轩1, 2, 3，王敦青3，李新民3，姚庆强2，吕元琦*3
（1. 济南大学-山东省医学科学院 医学与生命科学学院，山东 济南　. 山东省医学科学院药物研究所，山东 济南　250062； 3. 德州学院分析测试中心，山东 德州　253023）
摘要：介绍了毛细管电泳在线分析技术的原理，对该技术在黄酮类化合物分析中的应用进行了综述，对该技术的发展趋势进行了展望。
关键词：毛细管电泳；在线富集；黄酮类化合物
中图分类号：O625.34&&&&&&&&&文献标识码：A&&&& 文章编号：（2016）
Application of Capillary Electrophoretic on-line Preconcentration in Flavonoids Analysis
&ZHAO You-xuan1, 2, 3, WANG Dun-qing3, LI Xin-min3, YAO Qing-qiang2, LU Yuan-qi*3(1. School of Medical and Life Sciences, University of Jinan-Shandong Academy of Medical Sciences, Jinan 250062, C 2. Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan 250062, C 3. Analysis and Testing Centre, Dezhou University, Dezhou 253023, China), Huaxue Shiji, 2016, 38(4)
Abstract: In this work, the principles of capillary electrophoretic on-line preconcentration are introduced. The application of these techniques and their combinations in flavonoids analysis are reviewed. The trends of capillary electrophoretic on-line preconcentration in flavonoids analysis are discussed.
Key words: capil on-l flavonoids
非离子型微乳液增敏荷移反应光度法测定饲料中三聚氰胺
郭振良*，罗婷，王刚
（鲁东大学 化学与材料科学学院，山东 烟台& 264025）
摘要：OP\异戊醇\甲苯\水非离子型微乳液对电子给予体三聚氰胺与&电子受体茜素红的荷移反应有增敏作用，通过实验确定了微乳液增敏荷移反应的分光光度法测定条件。实验结果表明，微乳液增敏三聚氰胺与茜素红生成荷移络合物的最大吸收波长为560 nm，该络合物配位比为1 : 1.3，茜素红用量1.0 mL，温度55 ℃，加热反应时间40 min，pH 7.0为最佳反应条件，检出限为42.26 mg/L。
关键词：非离子型微乳液；三聚氰胺；茜素红；荷移反应；分光光度法
中图分类号：O657.3&&&&&& 文献标识码：A&&& 文章编号：（2016）
Determination of Melamine in Animal Feed via Spectrophotometryby Sensitized Reaction of Non-Ionic Microemulsion with Charge Transfer
GUO Zhen-liang*，LUO Ting，WANG Gang (School of Chemistry and Materials Science，Ludong University, Yantai& 264025, China)
Abstract: OP/isoamylol/methylbenzene/H2O microemulsion had strong sensitivity on the color reactions of the charge transfer reaction between melamine as electron donor and alizarin red as &-electron acceptor. The results showed that&melamine could react with alizarin red to form an 1∶1.3 complex under the condition of microemulsion sensitization. The maximum absorption peak was 560 nm. The reagent dosage of alizarin red 1.0 mL, temperature 55 ℃, heating reaction time 40 min and pH 7.0 were the optimum reaction conditions. The detection limit was 42.26 mg/L.
Key words：OP/isoamylol/methylbenzene/H2O microemulsion；melamine；alizarin red；charge transfer reaction；spectrophotometry
离子液体萃取-火焰原子吸收光谱法测定痕量铜
杜军良，周玉，何海艳，宋迪燊，何志坚，崔书亚*
（绵阳师范学院 化学与化学工程学院，四川 绵阳& 621000）
摘要：以N-正丁烷基苯并噻唑六氟磷酸盐温敏性离子液体为萃取剂，乙腈为分散剂，萃取富集痕量铜离子，用火焰原子吸收法测定，建立了一种快速、简便分析铜离子的新方法。考察了离子液体的浓度、冰浴时间、溶液pH、萃取温度、萃取时间等对萃取率的影响。结果表明，方法检出限为0.18 &g/L，相对标准偏差(RSD)为1.09%；对矿泉水和绿茶中铜离子进行分别检测，加标回收率为98.5% ~105.1%。
关键词：N-正丁烷基苯并噻唑六氟磷酸盐离子液体；重金属Cu2+；萃取；火焰原子吸收光谱法
中图分类号：O657.3&&& 文献标识码：A&&& 文章编号：（2016）
Determination of Trace Copper by Ionic Liquid-flame Atomic Absorption Spectrophotometry
DU Jun-liang, ZHOU Yu, HE Hai-yan, SONG Di-shen, HE Zhi-jian, CUI Shu-ya * (Department of Chemistry and Chemical Engieering, Mianyang Normal University, Mianyang 621000, China), Huaxue Shiji, 2016, Huaxue Shiji, 2016, 38(4)
Abstract: [C4Bth][PF6] used as extractant and acetonitrile used as dispersing solvent for extraction of copper ion in water samples. Coupled with flame atomic absorption spectrometry, a new analytical method for rapid and simple determination of trace amount of copper ion was developed. Effects of some experimental factors such as the amount of ionic liquid, dissolving temperature, extraction time and pH value were investigated and optimized. The results showed that under the optimized conditions the detection limit was 0.18 &g/L and the relative standard deviation (RSD) was 1.09%. The proposed method was applied in the analysis of Cu2+ in mineral water and green tea samples with spiked recoveries of 98.5% ~ 105.1%
Key words：[C4Bth][PF6] Cu2+; flame atomic absorption spectrometry
香精中小分子醇类的两种分析方法比较
司晓喜，朱瑞芝，张凤梅，刘春波，何沛，王昆淼，申钦鹏，刘志华
收稿日期：
基金项目：中国烟草总公司标准项目资助项目（）。
作者简介：司晓喜（1986-），男，云南昆明人，硕士，工程师，主要从事烟草化学和烟气化学研究。
通讯作者：刘志华，E-mail：。
(云南省烟草化学重点实验室 云南中烟工业有限责任公司技术中心，云南 昆明& 650231)
摘要：为快速测定香精中的小分子醇类，建立了溶剂萃取-气相色谱/质谱联用法（SE-GC/MS）和顶空-气相色谱/质谱联用法（HS-GC/MS）两种分析方法。对样品前处理条件和气相色谱/质谱检测条件进行了优化。溶剂萃取法（SE）选取5 mL乙醇为溶剂涡旋振荡5 min，顶空法以10 mL水为基质校正剂直接顶空进样。两种方法中样品均采用Innowax弹性毛细管柱分离，选择离子监测模式测定，选取氘代正丙醇-d5为内标，以内标法定量。结果表明，SE-GC/MS法相对标准偏差（RSD）＜3.8%，定量限低于0.86 mg/kg，加标回收率在93.8% ～ 106.3%。HS-GC/MS法RSD＜6.8%，定量限＜5.61 mg/kg，加标回收率在92.3% ～ 107.2 %。比较两种方法，两种方法回收率和RSD均满足分析要求；SE-GC/MS法定量限低于HS-GC/MS法，更适合低含量小分子醇类样品的测定；可根据分析样品的需要选择其一方法。
关键词：香精；醇类；溶剂萃取；顶空进样；气相色谱/质谱联用
中图分类号：O657.63　　文献标识码：A　 &文章编号：（2016）
Comparison of Two Methods to Determine the Small-Molecule Alcohols in Flavourings
&SI Xiao-xi, ZHU Rui-zhi, ZHANG Feng-mei, LIU Chun-bo, HE Pei, WANG Kun-miao, Sheng Qin-peng, LIU Zhi-hua*(Key Laboratory of Tobacco Chemistry, R&D Center of China Tobacco Yunnan Industrial CO., LTD, Kunming 650231, China)
Abstract: Two rapid methods were established for determination of small-molecule alcohols in flavourings that were solvent extraction coupled with gas chromatography/mass spectrometry (SE-GC/MS) and head space-gas chromatography/mass spectrometry (HS-GC/MS). The pre-treatment method of sample and the GC/MS condition were critically examined. The sample was extracted by vortex mixing for 5 min using 5 mL ethanol as solvent for solvent extraction (SE). The sample was direct sampled using 10 mL water as matrix correction agent for head space sampling (HS). The samples were separated by INNOWAX capillary column in selected ion monitoring (SIM) mode. The targets were quantitatively analyzed using internal standard method using n-propanol&d5 as internal standard. For SE-GC/MS, the relative standard deviations (RSDs) were below 3.8 %, and the limits of quantification (LOQs) were below 0.86 mg/kg, with the recoveries ranged from 93.8% to 106.3% at three spiked levels. For HS-GC/MS, RSDs were below 6.8 %, and LOQs were below 5.61 mg/kg, with recoveries ranged from 92.3% to 107.2% at three spiked levels. The recoveries and RSDs of both two methods could meet the analysis requirement. SE-GC/MS gave a lower LOQ than HS-GC/MS, which preferred for flavourings with low-content of small-molecule alcohols. Both two methods were adaptable to the rapid determination of small-molecule alcohols in flavourings, the choice may be based on need.
Key words: gas chromatography/mass spectrometry
罗丹明6G同步荧光法测定水中微量十二烷基苯磺酸钠
李岚*，郝洪庆，石雄峰
（嘉应学院 化学与环境学院，广东 梅州& 514015）
摘要：在pH 3.0磷酸氢二钠-柠檬酸缓冲液中，&D& = 25 nm，十二烷基苯磺酸钠(SDBS)对罗丹明6G的同步荧光有猝灭作用，SDBS的浓度在0.028 ~ 50 &g/mL范围内与lg(F0/F)呈良好的线性关系，方法的检出限为0.524 &g/L。据此建立了同步荧光猝灭测定微量十二烷基苯磺酸钠的新方法，该方法可用于水中十二烷基苯磺酸钠含量的测定。
关键词：十二烷基苯磺酸钠；罗丹明6G；同步荧光猝灭
中图分类号：O657.39&&&&& 文献标识码：A&&&&&&&& 文章编号：（2016）&&&&&&&&&&
Determination of Trace Sodium Dodecyl Benzene Sulfonate in Water by Synchronous Fluorescent Method with Rhodamine 6G
LI Lan*, HAO Hong-qing, SHI Xiong-feng (College of Chemistry and Environment, Jiaying University , Meizhou 514015, China), Huaxue Shiji, 2016, 38(4)
Abstract: A new method for the determination of micro-amounts of sodium dodecyl benzene sulfonate(SDBS) was developed based on the synchronous fluorescent quenching spectra. Synchronous fluorescent of Rhodamine 6G can be quenched with SDBS in the buffer solution of disodium hydrogen phosphate-citric acid with pH 3.0(&D& = 25nm). A good linear relationship between lg(F0/F) and the concentration of SDBS in the range of 0.028 ~ 50 &g/mL was obtained. The detection limit was 0.524 &g/L. The proposed method was applied in the determination of SDBS in water.
Key words: sodium dodec Rhodamine 6G; synchronous fluorescent quenching
有机进样-电感耦合等离子体发射光谱法测定汽油中的磷含量
吴志鹏*，秦平，钟惠蓓
（广州能源检测研究院，广东 广州& 510170）
摘要：采用有机进样-电感耦合等离子体发射光谱法测定汽油中磷的含量。以异辛烷为稀释剂，按照m (汽油) : m (异辛烷) = 1 : 3加以稀释后直接进入ICP-AES（电感耦合等离子体发射光谱）仪器测定。结果表明，本方法工作标准曲线在0 ~ 10 mg/kg（即稀释前磷含量在0 ~ 40 mg/kg）范围内线性关系良好，r = 0.9992，方法检出限为0.156 mg/kg，相对标准偏差＜5.0%，回收率在96.3% ~ 105.8%之间。
关键词：汽油；磷；有机进样；电感耦合等离子体发射光谱法
中图分类号： O657.31&&&&&&& 文献标识码：A&&&&&&& 文章编号：（2016）
WUZhi-peng*，QIN Ping，ZHONG Hui-bei（Guangzhou Institute of energy Testing，Guangzhou 510170，China）, Huaxue Shiji, )
Abstract：An organic direct injection-inductively coupled plasma atomic emission spectrometry was established for the analysis of phosphorus contents in gasoline. Isooctane as the diluent and the sample was diluted according to gasoline/isooctane (mass ratio)1/3 and determined by ICP-AES. The results showed that the standard curve of the method had a good linear relationship in the range of 0 ~ 10 mg/kg（namely the phosphorus contents was in the range of 0 ~ 40 mg/kg before the dilution）, the linear correlation coefficient was 0.9992; the detection limit by this method was 0.156 mg/kg and the recovery was 96.3% ~ 105.8% with relative standard deviation was less than 5.0%.
Key words: orga ICP-AES
基于酶辅助循环放大和银纳米簇技术构建荧光传感器用于MicroRNA的检测
刘景荣1，潘云苓1，赵燕苹2，陈梅2，夏垚坤2，兰建明2，韩志钟2，吴芳2，陈敬华2，李春艳*2
(1. 福州市第一医院 中西医结合肿瘤科，福建 福州& . 福建医科大学 药学院，福建 福州& 350108 )
摘要：基于双链特异性核酸酶(Duplex-specific nuclease，DSN)选择性切割DNA单链和DNA保护的银纳米簇的特性，建立了一种新型的荧光传感器用于MicroRNA(MiR-21)的高灵敏检测。当MiR-21存在时，与Cp杂交形成DNA/RNA双链结构，此时在DSN的水解下，释放出探针DNA部分片段和完整的MiR-21。释放出来的MiR-21可再次发生与Cp杂交、DSN酶切等反应，如此反复，可实现一条MiR-21分子与多条探针杂交、酶切的循环过程。经磁分离，上清液中的探针DNA部分片段与Ag+结合并在硼氢化钠（NaBH4）的还原下产生银簇，检测到较强的荧光信号。相反，当MiR-21不存在时，DSN对单链探针无酶切作用，不能水解Cp，经磁分离，上清液中检测不到荧光信号。在最佳条件下，该传感器检测MiR-21的线性范围为50 fmol/L ~ 10 pmol/L，检测限达6 fmol/L，而且具有较好的选择性，有望用于临床实际样本中微量MiR-21的检测。
关键词：磁珠；双链特异性核酸酶；银纳米簇；MiR-21；荧光生物传感器
中图分类号：O657.3&&&&&& 文献标识码：A&&&&& 文章编号：（2016）
A Fluorescence Sensor for MicroRNA Detection Based on Nuclease Assisted Target Recycling and Silver Nanoclusters
LIU Jing-rong1, PAN Yun-ling1, ZHAO Yan-ping2, CHEN Mei2, XIA Yao-kun2,& LAN Jian-ming2, HAN Zhi-zhong2, WU Fang2, CHEN Jing-hua2, LI Chun-yan*2 (1. Oncology of Traditional Chinese and Western Medicine, The First Hospital of Fuzhou City, Fuzhou 350009, C 2. School of Pharmacy, Fujian Medical University, Fuzhou 350108, China), Huaxue Shiji, 2016, 38(4)
Abstract: A novel fluorescence sensor was developed for microRNA (miR-21) detection based on duplex-specific nuclease (DSN) which can selectively cut the DNA single strand and DNA protected silver nanoclusters. In the presence of target miR-21, Cp hybridized with miR-21 to form a double-stranded DNA, which was recognized and digested by DSN, then the no complementary part of the Cp and the complete miR-21were released. The intact target miR-21 to hybridize with a new Cp and initiate the second cycle of hydrolysis. Eventually, through magnetic separation, the released DNA sequences can be combined with the Ag+ and produced silver nanoclusters under the reduction of sodium borate, and a strong fluorescent signal was detected. However, in the absence of the target miR-21, Cps cannot be hydrolyzed by DSN, after separation, no fluorescence signal was detected from the supernatant solution. Under the optimized conditions, the sensor showed a good linear relationship for miR-21 detection in the range of 50 fmol/L ~ 10 pmol/L with a detection limit as low as 6 fmol/L. Furthermore, the sensor exhibited a good selectivity, it&s expected to be used for the ultra-low detection of miR-21 in clinical real samples.
Key words: duplex- miR-21; fluorescence biosensor
氨基酸铜配合物的抗氧化活性分析
靳文娟*，杨帆&
(1.安康学院 化学化工系，陕西 安康& . 新疆库尔勒市塔里木油田建设工程有限责任公司，新疆 库尔勒& 841000)
摘要:采用氨基酸和醋酸铜为原料，设计合成4种不同配体结构的Cu(Ⅱ)金属配合物CuL1-4，并用紫外分光光度计和傅里叶红外检测仪对其化学结构进行了分析。采用改进的氮蓝四唑还原法确定了氨基酸铜金属配合物抗氧化活性最强时对应的浓度，并讨论了在相同浓度下不同种类氨基铜酸配合物的抗氧化活性与其化学结构之间的关系。结果表明，L-&-丙氨酸铜配合物由于金属活性中心周围空间位阻较小，其抗氧化活性高于苯丙氨酸铜配合物。
关键词：氨基酸；Cu(Ⅱ)配合物；抗氧化活性
中图分类号：TQ460.31&&& 文献标识码：A&&&&& 文章编号：（2016）
Amino Acid Copper Complexes Antioxidant Activity Analysis
JIN Wen-juan*，YANG Fan (1. Department of Chemistry and Chemical Engineering, Ankang University, Ankang 725000, C 2. Xinjiang Tarim Oilfield Construction Engineering Limited Company, Korla 841000, China), Huaxue Shiji, 2016, 38(4)
Abstract： Amino acids and copper acetate were used as raw materials to synthesize four kinds of Cu(Ⅱ) metal complexes (CuL1-4), the structure of complex was confirmed by UV and IR. The anti-oxidant activities and the optimal concentration were measured by using NBT illumination method. The relationship of the antioxidant activity of different type amino acid complexes and their chemical structure at the same concentration was discussed. The result shows that L-&-alanine has highest antioxidant activity because the copper complex has less steric hindrance around the metal center.
Key Words: Cu(Ⅱ) SOD-like activity
不同功能单体制备2-氨基喹啉印迹聚合物的分子识别特性
张铁莉*, 刘征原&&&
(唐山师范学院 化学系，河北 唐山　063000）
摘要：以2-氨基喹啉（2-AQ）为模板分子，分别以两种不同性质的酸性功能单体甲基丙烯酸(MAA)和三氟甲基丙烯酸(TFMAA)为功能单体，乙腈(MeCN)为致孔剂，制备了2-AQ分子印迹聚合物P(MAA)和P(TFMAA)，用色谱法表征了其分子识别性能，并比较了功能单体的性质对印迹效应的影响。结果表明，P(MAA)和P(TFMAA)对2-AQ均具有显著的印迹效应，在V(HAc)︰V(MeCN) = 5︰95流动相中，P(MAA)和P(TFMAA)对2-AQ的印迹因子IF分别为12.4和4.52。研究结果表明，能与2-AQ形成环状氢键的功能单体MAA较之与其主要形成单一氢键或静电作用的TFMAA相比较，环状氢键的形成更有利于印迹聚合物对2-AQ的选择性识别。
关键词：2-氨基喹啉；分子印迹聚合物；分子识别；功能单体; 高效液相色谱
中图分类号：O631.3&&&&&& 文献标识码：A&&&&& 文章编号：（2016）
Molecular Recognition Properties of 2-Aminoquinoline-Imprinted Polymers Synthesized Using Different Functional Monomers
ZHANG Tie-li*, LIU Zheng-yuan (Department of Chemistry, Tangshan Normal College, Tangshan 063000, China), Huaxue Shiji, 2016, 38(4)
Abstract: Two molecularly imprinted polymers P(MAA) and P(TFMAA) were prepared by non-covalent molecular imprinting technique using 2-aminoquinoline(2-AQ) as the template molecule and methacrylic acid (MAA) and trifluoromethacrylic acid (TFMAA) with different acidity as functional monomers, respectively, in the presence of acetonitrile porogen. The molecular recognition performances were evaluated by high-performance liquid chromatography. Also the comparison was made between the molecular imprinting effect of P (MAA) and that of P (TFMAA) in order to reveal the role of MAA and TFMAA on molecular recognition ability of molecularly imprinted polymers. The results demonstrated that both of the imprinted polymers P (MAA) and P (TFMAA) showed noticeable imprinting effects for 2-AQ. And the molecular imprinting factors of P (MAA) and P (TFMAA) for 2-AQ were 12.4 and 4.52, respectively, in the mobile phase of V(HAc)︰V(MeCN) = 5︰95. The result confirmed that MAA interacting with 2-AQ via cyclic/cooperative hydrogen bonding is more favorable for the preparation of high selective 2-AQ-binding imprinted polymer than TFMAA which interacts with 2-AQ via single hydrogen bonding or electrostatic interaction when they were chosen as the functional monomers.
Key words: 2- molecular m high-performance liquid chromatography
TEMPO抑制K2S2O8氧化甲苯生成苯甲醛过程中的过度氧化
林淑英，金旭康，刘仁华*
(华东理工大学 药学院，上海& 200237)
摘要：采用TEMPO/Cu(OAc)2为催化剂，探究其在抑制苯甲醛过度氧化成苯甲酸方面的能力，考察反应时间、反应温度、催化剂用量等因素对苯甲醛收率的影响。研究结果表明，TEMPO以及TEMPO衍生物在Cu(OAc)2催化下，可以有效地抑制甲苯合成苯甲醛的过程中苯甲醛进一步氧化成苯甲酸。优化条件下，甲苯氧化生成苯甲醛的收率高达78%，而且没有苯甲醇和苯甲酸生成。
关键词：甲苯氧化；苯甲醛；Cu(OAc)2 /TEMPO；K2S2O8
中图分类号：O626.2&&&&&&&&&文献标识码：A&&& &&&&&文章编号：（2016）
TEMPOs Suppressing Overoxidation in K2S2O8 Oxidation of Toluene to Benzaldehyde
LIN Shu-ying, JIN Xu-kang, LIU Ren-hua* (East China University of Science and Technology, Shanghai 200237, China), Huaxue Shiji, 2016, 38(4)
Abstract: The capability of inhibiting the overoxidation of benzaldehyde by using TEMPO/Cu(OAc)2 as the catalyst was investigated. The effects of operation parameters, such as reaction time, reaction temperature were investigated. The experimental results showed that the formation of benzoic acid from aldehyde products overoxidation can be inhibited by the addition of TEMPO and TEMPO derivatives in Cu(OAc)2 as the catalysts. Under the optimum&condition, the yield of benzaldehyde from toluene was up to 78%, while no benzyl alcohol and benzoic acid was formed.
Key words:
Cu(OAc)2/ TEMPO; K2S2O8
阳离子脂质体DLin-MC3-DMA合成
王晋萍，王胜，沈雪，杨帆*，汤杰
（华东师范大学 化学与分子工程学院，上海& 200062)
摘要：可电离的阳离子脂质体DLin-MC3-DMA是一种高效的siRNA运输载体，它能有效封装相应的siRNA并使其进入细胞质内，然后两者分离，siRNA发挥其功效。以价格低廉的亚油酸为起始原料，经还原、溴代、格氏和缩合等4步反应，高效合成了目标化合物DLin-MC3-DMA，不仅缩短了反应步骤，而且有效降低了成本。
关键词：阳离子脂质体；siRNA；运输载体；DLin-MC3-DMA
中图分类号：O623&& 文献标识码：A&&&&& 文章编号：（2016）
Synthesis of Cationic Lipid DLin-MC3-DMA
&WANG Jin-ping, WANG Sheng, SHEN Xue, YANG Fan*, TANG Jie (School of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200062), Huaxue Shiji, 2016, 38(4)
Abstract: DLin-MC3-DMA, as an efficient transport agent of siRNA, can package the siRNA to form LNPs/siRNA complex, and then transport them into cytoplasm efficiently. Afterwards, the complex separates and the siRNA plays its function. In this work, DLin-MC3-DMA was high efficiently synthesized via four steps including reduction, bromination, Grignard reaction, and condensation with cheaper linoleic acid as the starting material. The method shortened the reaction procedure and lowered the cost effectively as well.
Key words:
siRNA; DLin-MC3-DMA
糠醛缩异烟肼席夫碱的合成及其晶体结构
倪萌，范超逸，韦华传，李璇，韦立先，张秀清*
（桂林理工大学 化学与生物工程学院 广西电磁化学功能物质重点实验室，广西 桂林& 541004）
摘要：席夫碱配体及其配合物可应用于生物化学、分析化学、材料化学等方面，由于其广泛的应用，已成为现阶段研究者研究的热点。糠醛是重要的化工原料，异烟肼是抗结核病的主要药剂，采用这两种化合物，通过混合溶液法在80 ℃恒温水浴中，以新制备的糠醛溶液和异烟肼溶液为原料合成了一个小分子席夫碱，通过红外光谱、紫外光谱、质谱、X-射线衍射仪表征其结构。结果表明，该席夫碱属于单斜晶系，空间群为P21/c，晶胞参数为a = 10.7170 (6) &A ，b = 5.2389 (2) &A，c = 18.1235 (9) &A，& = 90&，& = 94.445 (5)&，& = 90&，Z = 4，& = 0.101 mm-1，F (000) = 448，De = 1.409 g&cm-3。
关键词：席夫碱；合成；表征
中图分类号：O626.32&&&&&& 文献标识码：A&&&&& 文章编号：（2016）
Synthesis and Crystal Structure of Furfural-isoniazid Schiff Base
NI Meng, FAN Chao-yi, WEI Hua-chuan, LI Xuan, WEI Li-xian, ZHANG Xiu-qing*(Guangxi Key Laboratory of Electrochemical and Magneto-chemical Functional Materials, College of Chemical and Biological Engineering, Guilin University of Technology, Guilin 541004, China), Huaxue Shiji, 2016, 38(4)
Abstract: Schiff base ligands and their complexes can be used in biochemistry, analytical chemistry, materials chemistry, etc. It has become a hot spotdue to its wide application approach Furfural is an important chemical raw materials and isoniazid is the main anti-TB drug. These two compounds, by mixing a solution method at 80 ℃ water bath to freshly prepared furfural and isoniazid solution synthesized Schiff base of a small molecule. The structure was confirmed by IR, UV, mass spectrometry, X-ray diffraction. The results showed that: the Schiff base belonging to the monoclinic system, space group P21/c, unit cell parameters: a = 10.717 0 (6), b = 5.238 9 (2), c = 18.123 5 (9), & = 90&, & = 94.445 (5)&, & = 90 &, Z = 4, & = 0.101 mm-1, F (000) = 448, De = 1.409 g&cm-3.
Key words: S characterization
烟酸类表面活性剂的合成研究
刘佳，王丽艳*，张玥，张超，刘世夫，田莹，赵明
(齐齐哈尔大学 化学与化学工程学院，黑龙江 齐齐哈尔& 161006)
摘要：以烟酸为原料，通过卤置换反应、酰胺化反应、季铵化反应3个步骤，合成[3, 3'- (对苯二氨甲酰基)]双N-烷基吡啶溴盐表面活性剂目标产物。用IR、1HNMR、13CNMR和MS对目标产物进行确认和表征，并通过单因素试验，确定了较佳的合成条件为：n (双(烟酰基)对苯二胺)︰n (溴代烷)＝1 : 2.6，反应温度为140 ℃，反应时间6 h。利用紫外分光光度法测量目标产物的临界反胶团浓度CrMC分别为2.09&10-5、2.27&10-5和2.39&10-5 mol/L。
关键词：烟酸；卤置换；酰胺化；季胺化；合成
中图分类号：TQ423&&&& 文献标识码：A&&&&&&&&&文章编号：（2016）
Synthesis of Niacin Surfactants
LIU Jia, WANG Li-yang, ZHANG Yue*, ZHANG Chao, LIU Shi-fu, TING Ying, ZHAO Ming (College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China)
Abstract: A series of [3, 3'-(p-phenyldiaminocarbonyl)] bis(N-alkyl) pyridinium bromide surfactants products were prepared by chloride displacement, amidation and quaterisation. The structure of products was confirmed by IR, 1HNMR, 13CNMR and MS. The reaction temperature was 140 ℃, the reaction time was 6 h, the mole ratio of intermediate bis (nicotinoyl) p-phenylenediamine and bromoalkane was 1 : 2.6. The critical reverse micelle concentration (CrMC) of the target products are 2.09&10-5, 2.27&10-5, 2.39&10-5 mol/L by UV spectrophotometer measurement respectively.
Key words:
chloride d synthesis
4-氯-5,6-二氢吡啶并[3,4-d]嘧啶-7(8H)-羧酸叔丁酯的合成
樊玲玲，曹俊，李永，崔杏，王建塔，汤磊*
( 贵州医科大学 药学院，贵州 贵阳& 550004 )
摘要:以4-氨基丁酸为原料，依次通过酯化、取代、两次关键环合、&Appel-Lee反应，成功合成了目标化合物，并通过1HNMR和MS对其结构进行了确认。该方法反应条件温和，原料成本低，操作简单，总收率53.9%，是经济价值较高的合成路线。
关键词:4-氨基丁酸； Appel-Lee反应；合成
中图分类号:& O626.4&&&&&& 文献标识码: A&&&&&&& 文章编号：（2016）
Synthesis of Tert-butyl-4-chloro-5,6-dihydropyrido[3,4-d]pyrim-idine-7(8H)-carboxylate
FAN Ling-Ling, CAO Jun, LI Yong, CUI Xin, WANG Jian-Ta, TANG Lei*&(College of Pharmacy, Guizhou Medical University, Guiyang 550004, China)
Abstract: Tert-butyl-4-chloro-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxylate was synthesized in 53.9% overall yield from 4-aminobutyric acid via esterification, substitution, two designated key cyclization, Appel lee reaction. The structure was confirmed by 1HNMR and MS spectra. The current method has the advantages of mild reaction conditions, low cost, simple operation, and high overall yield. Thus, it is the synthetic routes with high economic value.
Key Words: 4-aminobutyric acid; Appel-L synthesis
咪唑并[1,2-a]吡啶化合物的简便合成
樊红莉*，李鑫
（菏泽学院 化学化工系，山东 菏泽& 274015）
摘要：以2-氨基-3-羟基吡啶为原料，经过一锅两步反应合成了12个咪唑并[1, 2-a]吡啶类化合物。2-氨基-3-羟基吡啶与N，N-二甲基甲酰胺二甲基缩醛进行反应，几乎定量得到中间体（E）-N'-（3-羟基吡啶-2-基）-N，N-二甲基甲脒中间体，然后在NaHCO3作用下，于一锅中和活泼亲电化合物（溴乙酸乙酯、溴乙腈和2-溴代苯乙酮）发生合成咪唑环的反应及羟基上的取代反应，以50.3% ~ 85.2%的总收率得到目标产物。该一锅两步方法具有原料易得、反应时间短、操作简便、收率高等优点。
关键词：2-氨基-3-羟基吡啶；活泼亲电化合物；咪唑并[1, 2-a]吡啶；合成
中图分类号：O626.2&& &文献标识码：A&&&&& 文章编号：（2016）
Convenient Method for Synthesis of Imidazo[1,2-a]pyridines
FAN Hong-li*, LI Xin (Department of Chemistry and Chemical Engineering, Heze University, Heze 274015, China）
Abstract: Twelve imidazo[1,2-a]pyridines were prepared from 2-amino-3-hydroxypyridine via a two-step one-pot process. Firstly, 2-amino-3-hydroxypyridine reacted with N, N-dimethylformamide dimethyl acetal to afford the intermediate (E)-N'-(3-hydroxy-pyridin-2-yl)-N, N-dimethylformamidines almost quantitatively,& and then followed by the cyclization reaction and the substitution reaction of hydroxyl group with the active electrophiles (ethyl bromoacetate, bromoacetonitrile and 2-bromoacetophenone&) catalyzed by NaHCO3 in one-pot furnishing the target compounds with a yield ranged from 50.3% to 85.2%. The synthesis method has the advantages of readily available starting materials, short reaction time, easy workup and high yield．
Key words: 2-amino-3-
imidazo[1,2-a] synthesis
配合物Ni(C6H6NO3S)2(H2O)4的合成、表征及热稳定性
欧阳淼*1，王静*2，银秀菊1，张运良3，陆俊宇1，林宗宇1
（1. 河池学院 化学与生物工程学院，广西 宜州 　546300； 2. 东莞出入境检验检疫局，广东 东莞 　. 邵阳医学高等专科学校，湖南 邵阳 　422000）
摘要：用常温挥发法合成了一个新颖的单核配合物Ni(C6H6NO3S)2(H2O)4，并利用红外光谱、元素分析、热重分析及X-射线单晶衍射法对其结构进行了表征。结果表明，该配合物晶体属于单斜晶系，P121/n1空间群，晶胞参数为：a = 1.1912 nm，b = 0.633 nm，c = 1.224 nm，& = 108.936&，Z = 2，R1 = 0.0271，wR2 = 0.1007。在标题配合物中，每个Ni2+与4个H2O分子的氧原子及来自两个邻氨基苯磺酸的两个氮原子配位，形成一个畸变的八面体构型。在该配合物中，磺酸基的氧原子没有配位，这表明在该体系下，H2O的配位性能优于磺酸基氧原子。CCDC：1033789。
关键词：磺酸基；镍配合物；晶体结构
中图分类号：O61&&&&&文献标识码：A&&&&文章编号：（2016）
Synthesis, Characterization and Thermal Stability of a Complex Ni(C6H6NO3S)2(H2O)4
OUYANG Miao*1, WANG Jing*2, YIN Xiu-ju1, ZHANG Yun-liang3, LU Jun-yu1, LIN Zong-yu１(1. School of Chemistry and Bioengineering, Hechi University, Yizhou 546300, C 2. Dongguan Entry-Exit Inspection and Quarantine Bureau, Dongguan 523072, C 3. School of Medical, Shaoyang Medical College, Shaoyang 422000, China), Huaxue Shiji, 2016, 38(4)
Abstract: A novel mononuclear complex, Ni(C6H6NO3S)2(H2O)4, was prepared by a evaporation method at room temperature, and characterized by elemental analysis, infrared spectra, thermal stability analysis and X-ray single crystal diffraction method. The results show that the crystal structure belongs to monoclinic system with P121/n1 space group and parameters of crystallography are as follows: a = 1.1912 nm，b = 0.633 nm，c = 1.224 nm, & = 108.936&, Z = 4, R1 = 0.0271, wR2 = 0.1007. In the title complex, each Ni2+ is coordinated by four oxygen atom from four H2O molecular and two nitrogen atoms from two o-amino-benzenesulfonic acid, forming a distorted octahedral configurations. In the complex, sulfonic group did not participate in coordination, suggesting that the coordination ability of water priors to that of sulfonic acid group under this condition.
Key words:
依折麦布环醚杂质的制备及其晶体结构表征
胡延杰1，李战军1，李运丽1，陈水库2，张方杰2，郝平平2，李雯*3
（1. 郑州大学 a. 化工与能源学院；b. 药学院；河南 郑州& . 河南辅仁医药科技开发有限公司，河南 郑州& 450003）
摘要：药物杂质与药品的安全性和稳定性密切相关，对药物杂质进行充分研究是药品质量控制的必要过程。依折麦布、尿素在无水乙醇和无水甲醇溶剂中，室温存放可顺利获得依折麦布环醚杂质晶体，该环醚杂质结构经单晶衍射表征。结果显示，晶胞参数a = 6.1407（4），b = 7.6603（5），c = 11.1455(7)，& = 72.497(5)，& = 99. 535(2) &，& = 85.538(5)。属于三斜晶系，P1空间群。
关键词：依折麦布；环醚杂质；制备；单晶结构
中图分类号：R914.5&&&&&& 文献标识码：A&&&&&&& 文章编号：（2016）
Preparation and Crystal Structures of Cyclizate Ether Impurity of Ezetimibe
HU Yan-jie1, LI Zhan-jun1, LI Yun-li1, CHEN Shui-ku2, ZHANG Fang-jie2, HAO Ping-ping2, LI Wen*3（a. School of Chemical Engineering and E b. School of Pharmacy, Zhengzhou University, Zhengzhou 450001, C 2. Henan Furenmedicine Technology Development Co., Ltd., Zhengzhou 450003, China）, Huaxue Shiji, 2016, 38(4)
Abstract: Drug impurities are closely related to the safety assessment and stability of drugs. A comprehensive study of impurities is critical process for the drug quality control. Cyclizate ether impurity crystal of Ezetimibe was prepared by put Ezetimibe and urea in anhydrous ethanol and anhydrous methanol solvent under room temperature. The crystal structure of cyclizate ether impurity was confirmed by X-ray single crystal diffractometer. The results present that the cell parameters a = 6.1407（4）, b = 7.6603（5）, c = 11.1455(7) , & = 72.497(5) & , & = 99. 535( 2) &, & = 85.538(5) &, and belongs to triclinic, space group P1.
Key words: E cycl crystal structures
3,3,3-三氟-2,2-二甲基丙酸的合成
陈& 群*1，朱国彪2
（1.常州工程职业技术学院 化工与材料学院，江苏 常州& 213164；
2.常州大学 石油与化工学院，江苏 常州& 213164）
摘要：以自制的2,2-二甲基丙二酸单甲酯为原料，经氟代、水解和酸化反应制备出目标化合物，产率49.6%。分别考察了氟代时间、氟代温度、SF4用量对氟代反应的影响，氟代产物中CH2Cl2含量、水解时间对水解反应进程的影响。适宜的反应条件为：氟代反应时间3 h，氟代反应温度80 ℃，物质的量比n (2,2-二甲基丙二酸单甲酯) : n (SF4)= 1 : 6；氟代产物中CH2Cl2 含量& 0.5%，水解反应时间30 min。
关键词：2,2-二甲基丙二酸单甲酯；氟代；水解；酸化
中图分类号：O625.21&&&&&&&&&& 文献标识码：A&&&& 文章编号：（2016）
Synthesis of 3,3,3-Trifluoro-2,2-dimethylpropionic Acid
CHEN Qun1，ZHU Guo-biao2 (1. School of Materials and Chemistry and Chemical Engineering, Changzhou Institute of Engineering Technology, Changzhou . Petrochemical and Chemical Engineering School，Changzhou University，Changzhou 213164, China)
Abstract: 2,2-dimethyl-malonic acid monomethyl ester was used as raw material.The target compound was synthesized by the reactions of fluoridation, hydrolysis and acidification with an overall yield of 49.6%. The influence of time, temperature, amount of SF4 on the fluoridation& and& amount of &CH2Cl2, the time on the hydrolysis reaction were investigated. The optimized conditions were as follows: the time of fluoridation was 3 h，the temperature of fluoridation was 80 ℃, n ( 2,2-dimethyl-malonic acid monomethyl ester) : n ( SF4)= 1 : 6；amount of CH2Cl2 & 0.5%；the time of hydrolysis was 30 min.
Key Words: 2,2-dimethyl-malonic a acidification