含Co3O4自组装的3D石墨烯气凝胶及其电容器性能研究
闫慧君*，姜艳丽，田玫，杨丽娟，徐华北
(哈尔滨学院 食品工程学院，黑龙江 哈尔滨 150086)
摘要：设计了一种简单的一步水热法制备三维(3D)多孔的Co3O4/石墨烯气凝胶(GA)材料。因石墨烯(Graphene)所形成互相连通的三维孔道以及Co3O4纳米微球丰富多孔的结构，Co3O4/GA表现出良好的导电性和赝电容性，成为优异的用于能量储存装置的电极材料。该Co3O4/GA复合物拥有高比表面积（139 m2/g）和较宽的孔径分布（约为1～100 nm）。单纯GA的比电容值为175.5 F/g，由于Co3O4微球的引入，使复合物气凝胶的比电容值得到了显著提升，在电流密度为1 A/g时，比电容值高达1456.3 F/g。以Co3O4/GA为正极、GA为负极、LiOH/PVA为凝胶电解质组装成全固态非对称超级电容器，当功率密度为648.9 W/kg时，该SASC拥有优异的能量密度为68.1 W ·h ·kg-1，说明此Co3O4/GA是一种优异的超级电容器电极材料。
关键词：一步合成法；Co3O4/石墨烯气凝胶；全固态；非对称超级电容器
中图分类号：O611.64 文献标识码：A 文章编号：
Co3O4 Embedded in Self-assembled Three-dimensional Graphene Aerogel Networks for High-performance Supercapacitor YAN Hui-Jun*, JIANG Yan-Li, TIAN Mei, YANG Li-Juan, XU Hua-Bei (Department of Chemistry, College of foodengineering ,Harbin University, Harbin 150086, China)
Abstract：A facile one-step hydrothermal strategy has been developed to prepare 3D porous Co3O4/graphene aerogel (Co3O4/GA). Due to combination of a highly interconnected 3D network framework of GA and Co3O4 microspheres, Co3O4/GA electrode exhibits exceptional electrical conductivity and pseudocapacitance to make it an excellent material for energy storage devices. The Co3O4/GA composites possess a high specific surface area of 139 m2/g and a broad pore size distribution of 1 ～ 100 nm. Although GA shows a high specific capacitance of 175.5 F/g, the presence of Co3O4 microspheres are found remarkably effective in enhancing this of the composite aerogel up to 1456.3 F/g at 1 A/g. Furthermore, the combination of the two aerogel electrodes with LiOH/PVA gel electrolyte endow our all-solid-state asymmetric supercapacitor (SASC) of Co3O4/GA//GA a stable cycling performance, and superior electrochemical performance with an energy density of 68.1 W h kg-1 at a power density of 648.9 W/kg. These results indicate that Co3O4/GA could be a potential candidate in the field of supercapacitors.
Key words：one-step synthesis; Co3O4/graphene aerogels; all-solid-state; asymmetric supercapacitor
PW11Fe/聚苯胺/SnO2复合催化剂对孔雀石绿的光降解性能研究
马荣华*，王思元
（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：以铁元素取代钨磷酸盐为活性组分，制备了PW11Fe/PANI/SnO2三元复合催化剂，采用IR、UV、XRD、XPS和SEM表征了其结构，并通过测试孔雀石绿的光催化降解效果来评价PW11Fe/PANI/SnO2的光催化性能。结果表明，经过30 W的紫外灯照射，调节pH 2、孔雀石绿染料的浓度为5 mg/L、加入50 mg/L的PW11Fe/PANI/SnO2，在200 min的紫外光照降解下，降解率可达92.65%。PW11Fe/PANI/SnO2光催化降解孔雀石绿过程符合准一级动力学反应。该一级方程反应速率常数为0.00778 min-1。
关键词：杂多酸盐；光催化；孔雀石绿；降解
中图分类号：O643.3；O644.1 文献标识码：A 文章编号：0258-3283（2018）
Photodegradation Performance of Malachite Green by Composite Catalyst PW11Fe/ Polyaniline/SnO2 MA Rong-hua*,WANG Si-yuan(College of Chemistry and Chemical Engineering，Qiqihaer University, Qiqihaer 161006)
Abstract: With iron substituted heteropolytungstenphosphate asactive componentscomposite catalyst PW11Fe/PANI/SnO2 was prepared and characterized by IR, UV, XRD , XPS and SEM. The photocatalytic degradation of malachitegreen was selected as probe to evaluate the enhanced photocatalytic activity of the as-synthesized PW11Fe/PANI/SnO2. The degradation rate of malachitegreen achieved 92.65% when 5 mg/L of malachitegreen containing simulated solution at pH 2 was treated by 30 W ultraviolet light for 200 min with 50 mg/L ofPW11Fe/PANI/SnO2 as catalyst. The kinetics of the photodegradation of malachitegreen fitted by the pseudo-first-order equationwith a constant at 0.00778 min-1．
Key words:heteropolyacid;photocatalysis; malachite green; degradation
雀儿舌头光谱性质及其与BSA相互作用的研究
魏光璞，龙跃*
（郑州大学 化学与分子工程学院，河南 郑州 450001）
摘要：通过荧光光谱法和紫外吸收光谱法研究了中药雀儿舌头(Leptopus chinensis)的光谱性质以及LC与牛血清白蛋白(BSA)之间的相互作用。研究了溶剂、提取时间、浓度、pH值对雀儿舌头提取物荧光特性的影响。乙醇作为提取溶剂，提取时间设定为10 min，在中性条件下测定。在激发波长280 nm和狭缝宽度5 nm条件下，观察到BSA的荧光猝灭以及LC的荧光敏化。LC对BSA酪氨酸和色氨酸残基的影响结果表明，LC与BSA中色氨酸残基之间发生了能量转移。
关键词：雀儿舌头；牛血清白蛋白；紫外吸收光谱；荧光光谱；同步荧光光谱
中图分类号：R282.71 文献标识码：A 文章编号：
Spectral Properties of LeptopusChinensis and Interaction between LeptopusChinensis and Bovine Serum Albumin WEI Guang-pu, LONG Yue*(College of Chemistry and Molecular Engineering，Zhengzhou University，Zhengzhou 450001，China）, Huaxue Shiji, 2018, 40(4)
Abstract: The spectroscopic properties of L.chinensis(LC) and the interaction between LC and bovine serum albumin (BSA) were investigated by fluorescence spectroscopy and Ultraviolet absorption spectroscopy. The effects of solvent, extraction time, concentration, pH on the fluorescence properties of LC were investigated. The following experimental conditions were used finally: ethanol was selected as solvent, extraction time was set to 10 min, measured under neutral conditions. Fluorescence quenching of BSA was observed at an excitation wavelength of 280 nm and a slit width of 5 nm. BSA showed a fluorescence sensitization effect on LC. The effect of LC on the tyrosine and tryptophan residues of BSA showed that there was energy transfer between tryptophan residues in BSA and LC.
Key words: Leptopuschinensis(LC)；bovine serum albumin(BSA)；Ultraviolet absorption spectroscopy; fluorescence spectroscopy；synchronous fluorescence spectrum
Pt/WO3-x纳米催化剂的制备及其性能的研究
于志勇1, 2，余小龙2，华达银1，尹宏峰*2
（1. 宁波大学 理学院，浙江 宁波 315211；2. 中国科学院 宁波材料技术与工程研究所，浙江 宁波 315201）
摘要:首先采用水热法合成WO3-x前驱体，再用浸渍法和热分解法制得Pt/WO3-x纳米催化剂。利用XRD、TEM以及H2-TPR测试方法对其进行了表征分析。结果表明，Pt纳米颗粒在WO3-x表面分散性好，并且Pt纳米颗粒与WO3-x之间存在较强的相互作用。在对硝基苯酚加氢反应中，与Pt/Al2O3纳米催化剂相比，Pt/WO3-x纳米催化剂在300 ℃焙烧后显示出优越的催化性能，这可能归因于金属与金属氧化物之间的强相互作用。
关键字：Pt/WO3-x；催化加氢；对硝基苯酚；强相互作用
中国分类号：O643.3 文献标识码：A 文章编号：0258-3283（2018）
Catalytic Performanceand Preparation of Pt/WO3-XNanocatalysts YU Zhi-yong1,2,YU Xiao-long2, HUA Da-yin1, YIN Hong-feng* 2 (1.Faculty of Science, Ningbo University, Ningbo 315211,China; 2.Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Science, Ningbo 315201, China）
Abstract: WO3-X precursor was synthesized by water bath method. Pt /WO3-Xnanocatalyst was prepared by impregnation and thermal decomposition. XRD, TEM and H2-TPR were used to characterize them. The results show that Pt nanoparticles are well dispersed on the surface of WO3-x，and there is a stronger interaction between Pt nanoparticles and WO3-x. In the hydrogenation of p-nitrophenol, with the comparative activity of Pt/Al2O3nanocatalyst, the Pt/ WO3-Xnanocatalyst shows superior catalytic performance after calcination at 300℃, which may attribute to a strong interaction between the metal and the metal oxide.
Key words: Pt/WO3-X ; catalytic hydrogenation; p-nitrophenol; strong interaction
含卤素吡唑啉衍生物的合成及其初步抗肿瘤活性研究
韩金良，辛亚兵，樊杨懿，张文东，田玉顺*
（延边大学 药学院，吉林 延吉 133002）
摘要：设计并合成了8种含卤素的吡唑啉衍生物，经1HNMR，13CNMR和高分辨质谱验证并用MTT测试了其在9种细胞中的抗增殖活性。结果表明，所有化合物对所有细胞的抗增殖活性均大于阳性对照药DDP，且6种化合物对HeLa和SGC-7901两种细胞的抗增殖活性均明显强于阳性对照药Taxol，而2-氯-1-(5-(4-氯苯基)-3-(4-硝基苯基)-4,5-二氢-1H-吡唑-1-基)乙酮对HepG2细胞的毒性与Taxol的细胞毒性相当。所有化合物对肿瘤细胞和正常细胞显示选择性抑制活性。此外，吡唑啉环氮原子所连碳链长度为2的系列化合物，其IC50值均小于15 μmol/L，而当碳链长度为4时，其IC50值偏大。经初步分析，吡唑啉衍生物的细胞毒性和吡唑啉环氮原子上所连碳链长度有关，碳链越长，活性越差。但B环上的不同卤素取代基对活性没有明显的影响。
关键词：吡唑啉；抗肿瘤活性；选择性抑制；碳链长度；卤素
中图分类号:R914.5；R965.1 文献标识码: A
Synthesis and preliminary anti-tumor activity evaluation of pyrazoline derivatives bearing halogen HAN Jin-liang, XIN Ya-bing, FAN Yang-yi, ZHANG Wen-dong, TIAN Yu-shun* （College of Pharmacy, Yanbian University, Yanji 133002, China）
Abstract: Eight pyrazoline derivatives bearing halogen were designed and synthesized and the compounds were characterized with 1H NMR, 13C NMR and HRMS and the anti-proliferatory activities were evaluated by MTT assay against nine cell lines. The result indicated that all the synthesized compounds expressed stronger anti-proliferative effects than positive control DDP against all cell lines, and six compounds displayed significantly stronger anti-tumor activities than the positive control drug taxol in HeLa and SGC-7901 cells, but the toxicity of (2-chloro-1-(5-(4-chlorophenyl)-3-(4-nitrophenyl)-4,5-dihydro-1H-pyrazol-1-yl)ethanone) was comparable to that of taxol against HepG2 cells. In tumor cells and normal cells, all compounds showed selective inhibitory activity. In addition, the IC50 values of the series of compound which contains chains with two carbon on nitrogen atom of pyrazoline structure, were less than 15 μmol/L, but when the carbon chain length is four, the IC50 values became high. Preliminary analysis revealed that the cytotoxicity of pyrazoline derivatives were relative to the length of carbon chain on nitrogen atom of pyrazoline structure. However, the different halogen substituents The longer the carbon chain is, the worse activity the compound has.on the B ring have no obvious effect on the bioactivity.
Key words: pyrazoline; anti-tumor activity; selective inhibition; carbon chain length; halogen
氧化石墨烯固载硅钨酸催化氧化脱硫性能的研究
丁邦琴*，朱蓓蓓，李侠
(南通职业大学 化学与生物工程学院，江苏 南通 226007)
摘要：以市售氧化石墨烯固载硅钨酸制备硅钨酸/氧化石墨烯（SiW/GO）复合材料，利用X-射线衍射光谱（XRD）、红外光谱（FT-IR）对SiW/GO材料进行表征。以H2O2为氧化剂，考察该催化剂对模拟油中二苯并噻吩（DBT）的氧化性能。结果表明，硅钨酸与氧化石墨烯结合紧密，复合后仍保持了硅钨酸的Keggin结构；在H2O2加入量为1.5 mL、催化剂用量为12 mg/mL、反应温度为70 ℃、反应时间为80 min条件下，DBT的脱除率达96.4%。催化剂经过滤、洗涤和干燥后，循环使用5次，依然保持良好的脱硫性能。
关键词：硅钨酸；氧化石墨烯；二苯并噻吩；氧化脱硫
中图分类号：TE626 文献标识码：A 文章编号：
Catalytic Performance of Silicotungstic Acid Supported on Grapene Oxide for Oxidative Desulfurization DING Bang-qin*(College of Chemical and Biological Engineering, Nantong Vocational University, Nantong 226007, Jiangsu China)
Abstract：Silicotungstic acid/graphene oxide (SiW/GO) composites were prepared by supporting silicotungstic acid onto surfaceofmarket graphene oxide. The prepared composites were characterized by X-ray diffractometryand FT-IR. With SiW/GO as a catalyst, the oxidative desulfurization of model oil containing dibenzothiophene was carried out by using hydrogen peroxide as oxidant. The results showed that SiW/GO kept the Keggin structure with tight bonding between silicotungstic acid and graphene oxide.Thedibenzothiophene conversion can reach 96.4% under the conditions of H2O2 amount 1.5 mL, the catalyst concentration 12 mg/mL, reaction temperature 70 oC and reaction time 80 min. Moreover, the used SiW/GO still kept good desulfurization performance after 5 recycles, which were regenerated by filtering, washing and drying.
Key words：silicotungstic acid; graphene oxide; dibenzothiophene; oxidative desulfurization
碳纳米管及其改性材料在催化苯甲醇选择氧化中的应用
何萍*，张京京，潘懿
（营口理工学院 化学与材料工程系，辽宁 营口 115014）
摘要：环保政策日趋严格，传统的苯甲醇氧化反应受到挑战，开发绿色、高效的催化体系成为重要的研究课题。同时，碳纳米管由于其独特的结构和优异的理化性质，在催化领域受到人们的广泛关注。根据近几年的研究成果，介绍了以碳纳米管（CNTs）及其改性材料作为催化剂载体或催化剂，在苯甲醇选择氧化制苯甲醛中的应用。结果发现，多数反应体系都在无溶剂或水作溶剂，以分子氧或空气作为氧化剂的条件下进行，符合绿色化学原则。对碳纳米管进行掺杂、官能化能够改善CNTs表面物理化学性质，拓展CNTs在液相选择氧化方面的应用。
关键词：碳纳米管；苯甲醇选择氧化；掺杂碳纳米管；碳纳米管复合材料
中图分类号：O643.36 文献标识码：A 文章编号：0258-3283（2018）
Application of carbon nanotube materials in selective oxidation of benzyl alcohol HE Ping*, ZHANG Jing-jing, PAN Yi（Department of Chemical and Material Engineering, Yingkou Institute of Technology, Yingkou 115014, China）
Abstract: The traditional methods of oxidation of benzyl alcohol are challenged, because the request of environmental protection is more and more strict. Developing green and efficient catalytic system becomes an important research topic. Carbon nanotubes (CNTs) have attracted considerable attention in the fields of catalysis, due to its unique structure and excellent physical and chemical properties. According to the research results in recent years, the application of CNTs and modified carbon nanotubes as catalyst carrier or catalyst in the selective oxidation of benzyl alcohol to benzaldehyde was introduced. Most reactions were carried out without any solvent or with water as solvent, with molecular oxygen or air as oxidant, in accordance with the green chemical principle. The surface physical and chemical properties of carbon nanotubes can be improved by doping and fuctionalized to expand the application of CNTs in liquid phase selective oxidation.
Key words: carbon nanotubes; selective oxidation of benzyl alcohol; doping carbon nanotubes; CNTs nanohybrids
动态顶空-气相色谱质谱法测定家用搅拌机中7种苯系物迁移量
彭剑林，王志娟，李海玉，王婉，张庆，白桦，吕庆*
(中国检验检疫科学研究院 工业与消费品安全研究所，北京 100176)
摘要：基于动态顶空-气相色谱质谱技术，建立了家用搅拌机中7种苯系物迁移量的测定方法。采用0.8 L （10%）乙醇模拟液在搅拌机正常工作下进行迁移，以动态顶空吹扫捕集进样、气相色谱-质谱联用检测、外标法定量。该方法对7种苯系物的定量限（LOQ）为0.2 ～ 0.4 μg/L，具有较高的灵敏度，在0.2 ～ 20.0 μg/L浓度范围内线性关系良好（其中：苯的线性浓度范围为0.4 ～ 20.0 μg/L，7种苯系物的R2≥0.9956）。低、中、高3个添加浓度水平的平均回收率在76.7% ～ 123.3%之间，相对标准偏差（RSD，n = 6）在2.2% ～ 14.1%之间。该方法操作简单、快速、环保、灵敏度高，可用于家用搅拌机中苯系物的迁移量检测。
关键词：动态顶空；家用搅拌机；苯系物；迁移量
中图分类号： O657.63 文献标识码：A 文章编号：0258-3283（2018）
Determination of BTEXs Migration Amount in Food Blender by GC-MS with Dynamic Headspace Autosampler PENG Jian-lin, WANG Zhi-juan, LI Hai-yu, WANG Wan, ZHANG Qing, BAI Hua , LV Qing*(Institute of Industrial and Consumer Product Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China), Huaxue Shiji, 2018, 40(4)
Abstract: A method was developed for the determination of BTEXs migration amount in food blender by GC-MS with dynamic headspace autosampler (DHS). 0.8 L of food simulants were added to blender and the migration process was held 30 min under the normal operation, then the migration analytes were determined by GC-MS with DHS auto-sampler and quantified by external standard method. The limits of quantification (LOQ) of the method established were 0.2 ~ 0.4 μg/L for analytes. The linear ranges with good correlation coefficient (R2≥0.9956) were obtained as 0.4 ~ 20.0 μg/L for benzene and 0.2 ~ 20.0 μg/L for other analytes. Moreover, the average recoveries of analytes at three added levels ranged from 76.7% to 123.3% with relative standard deviations (RSD) varied from 2.2% to 14.1% (n=6) in food simulants. Finally, the method was applied to test nine commercial blenders. In conclusion, the method is simple, rapid, sensitive, environmentally-friendly and suitable for the analysis of BTEXs migration amount in blender.
Key words: dynamic headspace; blender; BTEXs; migration amount
长药八宝中酚酸类化合物的分离和含量测定
尹秀梅a，张敬东b，金慧娟c，王思宏*b, c，李东浩c
（延边大学 a. 药学院，b. 延边大学测试中心，c. 延边大学长白山生物资源与功能分子教育部重点实验室，吉林 延吉 133002）
摘要：首次对长药八宝中的化学成分进行了物质分离，分离出反式对羟基肉桂酸、顺式对羟基肉桂酸、异香草酸、对羟基苯甲酸和没食子酸这5种化合物。采用紫外光谱法对长药八宝中的反式对羟基肉桂酸、对羟基苯甲酸和没食子酸进行了定量研究。
关键词：长药八宝；酚酸类化合物；分离；波谱测定；紫外光谱；含量测定
中图分类号：R284.1 文献标识码：A 文章编号：0258-3283（2018）
Isolation and Content Determination of Phenolic Acids in HylotelephiumSpectabile (Bor.) H. Ohba YIN Xiu-meia, ZHANG Jing-dongb, JIN Hui-juanc, WANG Si-hong*b,c, LI Dong-haoc (a. College of Pharmacy, b. Analysis and Inspection Center, c. Key Laboratory of Natural Resource of the Changbai Mountain and Functional Molecules, Ministry of education, Yanbian University, Yanji 133002, China), Huaxue Shiji, 2018, 40(4)
Abstract: The chemical composition of Hylotelephiumspectabil (Bor.) H. Ohba was investigated, 5 known compounds：trans p-hydroxycinnamic acid, cis p-hydroxycinnamic acid, isovanillic acid, p-hydroxybenzoic acid, gallic acid were isolated. The content of trans-cinnamic acid, p-hydroxybenzoic acid and gallic acid were determined by ultraviolet spectroscopy. These substances were the basis for the antioxidation of H. spectabil.
Key words: Hylotelephiumspectabile (Bor.) H. Ohba; phenolic acids; isolation; spectroscopic measurement; ultraviolet spectrophotometry; content determination
共振光散射光谱法测定异烟肼的研究
朱梦a,b, 李倩a,b, 梁艳b,c, 马卫兴* b,c
（ 淮海工学院 a. 化学工程学院，b .药学院，c . 江苏省海洋药物筛选重点实验室，江苏 连云港 222005）
摘要：在pH 4.10的 B-R缓冲溶液中，利用异烟肼与过量的Fe3+先发生氧化还原反应，剩余的Fe3+再和4-(2-吡啶偶氮)-间苯二酚 (PAR)之间发生配位反应而生成配合物。异烟肼的加入使生成的配合物减少，从而引起体系的共振光散射信号显著减弱。在325 nm处减弱的共振光散射信号强度DI与浓度在0.05 ～ 0.30 μg/mL范围内的异烟肼呈现良好的线性关系，由此建立了一种新的检测异烟肼含量的共振光散射光谱（RLS）分析方法。线性回归方程为DI = 14879.7c (μg/mL) +448.6，相关系数(r)为0.9996，检测限(L=3d/S)为0.0135 μg/mL。所拟方法成功应用于异烟肼片的测定，结果与药典法一致。
关键词：异烟肼；4-(2-吡啶偶氮)-间苯二酚；共振光散射光谱法
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283(2018)
Determination of Isoniazid by Resonance Light Scattering Spectrometry ZHU Menga,b, LI Qiana,b , LIANG Yanb,c, MA Wei-xing*b,c (a. School of Chemical Engineering, b. School of Pharmacy, c.Jiangsu Key Laboratory of Marine Pharmaceutical School Screening, Huaihai Institute of Techology, Lianyungang 222005, China), Huaxue Shiji, 2018, 40(4)
Abstract： In the B-R buffer solution at pH value of 4.10, a novel resonance light scattering (RLS) analytical method of isoniazid was developed based on the redox reaction of isoniazid and excess Fe3+，then the complex reaction of remainingFe3+ with 4- (2-pyridylazo) –resorcinol(PAR) to form complexes. The addition of isoniazid reduced the formed complex, which resulting in a significant decrease of the resonance light scattering signal. The resonance light scattering signal intensity DI weakened at 325 nm showed a good linear relationship with the concentration of isoniazid in the range of 0.05 ～ 0.30 μg/mL. The linear regression equation was DI=14879.7C (μg/mL)+448.6. The correlation coefficient (r) was 0.9996. The limit of detection (L=3d/S) was 0.0135 μg/mL. The proposed method has been applied to the determination of isoniazid tablets with satisfactory results, which are in agreement with those obtained by the pharmacopoeia method.
Key words: isoniazid; 4- (2-pyridylazo)-resorcinol; resonance light scattering spectroscopy
电感耦合等离子体质谱法同时分析食盐中24种元素
汪勇，姚婷*，孙秉康，张轩
（黄山学院分析测试中心，安徽黄山245041）
摘要：采用电感耦合等离子体质谱（ICP-MS）仪同时准确测定食盐中Be（铍）、Mg（镁）、Al（铝）、Ca（钙）、V（钒）、Cr（铬）、Mn（锰）、Fe（铁）、Co（钴）、Ni（镍）、Cu（铜）、Zn（锌）、Ga（镓）、As（砷）、Se（硒）、Rb（铷）、Sr（锶）、Ag（银）、Cd（镉）、Cs（铯）、Ba（钡）、Hg（汞）、Tl（铊）、Pb（铅）共24种元素的含量。样品用2%硝酸溶解后，使用ICP-MS测定上述元素，以内标法消除基质效应等干扰，以不同梯度标准曲线分段计算元素含量。结果表明，24种元素在0～200 μg/L的范围内线性关系良好，相关系数R2均大于0.991，检出限（LOD）为0.0011～1.5316μg/L，定量下限（LOQ）为0.0038～5.1053μg/L，加标回收率为83.18 % ～126.53%，相对标准偏差（RSD）<8%。该方法前处理简单，分析速度快，灵敏度和准确度高，适用于食盐中多种元素的含量测定，为食盐的质量监控提供了参考依据。
关键词：电感耦合等离子体质谱；食盐；元素；分析
中图分类号：O657.63文献标识码：A
Determinations of 24 Elements in Saltby Using Inductively Coupled Plasma Mass SpectrometryWANG Yong,YAO Ting*, SUN Bing-kang, ZHANG Xuan（Analysis and Testing Center，HuangshanUniversity，Huangshan 245041，China）
Abstract：An analytical method was developed for the content of 24 kinds of elements(Be, Mg, Al, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se,Rb,Sr,Ag,Cd,Cs,Ba,Hg,Tl,Pb)in table salt at the same timeby inductively coupled plasma mass spectrometry (ICP-MS). After the samples were dissolved with 2 % HNO3, the above elements were determined by ICP-MS, and the matrix effects were eliminated by theinternal standard method, and the content of elements were calculated by the different gradient standard curves.The experimental results indicated that the elements had good linear relationships (R2>0.991) in the range of 0 ~ 200 μg/L.Thelimitsof detection (LOD)were in the range of 0.0011 ~ 1.5316μg/Land the limitsof quantitation (LOQ) were 0.0038~5.1053μg/L.Thespiked recoverieswere between 83.18% and 126.53%,withthe relative standard deviations (RSDs) less than 8%.This method wassimple, fast, sensitiveandaccuratewhich was suitable for determination of various elements in table salt.It provided reference for the quality monitoring of table salt.
Key Words：inductively coupled plasma mass spectrometry; table salt; element; determinations
抗风湿类中成药中保泰松的快速筛查研究
陈梓云*，姚婉清，彭梦侠
（嘉应学院 化学与环境学院，广东 梅州 514015）
摘要：对抗风湿类中成药中添加保泰松的快速筛查方法进行了研究。以15种市售抗风湿类中成药为研究对象，采集研究样品的红外光谱图（FT-IR），同时结合TQ Analyst 9.0软件，通过判别分析法（Discriminant Analysis）建立了抗风湿类中成药中保泰松的快速筛查模型。用此模型检测了另外15种市售抗风湿类中成药，结果表明其阴性样品和阳性样品的识别正确率为100%，误判数为0。
关键词：抗风湿类中成药；保泰松；红外光谱；快速筛查
中图分类号：O657.33 文献标识码：A 文章编号：0258-3283（2018）
Rapid Screening of Phenylbutazone in Anti-rheumatic Chinese Medicine CHEN Zi-yun*, YAO Wan-qing, PENG Meng-xia (School of Chemistry and Environment，Jiaying University，Meizhou 514015，China), Huaxue Shiji, 2018, 40(4)
Abstract: The method of rapid screening of phenylbutazonein anti-rheumatic Chinese medicine was investigated. Taking15 kinds of anti-rheumatic Chinese medicines as the object, the recognition model of phenylbutazone was established using FTIR combined with discriminant analysis. The model was used to detect the 15 samples, and the results showed that the correct recognition rate of model was 100%, and the miscarriage of justice was 0.
Key words: anti-rheumatic Chinese medicine; phenylbutazone; FTIR; rapid screening
新型苯环5位修饰甲磺隆类似物的合成及除草活性研究
石慧慧1，王美怡*1,2，李正名3
（1. 北方民族大学 化学与化学工程学院，宁夏 银川 750021；
2. 天津科技大学 化工与材料学院，天津 300457；
3. 南开大学 元素有机化学研究所，天津 300071)
摘要：为开发新型苯环5位取代的苯磺酰脲类化合物，以甲磺隆为前体，保持三嗪环不变，合成了8个新型苯环5位取代甲磺隆类似物。经1HNMR及高分辨质谱确证了结构，经油菜平皿法和盆栽法测试了其生物活性。结果表明，经苯环5位取代基改造后，除草活性与甲磺隆相比均有所降低。当5位取代基位为三氟乙酰胺基或乙酰胺基时，除草活性较好；当5位取代基为体积更大的取代苯甲酰胺基时，活性降低的更多。
关键词: 磺酰脲；苯环5-取代；合成；除草活性
中图分类号： O625.7 文献标识码：A
Synthesis and Herbicidal Activity of Analogues ofMetsulfuron-methyl Modified at 5-Position of Benzene Ring SHI Hui-hui1, WANG Mei-yi*2，LI Zheng-ming3(1. College of Chemistry and Chemical Engineering,Beifang University of Nationality, Yinchuan 750021, China; 2. College of Chemical Engineering and Materials Science, Tianjin University of Science & Technology , Tianjin 300457, China; 3. Research Institute of Elemento-organic Chemistry, Nankai University, Tianjin 300071, China)
Abstract:In order to investigate the bioactivity of novel sulfonylurea, 8benzenesulfonylurea derivativesmodified at the 5-position of the benzene ring were synthesizedbased on the precursor of metsulfuron-methyl. The structures of all compounds were confirmed by 1HNMR and HRMS．Herbicidal activity of these new compounds was determined by rape disc and pot bioassay experiments.The resultindicatedwhen the 5-position of the benzene ring wasmodified, the herbicidal activity was decreased in comparisonwith metsulfuron-methyl. The herbicidal activity was relatively good when the 5 substituent istrifluoroacetamide or acetamide. The activity decreased more when the 5 substituent was replaced by a larger volume, such as substituted benzamides.
Key words: sulfonylurea; benzene 5-substitued;synthesis; herbicidal activity
3-氨基-1,2,4-三氮唑的锌金属配位聚合物的
合成与晶体结构
周柯，岳凡*，张善蕊，陈华梅，王吉德
(新疆大学 石油天然气精细化工教育部和自治区共建重点实验室，新疆 乌鲁木齐 830046)
摘要：以3-氨基-1, 2, 4-三氮唑为主配体，烟酸为结构调整剂，采用溶剂热法，控制三唑与酸的物质的量比为1:1，合成了锌的金属配位聚合物{[(C2H3N4)7(H2O)2(μ-O) Zn6]·3NO3·3H2O}n。采用单晶衍射、XRD、热重分析、红外光谱、荧光分析等对其进行表征。结果表明该配合物属于六方晶系，R-3空间群，晶胞参数: a = 20.980(15) Å、b = 20.980(15) Å、c = 25.693(16) Å、γ = 120°，最终偏离因子 R1 = 0.0636、wR2 = 0.1593。生成的配位聚合物有较强的荧光强度。
关键词: 3-氨基-1,2,4-三氮唑；烟酸；配位聚合物；晶体结构
中图分类号: O635. 2 文献标识码:A 文章编号：0258-3283（2018）
Syntheses and Crystal Structures of Zinc (II)Coordination Polymer with 3-Amino-1,2,4-triazole ZHOU Ke, YUE Fan*, ZHANG Shan-rui, CHEN Hua-mei, WANG Ji-de (Key Laboratory of Oil and Gas Fine Chemicals, Ministry of Education ＆ Xinjiang Uyghur Autonomous Region, Xinjiang University, Urumqi 830046, China)
Abstract:In this work, 3-amino-1,2,4-triazole as the main ligand, nicotinic acid as the chemical agents for structural adjustment. The proportion of triazole and acid was controlled for 1:1. Zn(II) coordination polymer{[(C2H3N4)7(H2O)2(μ-O) Zn6]·3NO3·3H2O}n has been synthesized by solvothermal method. It was confirmed by X-ray-single-crystal diffraction, powder XRD, thermo-gravimetric analysis,infrared spectrum and fluorescent analysis. It belongs to thehexagonal crystal, R-3 /n space group with a = 20.980(15) Å, b = 20.980(15) Å, c = 25.693(16) Å, γ= 120°;R1 = 0.0636, wR2 =0.1593. The compound have high fluorescence intensity.
Key words: 3-Amino-1,2,4-triazole; nicotinic acid; coordination polymer;crystal structure
一类黄酮糖苷类化合物的合成及其α-葡萄糖苷酶抑制活性研究
薛向南1, 2, 3，曾晓萍2, 3，童洋1, 2, 3，韦可心1, 2, 3，梁光义2, 3，徐必学*2,3
(1. 贵阳中医学院 药学院，贵州 贵阳 550002；
2. 贵州医科大学 省部共建药用植物功效与利用国家重点实验室，贵州 贵阳 550014；
3. 贵州省中国科学院天然产物化学重点实验室，贵州 贵阳 550014)
摘要：以芦丁为原料合成了5个黄酮糖苷类化合物，并经ESI-MS、1HNMR及13CNMR确证其结构。以阿卡波糖为阳性对照测试了所合成的目标产物对α-葡萄糖苷酶的抑制活性，发现该类化合物中3位和5位羟基上取代烷基的链长对α-葡萄糖苷酶的抑制活性有一定影响，其中前4种化合物在检测浓度为1 × 10-4 mol/L的抑制率分别为(29.00±2.58) %、(33.53±4.92) %、(36.51±5.32) %、(37.34±3.54) %，而当3, 5, 3', 4'位羟基全部烷基化后所得衍生物的活性消失。这将为该类化合物在降糖活性方面的深入研究提供参考。
关键词：黄酮糖苷；合成；α-葡萄糖苷酶；抑制活性
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283(2018)
Synthesis of Flavonoid Glycosides and α-Glucosidase Inhibitory Activities XUE Xiang-nan1,2,3, ZENG Xiao-ping2,3, TONG yang1,2,3, WEI Ke-xin1,2,3, LIANG Guang-yi2,3, XU Bi-xue*2,3 (1. Guiyang College of Traditional Chinese Medicine, Guiyang 550002; 2. State Key Laboratory of Functions and Applications of Medicinal Plants, Guizhou Medical University, Guiyang 550014; 3. The Key Laboratory of Chemistry for Natural Products of Guizhou Province and Chinese Academy of Sciences, Guiyang 550014)
Abstract: Five flavonoid glycosides were synthesized starting from rutin and the structures were confirmed by 1HNMR, 13CNMR and MS. The inhibitory activities of those compounds against α-glucosidase were evaluated in vitro. The results showed that the different alkyl groups substituted in 3- or 5-hydroxyl group had a certain effect on the inhibitory activities against α-glucosidase. The inhibition rate of four compounds was (29.00±2.58)%, (33.53±4.92) %, (36.51±5.32)%, (37.34%±3.54)%, respectively, and another compound exhibited no activity when the 3,5,3',4'-hydroxyl groups were peralkylated. This work may provide a reference for the studies on the hypoglycemic activity of flavonoid glycosides.
Key words: Flavonoid glycosides; Synthesis; α-Glucosidase; Inhibitory activity
新型二茂铁取代的香豆素衍生物的合成及其清除自由基的研究
孟宪娇，曹端林,李生玲，马文兵*
（中北大学，化学工程与技术学院，山西 太原，030051）
摘要：合成了未见文献报道的二茂铁取代的香豆素衍生物(FLC)，采用FT-IR，1HNMR，13CNMR和ESI-MS对其结构进行表征，利用紫外-可见分光光度法对比研究了FLC及与其类似结构的呋喃香豆素(FNC)对DPPH自由基、ABTS自由基和Galvinoxyl自由基的清除活性。结果表明，两种药物均不具有捕获Galvinoxyl自由基的能力；对DPPH自由基具有较好的清除能力；在捕获ABTS自由基能力测试中，化合物FNC的抗氧化效果优于化合物FLC。
关键词：二茂铁；香豆素；抗氧化
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283(2018)
Synthesis and Free Radical Scavenging Abilities of Novel Ferrocenyl Substituted Coumarin Derivatives MENG Xian-jiao, CAO Duan-lin, LI Sheng-ling, MA Wen-bing*（School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, China）, Huaxue Shiji, 2018, 40(4)
Abstract: One new ferrocenyl substituted coumarin derivative (FLC) was designed and synthesized for the first time, and its structure was characterized by FT-IR, 1HNMR, 13CNMR and ESI-MS. The antioxidant activities were determinate with DPPH, ABTS and Galvinoxyl radicals by ultraviolet-visible spectrophotometry, comparing with furan coumarin (FNC) containing similar structure. The results showed that two kinds of compounds were non-effective in scavenging Galvinoxyl radical, and have a good ability to scavenging DPPH radical, and while the compound FNC exhibited more obviously antioxidant activity than compound FLC against ABTS radical.
Key words: ferrocenyl; coumarin; antioxidant
茄酮草酸酯的合成及其在卷烟加香中的应用
白冰，刘崇盛，惠志铮，张改红，毛多斌*
(郑州轻工业学院 食品与生物工程学院，河南 郑州 450000)
摘要：为了改善茄酮在卷烟加香中的稳定性，以茄酮为原料，经过羰基保护、硼氢化-氧化反应、酯化反应合成了新型烟用香料茄酮草酸酯，利用质谱、核磁共振、元素分析对目标产物结构进行了表征。采用在线热裂解-气相色谱-质谱联用对目标产物的热裂解产物进行了分析，并对茄酮草酸酯在卷烟中的加香作用进行了研究。结果表明，目标产物能够改善茄酮不稳定，易挥发的缺点，其主要裂解产物是对卷烟有积极贡献的茄酮，且裂解越高裂解产物越多；目标产物加入卷烟，可以显著提高香气质量、降低刺激性以及改善余味。
关键词：茄酮；草酸酯；热裂解
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283(2018)
Synthesis of Solanone Oxalate and Its Application to Cigarette Flavoring BAI Bing, LIU Chong-sheng, HUI Zhi-zheng, ZHANG Gai-hong, MAO Duo-bin* (School of Food & Biological Engineering, Zhengzhou University of Light Industry, Zhengzhou 450000, China), Huaxue Shiji, 2018, 40(4)
Abstract：Solanone oxalate was synthesied from solanone via ketalization, hydroboration-oxidation reaction, esterification in order to improve stability of solanone. Its structure was confirmed by MS, NMR, elemental analysis. Pyrolysis products of the title compound was studied by means of pyrolysis-GC-MS. The effect of the title compound on flavor of cigarettes by smoking was preliminarily evaluated．The results showed that the title compound is more stable and less volatile compare with solanone, and its mainly pyrolysis product is solanone. The title compound had the functions of enhancing aroma quality and quantity of cigarette smoke, reducing irritancy and improving aftertaste.
Key words：solanone; oxalate; pyrolysis
3′, 5′—二氨基脱氧核苷的新合成方法
孙亚伟*，程童，姬燕云
(中国石油大学 化学工程学院，山东 青岛 266580)
摘要：以商业化的2′-脱氧核苷为原料，经过两步Mitsunobu反应得到构型保持的3′和5′端叠氮取代的脱氧核苷，并通过一步Staudinger还原反应，以较高收率制备得到构型保持的3′, 5′-二氨基脱氧核苷。该方法采用安全性较好的叠氮磷酸二苯酯作为叠氮源来取代叠氮化钠，实现了叠氮化合物的制备，以三苯基膦作为还原剂实现对叠氮的原位还原，避免了强腐蚀性和剧毒易爆原料的使用以及叠氮化合物的分离，以高效、简洁的操作实现了目标分子的制备，为安全高效地大规模生产该类化合物提供了新的方法。
关键词：3', 5'-二氨基脱氧核苷；2'-脱氧核苷；Mitsunobu反应；Staudinger还原反应
中图分类号：O629.74 文献标识码：A 文章编号：0258-3283（2018）
A New Synthesis Method of 3’, 5’ –Diaminedeoxynucleoside SUN Ya-wei*, CHENG Tong, JI Yan-yun (College of Chemical Engineering, China University of Petroleum, Qingdao 266580,China)
Abstract：A new synthesis method of 3’, 5’ –diaminedeoxynucleoside was reported by using 2’-deoxynucleoside as the starting material, two Mitsunobu reaction and one Staudinger reduction was utilized to obtained the configuration maintained 3’, 5’ –diaminedeoxynucleoside. The hydroxyl group on 2’-deoxynucleoside was transfer to azide group by two subsequent Mitsunobu reaction, with the ribose’s configuration unchanged. In our research, the non-explosive diphenylphosphorylazide was utilized as azide source to replace toxic sodium azide, avoiding the use of hazard chemicals. The triphenylphosphine was chosen as reductant to turn azide to amine without the separation of azide containing compounds. The whole process is easy to handle and no toxic or explosive reagents was used, provides us new choice in 3’, 5’ –diaminedeoxynucleosides’ synthesis.
Key words：3’, 5’ -diaminedeoxynucleoside; 2’-deoxynucleoside; Mitsunobu reaction; Staudinger reduction
磺酸基功能化的介孔材料HSO3-Zr-La-SBA-15的制备
刘婧*1, 2，杨武2，毛学荣3，薛瑞2，郭昊2
（1. 甘肃农业职业技术学院 食品化工系，甘肃 兰州 730020；2. 西北师范大学 化学化工学院，甘肃 兰州 730070；
3. 荆楚理工学院 化工与药学院，湖北 荆门 448000）
摘要：介孔材料具有孔径均匀且可调、比表面积高、形貌可控，表面可功能化以及孔道结构规则有序等特点，在很多传统的微孔沸石及分子筛都难以完成的在大分子的吸附、分离，特别是催化等领域有着非常广泛的应用。本文在没有加任何无机酸的情况下，水热法一步制备了双金属掺杂的介孔材料Zr-La-SBA-15 (ZLS)，接着以3-巯丙基-三甲氧基硅烷为有机功能试剂，通过采用后接枝法合成了磺酸基功能化的介孔材料HSO3-ZLS，并通过小角X-射线衍射(SXRD)、氮气吸附-脱附、红外光谱(IR)、透射电镜(TEM)和热重(TG)等分析方法进行了详细地表征。结果表明，修饰后的样品依然保持了SBA-15有序二维六方相介孔结构，且比表面、孔容较大，孔径分布较窄，热稳定性较高。
关键词：介孔材料；功能化；合成
中图分类号：O69 文献标识码：A 文章编号：0258-3283（2018）
Preparation of Sulfonic-functionalized Mesoporous Materials HSO3- Zr-La-SBA-15 LIU Jing *1,2，YANG Wu1，MAO Xue-rong3，XUE Rui1，GUO Hao1(1. Department of Food and Chemical Engineering，Gansu College of Agriculture Technology，Lanzhou，Gansu730020，China; 2. College of Chemistry and Chemical Engineering，Northwest NormalUniversity，Lanzhou，Gansu730070，China; 3.College of Chemical Engineering and pharmacy，Jingchu University of Technology，Jingmen，Hubei 448000，China)
Abstract: Due to uniform and adjustable pore size, high surface area, well-controlled morphology, and easily functionalized surface, as well as regular and ordered channel structures, mesoporous materials have been used in various fields such as absorption, separation, especially catalysis of macromolecules, which are usually difficult to be finished by classical microporous zeolite or molecular sieves. In this paper, the bimetallic mesoporous materials Zr-La-SBA-15(ZLS) were synthesized by a one step hydrothermal route, without addition of mineral acids, then sulfonic-functionalized HSO3-ZLS mesoporous materials were synthesized by a post-grafting procedure using 3-mercaptopropyl trimethoxysilane as organic modifiers, and their structures and physicochemical properties were characterized by SXRD, N2 adsorption-desorption isotherm techniques, IR, TEM and TG. The results indicated that the synthesized materials still maintained ordered mesoporous of two-dimensional hexagonal channel structure，very large specific surface area and pore volume，narrow pore size distribution，high thermostability.
Keywords: mesoporous materials; functionalization; synthesis
meso-苯基-4-吡啶基取代卟啉混合物的合成规律研究
赵文伯，路沛贤，邓亚茹，秦会安*
（郑州师范学院 化学化工学院，河南 郑州 450044）
摘要：以苯甲醛、4-吡啶甲醛、吡咯为原料，同时合成6种卟啉化合物，通过改变溶剂、反应物浓度、反应时间、氧化剂用量和原料比例等反应条件，探讨了meso-苯基-4-吡啶基取代卟啉混合物的合成规律。经研究发现，在70 mL V(乙酸)︰V(丙酸) = 1 : 1、10 mL硝基苯、反应温度为110 ℃、反应物浓度为0.2 mol/L、反应时间为1.5 h条件下，当n(苯甲醛)︰n(4-吡啶甲醛) = 1 : 7 ~ 7 : 1之间，卟啉的总收率在23.4% ~ 31.2%；当n(苯甲醛)︰n(4-吡啶甲醛) = 1 : 7时，5-（4-吡啶基）-10，15，20-三苯基卟啉的最高选择性为24%，5, 10-二（4-吡啶基）-15, 20-二苯基卟啉的最高选择性为15%；当n(苯甲醛)︰n(4-吡啶甲醛) = 7 : 1，5, 15-二（4-吡啶基）-10, 20-二苯基卟啉的最高选择性为25%，5, 10, 15-三（4-吡啶基）-20苯基卟啉的最高选择性为31%。
关键词：meso-苯基-4-吡啶基取代卟啉；合成规律；原料比例
中图分类号：O625.6 文献标识码：A 文章编号：0258-3283（2018）
Synthesis Rules of Meso-porphyrins Substituted by Phenyl and 4-Pyridyl Groups ZHAO Wen-bo, LU Pei-xian, DENG Ya-ru, QIN Hui-an* (College Chemistry and Chemical Engineering, Zhengzhou Normal University, Zhengzhou 450044)
Abstract：In this work, six kinds of porphyrins were synthesized by using benzaldehyde, 4-pyridinecarboxaldehyde and pyrrole as raw materials. It is discussed about the synthesis regulation of meso-phenyl-4-pyridyl substituted porphyrins.Mainly related to the kinds of solvent, the concentration of reactants, reaction time, the amount of oxidant and the proportion of raw materials. Under the condition of 70 mL of acetic acid and propionic acid mixed solvent (volume ratio of 1: 1), 10 mL of nitrobenzene, reaction temperature of 110 ℃, reactant concentration of 0.2 mol/L and reaction time of 1.5 h,the total yield of porphyrin was between 23.4% and 31.2% when the ratio of benzaldehyde to 4-pyridinecarboxaldehyde was between 1 : 7 and 7 : 1. When the ratio of benzaldehyde to 4-pyridinecarboxaldehyde is 1 : 7, the highest selectivity of 5- (4-pyridyl) -10,15,20-triphenylporphyrin and 5,10-bis (4-pyridyl) -15,20-diphenylporphyrin was 24% and 15%,respectively. When the ratio of benzaldehyde to 4-pyridinecarboxaldehyde was 7 : 1,the highest selectivity of 5,15-bis (4-pyridyl)-10,20-diphenylporphyrin and 5,10,15-tris (4-pyridyl) -20 phenylporphyrin was 25% and 31%, respectivity.
Keywords：meso-phenyl-4-pyridyl substituted porphyrin; synthesis rule; raw materials proportion
负载型阳离子交换树脂催化合成匹多莫德
张文雯*，叶爱英，陈绘如
（常州工程职业技术学院制药与生物工程技术系，江苏常州213164）
摘要：以L-半胱氨酸为原料合成L-噻唑烷-4-甲酸后，与L-焦谷氨酸在负载型阳离子交换树脂催化下合成匹多莫德。研究了以负载ZnCl2的凝胶型低交联度大交换量的阳离子交换树脂为催化剂合成匹多莫德的工艺条件。结果表明，L-焦谷氨酸与L-噻唑烷-4-甲酸的物质的量比为1.16，以DMF为溶剂，催化剂用量为总物料的15.9%，在70℃反应2h，匹多莫德总收率达69%，催化剂可重复使用。
关键词：匹多莫德；负载型；阳离子交换树脂；催化剂；合成
中图分类号：O626.2文献标识码：Ａ文章编号：0258-3283（2018）
Pidotimod Synthesis Catalyzed byMetal Ions Loaded Cation Exchange Resin ZHANG Wen-wen, YE ai-ying,CHEN Hui-ru(Institute of Pharmaceutical and Environmental Engineering, Changzhou Vocational Institute of Engineering, Changzhou 213164)
Abstract: Started from L-cysteine to afford (R)-thiazolidine-4-carboxylic acid, which reacted with L-pyroglutamic acid to obtain pidotimod catalyzed by loaded cation exchange resin. The reaction conditions were investigated with ZnCl2-loaded geltype, low crosslinking degree and high exchange capacity cation exchange resin as catalyst. Results reveal that the optimum reaction conditions was as follows: molar ration of L-pyroglutamic acid to (R)-thiazolidine-4-carboxylic acid 1.16, DMF as solvent, catalyst amount 15.9% of total material, reaction temperature 70 ℃，reaction time 2h. The total yield reached 69% and catalyst can be reused.
Keywords: pidotimod;loading;cation exchange resin;catalyst;synthesis
2,3-二氢-5-甲氧基-螺[1H-茚-1,2’-吡咯烷]的合成研究
赵长阔，王先恒*，徐浪，曹颖，黄梅，袁智
(遵义医学院 药学院，贵州 遵义 563099)
摘要:茚的含杂原子五员螺环结构是新药设计与天然产物结构修饰引入的重要活性片段。以3-甲氧基苯甲醛为起始原料，依次通过魏悌希反应延长碳链、催化氢化还原烯键、苯环溴代、克莱森缩合、重排、成环等6步反应得到标题化合物，总收率为19.6%。该研究为五员氮杂螺环衍生物的构效研究奠定了合成基础。
关键词:3-甲氧基苯甲醛；2,3-二氢-1H-茚；魏悌希反应；催化氢化；重排
中图分类号: O626.1 文献标志码: A 文章编号
Synthesis of 2,3-Dihydro-5-Methoxy-Spiro[1H-Indene-1,2’-Pyrolidine ZHAO Chang-kuo, WANG Xian-heng*, XU Lang, CAO Ying, HUANG Mei, YUAN Zhi (School of Pharmacy, Zunyi Medical University, Zunyi 563099,China
Abstract：The structure of 5-membered spiro heterocyclic of indene is an important active fragment which is widely used in new drug design and natural product structure modification.Starting from 3-methoxybenzaldehyde, the spirocyclicderivatives of 2,3-dihydro-1H-indene was synthesizedvia six steps, in turn with Wittig reaction to extending carbon cyclic chain, catalytic hydrogenation to reduce double bond, bromination on benzene ring, Claisen condensation, rearrangement and cyclization were obtained in two steps. Total yield of the targeted product was 24.5%. This workprovides a foundation for furtherresearch on structure-activity of these spiro heterocyclic compounds.
Keywords：3-methoxybenzaldehyde; 2,3-dihydro-1H-indene; Wittig reaction; catalytic hydrogenation；rearrangement
聚丙烯酰胺和pH双重调控合成单分散碳球
章平平，周佳，朱圣平，唐传球*
(汉江师范学院 生物化学与环境工程系，湖北 十堰 442000)
摘要：采用水热法，以葡萄糖为原料、聚丙烯酰胺和pH为双重调控剂，成功地制备出粒径在100 ～ 4500 nm之间的单分散微球，解决了水热条件下难以在较大范围内控制尺寸大小与分散性的问题。进一步通过扫描电镜（SEM）、X-射线光电子能谱仪(XPS）和红外光谱（FT-IR）对最终产物的形貌、组成进行表征。结果表明，碳球的分散性和粒径尺寸取决于聚丙烯酰胺的用量和反应体系的pH。在pH 12、聚丙烯酰胺浓度为1.0 g/L时，碳球分散性好、球形规则，最大粒径可达4500 nm。
关键词：聚丙烯酰胺；pH；粒径可控；碳球
中图分类号：O613.71 文献标识码：A 文章编号：0258-3283（2018）
Effect of Polyacrylamide and pH on Size-tunable Synthesis of Mono-disperse Carbon Spheres ZHANG Ping-ping, ZHOU Jia, ZHU Sheng-ping, TANG Chuan-qiu*（Department of Chemical, Biological and Environmental Engineering, Hanjiang Normal University, Shiyan 442000, China), Huaxue Shiji, 2018, 40(4)
Abstract: Mono-disperse carbon spheres with a tunable diameter of 100 ～ 4500 nm were synthesized using glucose as carbon sources with polyacrylamide and pH as controlling reagent, which also demonstrated the feasibility of controlling the size and dispersion of the carbon spheres under water thermal condition over a wide range. The morphology and composition of the carbon spheres were confirmed by SEM, XPS and FT-IR. The results show that the size and depressiveness of the carbon spheres were influenced by the solution of pH and the concentration of polyacrylamide. The largest sizes of carbon spheres was 4500 nm without damage to their morphology with the addition of 1.0 g/L polyacrylamide at pH 12.
Keywords: polyacrylamide; pH; tunable diameter; carbon spheres
超声波辅助下PPh3-I2共催化的室温Beckmann重排反应
赵春阳，董书达，尹钰芸，李昊，金城安，何静耀*
（绍兴文理学院 化学化工学院，浙江 绍兴 312008）
摘要：发展了超声波辅助下PPh3和I2共催化的室温Beckmann重排反应。首先，以二苯甲酮肟为底物对Beckmann重排反应条件进行了优化，结果表明：超声波辅助下，以10 mol% PPh3和10 mol% I2为催化剂，二氯甲烷为溶剂，二苯甲酮肟即可在室温下完成Beckmann重排反应（20 min），并以95%的分离收率得到N-苯基苯甲酰胺；然后，我们用其他的肟研究了超声波辅助下，PPh3和I2共催化的室温Beckmann反应的底物普适性。结果表明取代二苯甲酮肟、取代苯乙酮肟、吡啶乙酮肟都顺利进行Beckmann重排反应，并能以很好的产率得到产物。采用1HNMR、13CNMR、dept 135、dept 90、GC-MS等手段对9种Beckmann重排产物酰胺进行了全面表征，并测定了这些酰胺的Rf值和熔点。
关键词：Beckmann重排；超声波；碘催化；三苯基膦催化；酰胺合成
中图分类号：0622.4
Ultrasonic Assisted PPh3-I2Co-catalyzed Beckmann Rearrangement Reaction at Room Temperature ZHAO Chun-yang, DONG Shu-da, YIN Yu-yun, LI Hao , JIN Cheng-an (College of chemistry and chemical engineering , Shaoxing University, Shao Xing 312008)
Abstract：In this work, a room temperature Beckmann rearrangement reaction with the ultrasonic-assisted[1]was developed, which is catalyzed by PPh3 and I2.Firstly, the reaction conditions of Beckmann rearrangement were optimized with benzophenone oxime as a substrate. And the results showed that using 10 mol% PPh3 and 10 mol% I2 as the catalyst, dichloromethane as the solvent could help benzophenone oxime to complete the room temperature Beckmann rearrangement reaction (20 min) and obtain the N-phenylbenzamide at an isolated yield of 95%. Then, the other oximes were used to research the universality of the Beckmann rearrangement reaction’ substrateat room temperature. This work have shown that substituted benzophenone oxime, substituted acetophenone oxime and pyridine oxime successfully carried out the Beckmann rearrangement reaction and the product could be obtained in a very good yield.In the study, 9 kinds of Beckmann rearrangement products amides were fully characterized by 1HNMR, 13CNMR, dept 135, dept 90 and GC-MS and the Rf values and melting points of these amides were determined.
Keywords：Beckmann rearrangement reaction; ultrasound;catalyst I2;catalyst PPh3;amide synthesis
