富勒烯衍生物与抗癌药物分子连接的研究进展
王兴浩，刘文迎，张静*
（郑州大学 化工与能源学院，河南 郑州 450001）
摘要：富勒烯及其衍生物可广泛作为化学药物和基因药物的转运载体。把富勒烯与抗癌药物进行连接，可以改善疏水性药物的生物相容性，通过高通透性和EPR效应聚集在靶组织，而且得到的富勒烯衍生物具有富勒烯和抗癌药物的双重特性，提高了抗癌药物的活性和生物利用度。对富勒烯及其衍生物耦合脱氢枞胺、阿霉素、紫杉醇等抗癌药物的研究进展进行综述。
关键词：富勒烯衍生物；脱氢枞胺；阿霉素；紫杉醇；抗癌药物
中图分类号：TQ463 文献标识码：A 文章编号：0258-3283（2018）
Progress on the Connection between FullereneDerivatives and Anticancer Drugs WANG Xing-hao, LIU Wen-ying, ZHANG Jing* (College of chemical and energy, Zhengzhou University, Zhengzhou 450001, China)
Abstract：Fullerene derivatives can be widely used as the chemical drug and gene drug delivery vector. The fullerene and anticancer drug connection,not only can improve the biocompatibility of hydrophobic drugs, and gathered in the target tissuevia high pass and the EPR effect, and has dual characteristics of fullerene and the anticancer drug obtained fullerene derivatives, improve the activity and bioavailability of anticancer drugs. Progress of the fullerene connection dehydroabietylamine, doxorubicin, paclitaxel and other anticancer drugs were reviewed.
Key words：Fullerene derivatives; dehydroabietylamine; doxorubicin; paclitaxel; anticancer drugs
Mn掺杂g-C3N4的制备及其可见光催化研究
艾兵*，李思源，侯栋珺，李德刚
(山东理工大学 化学化工学院，山东 淄博 255049)
摘要：为研究可见光降解有机污染物以解决环境问题，以三聚氰胺为前驱体，采用热聚合法合成了类石墨相氮化碳(g-C3N4)光催化剂，并用同样的方法以掺入一定质量比例MnSO4的三聚氰胺为前驱体合成了Mn/g-C3N4复合光催化剂。使用XRD、UV-Vis DRS、FT-IR、SEM等对制备的光催化剂进行了表征。通过可见光催化降解亚甲基蓝(MB)探究了Mn的掺杂量对光催化活性的影响。研究结果表明，0.5 wt%的Mn掺杂效果最好，降解效率可达28.18%。最后，探究了亚甲基蓝浓度、催化剂用量、反应温度、循环使用次数对复合光催化剂催化性能的影响。
关键词：类石墨相；氮化碳；光催化；Mn掺杂
中图分类号：O649；O643 文献标识码：A 文章编号：0258-3283（2017）
Preparation and Visible-light Photocatalysis of Mn-doped Graphitic Carbon Nitride AI Bing*, LI Si-yuan, HOU Dong-jun, LI De-gang (School of Chemistry and Chemical Engineering, Shandong University of Technology, Zibo 255049, China)
Abstract：In this work, graphitic carbon nitride (g-C3N4) photocatalyst was prepared by using thermal polymerization method from melamine, aiming at efficiently degrading organic pollutants under visible light irradiation to resolve the environmental problems. Furthermore, the Mn/g-C3N4 composite photocatalyst was prepared by adding MnSO4 before the catalyst preparation. The samples were characterized by XRD, UV-Vis DRS,FT-IR and SEM. The content effects of Mn species on the photocatalytic activity was investigated by the degradation of methylene blue under visible light irradiation. Results showed that the photocatalytic activity could be significantly enhanced and the degradation efficiency could reach up to 28.18% when the mass fraction of Mn was 0.5 wt%. Finally, the effects of methylene blue concentration, catalyst dosage, and reaction temperature on photocatalytic activity, the recycling capability were investigated.
Key words：graphitic phase; carbon nitride; photocatalysis; Mn doping
三维有序大孔硅材料载体固定化脂肪酶研究
黄孝明*1，陈瑶2，田景芝1，郑永杰1
(1. 齐齐哈尔大学 化学与化学工程学院，黑龙江 齐齐哈尔 161006；
2. 齐齐哈尔市环境监测中心站，黑龙江 齐齐哈尔 161005)
摘要：以聚苯乙烯胶体晶体为模板，制备三维有序大孔硅材料（3DOM-SiO2）作为载体固定脂肪酶。分别考察了脂肪酶加入量、反应体系pH值、固定反应时间对固定化效果的影响。结果表明，3DOM-SiO2材料固定脂肪酶的最佳酶液加入量为200 mL/g，固定化最适宜pH值为7.0，最佳反应时间为5 h。固定化的脂肪酶在催化性能上与游离脂肪酶相比优势明显，最适宜反应温度提高到40 ℃左右，并且随温度变化酶活变化率低，热稳定性明显提高；脂肪酶固定化后对pH的敏感度降低，适应范围更宽，催化反应的最适pH值为8.0；固定化脂肪酶重复使用8次后，相对酶活保持在62%。由此可见，3DOM-SiO2材料是固定脂肪酶优良载体，在酶固定化领域应用前景广阔。
关键词：三维有序大孔硅材料；固定化；脂肪酶
中图分类号：Q81；O69 文献标识码：A 文章编号：0258-3283（201*）
Immobilized Lipase of Three-dimensionally Ordered Macroporous Silica Material Carrier HUANG Xiao-ming*1, CHEN Yao2, TIAN Jing-zhi1, ZHENG Yong-jie1 (1.College of Chemistry and Chemistry Engineering Qiqihar University, Qiqihar 161006, China; 2. Environment Monitoring Center Station of Qiqihar City, Qiqihar 161005, China)
Abstract：Three-dimensionally ordered macroporous silica material (3DOM-SiO2) were prepared by polystyrene colloidal crystal as template. 3DOM-SiO2 was used as a carrier to immobilize lipase. The effects of the amount of lipase, the pH value of the reaction system and the reaction time on the immobilization efficiency were investigated. The results showed that the optimum amount of immobilized lipase, pH and the reaction time were 200 ml/g, 7.0 and 5 h respectively. The immobilized lipase has obvious advantages over the free lipase in catalytic performance. The optimum reaction temperature is increased to about 40 ℃, and the change rate of enzyme activity is low and the thermal stability is improved obviously with temperature. The sensitivity of pH was reduced after lipase immobilization, and the adaptation range was wider. The optimum pH value of the catalytic reaction was 8.0. The relative activity was maintained at 62% after the immobilized lipase was reused 8 times. The above results show that the 3DOM-SiO2 material are an excellent carrier of immobilized lipase and have wide application prospect in the field of enzyme immobilization.
Key words：three-dimensionally ordered macroporous silica material; immobilized; lipase
钒取代多钨酸盐/中性红复合膜的制备及电致变色性能研究
付勇，钟坚强，杨艳艳*，曲小姝，韩晴晴
(吉林化工学院 化学与制药工程学院，吉林 吉林 132022)
摘要：采用层接层技术将Dawson结构钒取代型多酸K7P2W17VO62·18H2O（P2W17V）和有机染料中性红（NR）构筑成复合膜材料。利用紫外-可见吸收光谱、扫描电镜和循环伏安扫描对复合膜的形貌及氧化还原性质进行了表征，使用电化学工作站和紫外-可见吸收光谱联机对复合材料的电致变色性能进行了研究。通过数据得知，成功地将K7P2W17VO62·18H2O（P2W17V）和中性红复合，且复合材料具有良好的电致变色性能，光反差为14.68%，着色时间为6.63 s，褪色时间为3.26 s，最大着色效率达到222 cm2/C，实现了粉色到深蓝色之间的可逆颜色变化，以及可调颜色的电致变色。
关键词：电致变色；钒取代多钨酸盐；中性红；LbL法
中图分类号：O 61 文献标识码：A 文章编号：0258-3283（2018）
Preparation and Electrochromic Property of Vanadium Substituted Polyoxotungstate/Neutral Red Nanocomposite FU Yong, ZHONG Jian-qiang, YANG Yan-yan*, QU Xiao-shu, HAN Qing-qing (College of Chemistry and Pharmaceutical Engineering, Jilin Institute of Chemical Technology, Jilin 132022, China), Huaxue Shiji, 2018, 40(2)
Abstract: A electrochromic material based on K7P2W17VO62·18H2O（P2W17V） and neutral red was prepared by layer-by-layer (LbL) method. The characterization of the composite film was investigated by UV-Vis spectroscopy, scanning electron (SEM) and cyclic voltammograms. The electrochromic properties of the film were characterized via chronoamperometric and spectroelectrochemistry. The composite film shows adjustable colors and undergoes transitions from pink to darkblue, resulting in an optical contrast of 14.68 % and a coloration efficiency of 222 cm2/C. Furthermore, the switching times were 6.63 s for coloration and 3.26 s for bleaching.
Key words: electrochromic; vanadium polyoxotungstate; neutral red; layer-by-layer
四种典型表面活性剂对恩诺沙星荧光强度的影响研究
李军德a，孙娇b，宋吉英*b
（青岛农业大学 a.校医院，b.化学与药学院，山东 青岛 266109）
摘要：采用荧光光谱法探究了4种典型表面活性剂在不同因素条件下如pH值、表面活性剂用量、反应时间、反应温度等对恩诺沙星荧光强度的影响。结果表明，在最大激发波长277 nm，最大发射波长441 nm，体系溶液在pH 4 ～ 6范围的弱酸性环境下，表面活性剂浓度达到临界胶束浓度，30 ℃下反应2 h，阴离子表面活性剂十二烷基苯磺酸钠、阳离子型表面活性剂十六烷基三甲基溴化铵、非离子型表面活性剂吐温80、两性表面活性剂十二烷基二甲基甜菜碱对恩诺沙星的荧光强度都有增敏作用。其中十二烷基苯磺酸钠的增敏幅度最大，其次是十六烷基三甲基溴化铵，吐温80和十二烷基二甲基甜菜碱的增敏效果不明显。
关键词：恩诺沙星；荧光强度；十二烷基苯磺酸钠；十六烷基三甲基溴化铵；吐温80；十二烷基二甲基甜菜碱
中图分类号:O657 文献标识码: A 文章编号：0258-3283（2017）
Four Kinds of Typical Surfactant for Fluorescence Intensity of Enrofloxacin LI Jun-dea, SUN Jiaob, SONG Ji-ying*b (a. Hospital of Qingdao Agricultural University, b. College of Chemistry &Pharmacy, Qingdao Agricultural University, Qingdao 266109, China）, Huaxue Shiji, 2018, 40(1)
Abstract：In this work, effect of four typical surfactants under different factors on fluorescence intensity of enrofloxacin was investigated by fluorescence spectrometry. These factors included pH value, concentration of surfactant, reaction time and temperature. The results indicated that efficiency of surfactants was optimal when pH ranged from 4 to 6, concentration reached a critical micelle concentration, temperature was 30 ºC and reaction time was 2 h. The maximum value of excitation wavelength was 277 nm with corresponding emission peak located at 441 nm. Fluorescence intensity was also strengthened by anionic surfactant SDBS, cationic surfactant CTAB, nonionic surfactant Twain-80, ampholytic surfactant BS-12. The best was SDBS, followed by CTAB. Effect of Twain-80 and BS-12 was unapparent on fluorescence intensity.
Key words: Enrofloxacin; fluorescence intensity; sodium dodecyl benzene sulfonate(SDBS); cetyltrimethyl ammonium bromide(CTAB); Twain-80; dodecyl dimethyl betaine(BS-12)
灰尘鞋印化学增强技术的研究进展
田亚杰1，曾祥凯1，范贤涛1，崔佳*2，刘 晋2，王明直2，刘伟平2
（1.中国人民公安大学，北京 100038；2.公安部物证鉴定中心，北京 100038）
摘要：鞋印是最容易遗留在犯罪现场的一种痕迹物证，伴随着犯罪活动的全部过程，在案件侦查和检察诉讼中起着至关重要的作用。但犯罪现场发现的鞋印大部分由于形成鞋印的介质物质含量低，与客体背景反差小，无法直接照相提取。因此，法庭科学研究者探索出一系列光学、物理和化学增强提取方法。化学增强法提供了进一步获取鞋印细节特征的手段，进而促进更全面更可信的检验。目前灰尘鞋印国内外常用的化学增强技术有硫氰酸钾法、硫氰酸铵法、铁氰化钾法、2,2'-联吡啶法和pH指示剂法。总结了灰尘鞋印化学增强方法及其应用现状，并对其新的发展趋势予以展望。
关键词：灰尘鞋印；化学增强；承痕客体；犯罪现场
中图分类号：DF794.1 文献标识码：A 文章编号：0258-3283（2017*）
Progresses in the Chemical Enhancement of Dust Footwear Impressions Tian Yajie1, Zeng Xiangkai1,Fan Xiantao1,Cui Jia*2,Liu Jin2, Wang Mingzhi2, Liu Weiping2(1. People' s Public Security University of China,Biejing 100038,China; 2.Institute of Forensic Science, Ministry of Public Security, Beijing 10038,China)
Abstract:Footwear impression evidence is one of the most common forensic evidence types left at crime scenes,and can provide substantial informations relating to potential suspects. In criminal investigations it is often necessary to enhance weak,two-dimensional footwear impressions. Various chemical reagents were reported as being effective for the enhancement of dust footwear impressions,such as、2,2'-Dipyridyl、Potassium thiocyanide、Potassium Hexacyanoferrate、Ammonium thiocyanate、pH indicators.etc.The advance of research on the enhancement of dust footwear impressions were summarized,and the future and perspective research of dust footwear impressions enhancement was predicted in this work.
Key words:dust footwear impressions; chemical enhancement; substract; crime scene
呋虫胺关键中间体的合成研究进展
徐庆，冯高峰，金城安*
( 绍兴文理学院 化学化工学院，浙江 绍兴 312000)
摘要：呋虫胺是第三代新型烟碱类杀虫剂，具有高效、低毒、杀虫广谱等优点，广泛应用于各种农作物的病害虫防治。目前，国内外合成呋虫胺主要有3–羟甲基四氢呋喃衍生化法和3–氨甲基四氢呋喃衍生化法。然而，传统生产工艺存在绿色性差、收率低、三废多等缺点，严重限制了企业清洁化生产。改善反应的方向主要集中在关键中间体3–羟甲基四氢呋喃和3–氨甲基四氢呋喃的高效、绿色合成。综述了近几年来呋虫胺关键中间体3–羟甲基四氢呋喃和3–氨甲基四氢呋喃的研究进展，比较了各自路线的优缺点，并对其合成方法进行了展望。
关键词：呋虫胺；3–羟甲基四氢呋喃；3–氨甲基四氢呋喃；合成方法
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283（2018）
Progress in Synthesis of Significant Intermediates about Dinotefuran XU Qing, FENG Gao-feng, JIN Cheng-an* (College of Chemistry and Chemical Engineering, Shaoxing University, Shaoxing 312000, China), Huaxue Shiji, 2018, 40(2)
Abstract： As the third-generation neonicotinoid insecticide, dinotefuran with many advantages such as: high-efficiency, low-toxicity, great insecticide and so on, which is widely used in pest control. Nowadays, there are two main methods for the synthesis of dinotefuran: 3-hydroxymethyltetrahydrofuran and 3-aminomethyltetrahydrofuranderivatization reaction. However, there are lots of inferiorities in conventional manufacturing technology, such as: unfriendly environment, low yield, tremendous pollution, which are bad for cleaning production. Therefore, the green and efficient preparation methods for significant chemical intermediates of dinotefuran are focused. This work talks about the synthetic methods about significant chemical intermediates of dinotefuran : 3-hydroxymethyltetrahydrofuran and 3–aminomethyltetrahydrofuran. Comparation of the merits and shortcomings, and the prospect for synthesis methods are discussed.
Key words：dinotefuran; 3-hydroxymethyltetrahydrofuran; 3-aminomethyltetrahydrofuran; synthetic methods
卡尔·费休库仑滴定法准确定量有机纯物质中痕量水分杂质
杨菡1, 2，全灿* 2，金君素1，王海峰2，李红梅2，刘李亮2，孔金隆2，郝媛2
（1. 北京化工大学 化学工程学院，北京 100029；
2. 中国计量科学研究院，北京 100029）
摘要：以双酚A高纯物质为目标物，采用库仑法水分滴定仪和控温、控湿型手套箱，考察卡尔·费休库仑滴定法准确测量高纯双酚A中痕量水分杂质过程条件及环境等因素的影响，以提高有机高纯物质质量平衡法定值水平，降低水分杂质的不确定度分量。研究结果表明：环境湿度对痕量水分杂质的定量具有显著影响。环境湿度会导致仪器漂移升高，空白响应增大；环境湿度还会引起被测样品水分含量的变化。实验也考察了样品质量、搅拌时间等仪器参数的影响。当样品质量较小时，测量结果明显偏高，随着样品质量的增大，滴定时间随之增加，测量结果趋于稳定；搅拌时间对测量结果没有显著影响。实验使用固体水分含量标准物质对实验方法进行确证，实验结果稳定在其不确定度范围内。
关键词：有机高纯物质；痕量水分；双酚A；卡尔·费休库仑滴定法；环境湿度
中图分类号：O657.12 文献标识码：A 文章编号：0258-3283（2018）
Accurate Measurement of Trace Level Water Impurities in High Purity Organic Materials with Karl Fischer Coulometry YANG Han1，2, QUAN Can*2, JIN Jun-su1, WANG Hai-feng2, LI Hong-mei2, LIU Li-liang2, KONG Jin-long2, HAO Yuan2（1. College of Chemical Engineering, Beijing University of Chemical Technology, Beijing 100029, China; 2. National Institute of Metrology, Beijing 100029, China）, Huaxue Shiji, 2018, 40(1)
Abstract：This work investigated the influences of operating parameters & environmental conditions of Karl Fischer coulometry to accurately measure trace level water content in high purity organic materials with the example of bisphenol A by using coulometric titrator and glove box. The aim of this work was to improve the ability of mass balance approach of organic high purity materials and reduce the measurement uncertainty of water content. The results indicated that the environmental humidity had a significant effect on the quantification of trace level water content: the penetration of the environmental humidity could disturb the instrument drift value as well the background, and also interfere the water content in samples. The results also proved the effects of the operating parameters such as sample mass intake and stirring time: less sample mass caused much higher water content and the mixing time had no significant effect on the results. The established method was further verified with solid-matrix water content reference material and the results were stable within the range of uncertainty.
Key words：high purity organic material; trace level water content; bisphenol A; Karl Fischer coulometry; environmental humidity
新型固相微萃取膜的制备及其用于茶叶中
拟除虫菊酯的测定
申书昌*，邹明宇，刘艳萍，吕伟超
(齐齐哈尔大学 分析测试中心，黑龙江 齐齐哈尔 161006)
摘要：合成了聚硅氧烷改性聚乙二醇型聚氨酯，涂布于铝箔纸上制成固相微萃取膜，与气相色谱仪联用，测定了茶叶中联苯菊酯、甲氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯的残留量。样品经80 ℃水超声提取，固相微萃取膜富集，V（丙酮）︰V (正己烷) = 7 : 3溶剂洗脱后，用气相色谱（GC-ECD）检测，外标法定量。考察了萃取温度、萃取时间、盐用量对萃取效率的影响，选择最佳洗脱溶剂。在0.005 ～ 1.0 μg/mL范围内，5种农药的色谱峰面积与浓度呈良好的线性关系，相关系数（R2）分别为0.9985、0.9994、0.9989、0.9993和0.9991，方法检出限分别为为0.047、0.035、0.039 、0.034和0.031 μg·L-1。
关键词：固相微萃取膜；气相色谱；拟除虫菊酯农药；茶叶
中图分类号： O657.7 文献标识码：A 文章编号：0258-3283(2018)
Preparation of Solid Phase Microextraction Membrane and Determination of Pyrethroid Pesticides in Tea SHEN Shu-chang*，ZOU Ming-yu，LIU Yan-ping，LU Wei-chao (Analytical and Testing Center，Qiqihar University, Qiqihar 161006, China), Huaxue Shiji, 2018, 40(1)
Abstract: The silicone modified polyethylene glycol polyurethane solid phase microextractionmembrane on aluminum foil was prepared . Five pyrethroidpesticides, such as bifenthrin, fenpropathrin, cypermethrin, fenvalerate and deltamethrin in the tea were determined by membrane solid phase microextraction coupled with gas chromatography. The pyrethroid pesticides were extracted in 80℃ water and ultrasonicwave, enriched on solid phase microextractionmembrane, evaluated in acetone and n-hexane(V（ acetone）︰V ( n-hexane) = 7 : 3), determinated by GC-ECD, quantitated analysis byexternalst and ardcurve. The effects of the temperature , time and salt content on extraction ratio were investigated and the best elution solvent was chosen. In the range from 0.005-1.0μg.mL-1, the relationship between the peak area and concentration of bifenthrin, fenpropathrin, cypermethrin, fenvalerate and deltamethrin were linear. The correlation coefficients(R2) were 0.9985, 0.9994, 0.9989, 0.9993and 0.9991 respectively. The detection limits for five pyrethroid pesticides were 0.0471, 0.035, 0.039, 0.034 and 0.031 μg/L respectively.
Key words: solid phase microextractionmembrane; gas chromatography; pyrethroidpesticides; tea
五种LC-MS级试剂的技术指标及适应性检测方法
陈浩云1，凌芳*1，顾小焱1，蔡璇2，洪亚云2，赵红莉*2
(1.国药集团化学试剂有限公司，上海 200002；2.华东理工大学 化学与分子工程学院，上海 200237)
摘要：液相色谱-质谱联用（LC-MS）检测作为一种常规分析手段，对流动相试剂的纯度要求非常高。然而国产LC-MS色谱级试剂质量不够稳定，国内难以检索到公开的LC-MS级色谱试剂的技术标准，使得绝大部分科研实验室只能采用进口试剂。因此，建立公开透明的LC-MS级试剂技术指标以及产品分析检测方法意义重大。本文分析了国内外LC-MS色谱试剂生产现状，以甲醇为例，列出了国外LC-MS甲醇的技术指标，简要概括了各指标的检测方法。并以五种国产LC-MS级试剂-甲醇、乙腈、乙酸乙酯、正己烷、异丙醇为实验对象，建立了各试剂的LC-MS适应性检测分析方法，同时采用相应的进口LC-MS色谱试剂进行对照，证明了所建方法的可行性。
关键词：LC-MS级试剂；技术指标；检测方法；适应性检测
中图分类号: O657. 7 文献标识码: A 文章编号:
Suitability Test and Technical Indexes for Five Generally Used LC-MS Grade Solvents CHENHao-yun1, LING fang*1, GU Xiao-yan1, CAI Xuan2, HONG Ya-yun2, ZHAO Hong-li*2 (1.Sinopharm Chemical Reagent Co., Ltd, Shanghai 200002, China; 2. School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237,China)
Abstract: As a kind of widely used analysis method, liquid chromatography-mass spectrometry (LC-MS) requires mobile phase reagents with extremely high purity. However, the quality of domestic LC-MS grade reagents is not stable. And the absence of technical standards of domestic LC-MS chromatogram reagents has urged most research laboratories to use imported reagents. Therefore, to establish technical indexes and analysis methods of LC-MS grade reagents is of great significance. In this work, the current status of LC-MS grade reagents production both at home and abroad was analyzed. The technical indexes and analysis methods of imported LC-MS grade methanol were listed as an example. With five kinds of domestic LC-MS grade reagents (methanol, acetonitrile, ethyl acetate, n-hexane and isopropanol) as experimental object, the suitability test methods of these solvents were established. In addition, the test results of both domestic and imported reagents were compared, indicating the feasibility of the analysis methods proposed.
Key words:LC-MS grade solvent; technical indexes; analysis methods; suitability test
化学试剂甲苯中水分含量测定的能力验证
王豪*，袁丽凤，罗川，章再婷
(宁波出入境检验检疫局，浙江 宁波 315048)
摘要：为了解和提高国内实验室对液体化学试剂水分含量的检测技术水平，能力验证提供者（CNAS PT0031）组织了甲苯水分含量测定的能力验证活动，有18个省、市、自治区共48家实验室参加。介绍了能力验证计划的样品制备、均匀性和稳定性检验、以及基于稳健算法A迭代法结果统计和分析等实施过程，对各实验室采用的水分含量测试标准进行了统计和分析，提出了水分含量测定的技术建议。能力验证计划统计表明，满意的实验室有43家，占反馈总数的89.6%。
关键词：化学试剂；甲苯；水；能力验证；
中图分类号：O652.3 文献标识码：A 文章编号：
Proficiency Testing for Determination of Water Content in Toluene of Chemical reagent WANG Hao*, YUAN Li-feng, LUO Chuan, ZHANG Zai-ting (Ningbo Entry-Exit Inspection & Quarantine Bureau, Ningbo 315048)
Abstract: In order to investigate and improve the level of detection technology of water content in liquid chemical reagents of domestic laboratories, proficiency testing provider PT0031 (CNAS) has organized proficiency testing program of water content in toluene, 48 laboratories from 18 provinces/cities/municipals took part in the PT. This work introduces the implementation process of proficiency testing for determination of water content in toluene, including sample preparation, homogeneity and stability test, the results of statistics of iteration robust statistic technique and analysis,summarized and analyzed those of the different test standards which are widely used in the laboratories, put forward the technological suggestions for the improvement of the test quality of water content. Satisfactory results were obtained by 43 laboratories, amounting to 89.6% of the total participating laboratories.
Key words: chemical reagents; toluene; water; proficiency testing
HPLC法测定原料药尿素-13C及其有关物质含量
王帅1, 2，李虎林2，雷雯2，侯捷2，邱俊*2，任玉杰*1
(1. 上海应用技术大学 化学与环境工程学院，上海 201418；2. 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：采用COSMOSIL-C18色谱柱，以90%乙腈-水溶液为流动相，流速为1.0 mL/min，柱温为30 ℃，进样量为20 μL，检测波长为200 nm。建立了HPLC测定原料药尿素-13C及其有关物质含量的方法。尿素-13C原料药在3.2 ~ 4.8 mg/mL范围内线性关系良好（r = 0.9995），平均回收率为99.40%（RSD = 0.63%）；有关物质缩二脲在0.6 ~ 9.0 μg/mL范围内线性关系良好（r = 0.998），加标回收率为100.4%（RSD = 1.53%）。此方法简便、结果准确，可用于原料药尿素-13C及其有关物质含量的测定。
关键词：尿素-13C；有关物质；高效液相色谱；含量测定
中图分类号：R917 文献标识码：A 文章编号：0258-3283（2017）
Determination of Urea C13 and Its Related Substances by HPLC WANG Shuai1,2, LI Hu-lin2,3,4, LEI Wen2,3,4, HOU Jie2,3,4, QIU Jun*2,3,4, REN Yu-jie*1( 1.College of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2.Shanghai Engineering Research Center of Stable Isotope, Shanghai Research Institute of Chemical Industry; Shanghai 200062, China)
Abstract: To establish HPLC method for the content determination of urea C13 and its related substances. The detection was conducted by a UV detector at 200 nm with 90% acetonitrile solution as the mobile phase on a COSMOSIL-C18 column. The flow rate was 1.0 mL/min, the column temperature was 30 ℃ and the injection volume was 20 μL. The calibration curve was linear in the range of 3.2 ~ 4.8 mg/mL for urea C13 (r = 0.9995). The average recovery was 99.40% (RSD = 0.63%). It was linear in the concentration range of0.6 ~ 9.0 μg/mL for Biuret (r = 0.998), and the recovery was 100.4% (RSD = 1.53%). The method appeared to be simple, quick and specific, it was suitable for determination of urea C13 and its related substances in the drug substance.
Key words:Urea C13; related substance; HPLC; content determination
同时蒸馏萃取和超临界流体萃取两种方法研究卷烟主流烟气香气成分
崔婷惠1,2，唐石云1，刘春波1，何沛*1，朱瑞芝1，蒋丽红2，刘志华1，杨光宇1，
申钦鹏*1
(1. 云南中烟工业有限责任公司 云南省烟草化学重点实验室，云南 昆明 650231；
2. 昆明理工大学 化学工程学院，云南 昆明 650224)
摘要：为考察卷烟主流烟气中的香气成分，先用剑桥滤片收集主流烟气的总粒相物，再对同时蒸馏萃取和超临界流体萃取条件进行优化，然后分别采用这两种萃取方法对捕集了烟气粒相物的剑桥滤片进行前处理，再经气相色谱质谱联用仪分析所得样品。结果表明，同时蒸馏萃取得到94种挥发性香气成分，超临界流体萃取得到118种挥发性香气成分，两者共得到香气成分总量达181种。可见，两种方法结合起来分析烟气中香气成分更具优势。
关键词：主流烟气；超临界流体萃取；香气成分
中图分类号：O656.3 文献标识码：A 文章编号：0258-3283(2018)
Explore the Aroma Components in Mainstream Cigarette Smoke by Simultaneous Distillation Extraction and Supercritical Fluid Extraction CUI Ting-hui1,2, TANG Shi-yun1, LIU Chun-bo1, HE Pei*1, ZHU Rui-zhi1, JIANG Li-hong2, LIU Zhi-hua1, YANG Guang-yu1, SHEN Qin-peng*1 (1. Key Laboratory of Tobacco Chemistry of Yunnan Province, China Tobacco Yunnan Industrial Co., Ltd., Kunming 650231, China; 2. Academy of Chemical Engineering, Kunming University of Science and Technology, Kunming 650224, China), Huaxue Shiji, 2018, 40(1)
Abstract: In order to investigate the aroma components in main stream cigarette smoke, the total particulate matters of the mainstream cigarette smoke were collected by cambridge filter. Then the cambridge filter was extracted by simultaneous distillation extraction or supercritical fluid extraction under optimized conditions. And samples were analyzed by gas chromatography mass spectrometry. The result showed that 94 kinds of aroma components were obtained by simultaneous distillation extraction and 118 kinds of aroma components were achieved by supercritical fluid extraction. The total amount of the aroma components were up to 181 kinds. So, it would be better to analyze the aroma components of the main stream cigarette smoke by the two methods at the same time.
Key words: mainstream cigarette smoke; supercritical fluid extraction; aroma components
双显色体系计算分光光度法测定银杏单宁含量
张丝柳，郭丽萍，杜小弟，胡婧，雷家珩*
（武汉理工大学 化学化工与生命科学学院，湖北 武汉 430070 ）
摘要：为了消除分光光度法测定单宁过程中黄酮类物质产生的干扰，采用酒石酸亚铁和硝酸铝-亚硝酸钠双显色体系进行测定，并通过计算分光光度法求解二元方程组获得单宁含量，同时也解得黄酮含量。单宁和黄酮分别在酒石酸亚铁显色体系和硝酸铝-亚硝酸钠显色体系中都具有线性响应，线性相关系数在0.9987～0.9999范围内。酒石酸亚铁体系中，ε单宁1= 0.01032 L/(mg·cm)，ε黄酮1= 0.005750 L/(mg·cm)；硝酸铝体系中ε黄酮2= 0.01245 L/(mg·cm)，ε单宁2= 0.002707 L/(mg·cm)。在实际混合体系中，吸光度符合加和性，通过方程组解得的单宁含量标准偏差为0.024% ～ 0.062%，加标回收率为101.8% ～ 108.0%，说明本方法精密度和准确度较高。同时还求得黄酮含量标准偏差为0.013% ～ 0.033%，加标回收率为102.7% ～ 104.9%。通过此方法测出银杏叶（春）、银杏叶（秋）、外种皮、白果中的单宁含量分别为1.605%、1.031%、0.947%、0.055%。
关键词：银杏；单宁；计算分光光度法；酒石酸亚铁光度法；硝酸铝-亚硝酸钠光度法
中图分类号：O657.32 文献标识码：A 文章编号：0258-3283（201*）
Determination of Ginkgo BilobaTannin Content by Dual ChromophoricSystems Computational Spectrophotometry ZHANG Si-liu, GUO Li-ping , DU Xiao-di, Hu Jing, LEI Jia-heng*（School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, China）
Abstract: To eliminate the interference of flavonoids in the determination of tannins by spectrophotometry, this work adopted the ferrous tartrate and aluminum nitrate-sodium nitrite dual chromophoric systems, and tannin content was calculated by computational spectrophotometry, flavonoid content was obtained as well. There were linear relationships both of tannins and flavonoids in ferrous tartrate chromogenic system and aluminum nitrate-sodium nitrite chromogenic system, and the linear correlation coefficient in the range of 0.9987 to 0.9999. In the ferrous tartrate system, ε tannin1=0.01032 L/(mg·cm), εflavonoid1= 0.005750 L/(mg·cm); In aluminum nitrate-sodium nitrite system, ε flavonoid2 = 0.01245 L/(mg·cm), ε tannin2=0.002707 L/(mg·cm). In the mixed system, the absorbance conformed to the additive property, through the equations, the standard deviation of tannin content was 0.024% ～ 0.062%, the recovery was range from 101.8% to 108.0%, it means that this method has high precision and accuracy. At the same time, the standard deviation of flavonoid content was determined which was 0.013% to 0.033%, and the recovery was range from 102.7% to 104.9%. Via this method, the tannin content of ginkgo leaves (spring), ginkgo leaves (autumn), ginkgo sarcotestas, ginkgo seeds were 1.605%, 1.031%, 0.947% and 0.055% , respectively.
Key words: gingko; tannins; computational spectrophotometry; ferrous tartrate spectrophotometry; aluminum nitrate-sodium nitrite spectrophotometry
硝酸钯-硝酸镁用于消除硫酸盐对石墨炉原子吸收法
测量钼的干扰研究
杜青
（南京市环境监测中心站，江苏 南京 210013）
摘要：钼是饮用水、地表水和地下水水质的控制指标之一。硫酸盐(以SO42-计)浓度达到500 mg/L时，对钼的石墨炉原子吸收分析法产生显著干扰。考察了氯化钙、硝酸铵、硝酸镁、硝酸钯、磷酸二氢铵和抗坏血酸几种基体改进剂对石墨炉原子吸收法对测量钼的干扰研究。结果表明，硝酸钯-硝酸镁混合基体改进剂消除硫酸盐干扰效果最佳，其他基体改进剂虽能不同程度提高测量准确度，但灵敏度下降、背景吸收较大、测量精度不高。通过对石墨炉升温程序的优化，采用硝酸钯-硝酸镁基体改进剂，灰化温度可达1400 ℃，利于基体驱除，而且背景值小、吸收峰形好。钼的线性测量范围为0 ～ 50 μg/L，方法检出限为0.6 μg/L；实际样品测量的相对标准偏差为5.7% ～ 14.8%（n = 6），加标回收率为81% ～ 96%。与MIBK萃取GFAAS法和ICP-MS法相比，该方法操作简便、分析成本低、易于推广应用。
关键词：钼的测量；硫酸盐干扰；硝酸钯-硝酸镁基体改进剂；石墨炉原子吸收法。
中图分类号：O657.3 文献标识码：A 文章编号：
Pd(NO3)2-Mg(NO3)2 Matrix Modifier for Reducing Sulfate Interference in Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry DU Qing (Nanjing Environmental Monitoring Centre, Nanjing 210013, China)
Abstract:Molybdenum is one of the control targets in environmental quality standards for drinking water, surface water and groundwater. The determination of molybdenum by GFAAS was interfered by only 500 mg/L SO42-. Experimental results showed that among the matrix modifiers of CaCl2, NH4NO3,Mg(NO3)2, Pd(NO3)2,NH4H2PO4 and C6H8O6, Pd(NO3)2 in conjunction with Mg(NO3)2 achieved the optimal results. Other matrix modifiers could reduce sulfate interference somewhat, but had low sensitivity, high background absorbance and poor precision. When applied with Pd(NO3)2-Mg(NO3)2, the ashing temperature reached to 1400℃ to the benefit of matrixes eliminating. Low background absorbance and well-shaped absorption peak were available based on the optimum graphite furnace program. The linear measuring range of molybdenum was 0 ～ 50 μg/L, the MDL was 0.6 μg/L. The RSD (n = 6) of practical sample measurement ranged from 5.7% to 14.8%, the spiked recoveries were between 81% and 96%. Compared with MIBK extraction-GFAAS and ICP-MS, this method was simple and convenient in operation with low costs and broad application.
Key words: determination of molybdenum; sulfate interference; Pd(NO3)2-Mg(NO3)2 matrix modifier; GFAAS
9组分挥发性有机物溶液标准物质制备技术研究
张鹏辉1，王德峰2，张惠1，杨娜1，杨嘉伟1，潘义*1
（1. 中国测试技术研究院，四川 成都 610021；
2. 内蒙古自治区阿拉善盟产品质量计量检测所，内蒙古 阿拉善盟 750300）
摘要：建立了9组分挥发性有机物溶液标准物质的制备技术方法和分离分析手段，确保多组分、低沸点、易挥发有机物的精确制备以及异构体之间的完全分离。考虑相对校正因子的影响，以气相色谱面积归一化法对每种原料及关键杂质的含量准确定值。以重量-容量法的配制值作为认定值，制备1000 μg/mL的9组分挥发性有机物溶液标准物质，其均匀性和稳定性通过了F检验和t检验，在12个月有效期内量值准确可靠，最终定值的不确定度为5%（k = 2），可用于环境污染物中挥发性有机物的含量分析，为挥发性有机物检测量值溯源关键技术提供依据。
关键词：挥发性有机物；标准物质；认定值；不确定度
中图分类号：O625. 11 文献标识码：A 文章编号：
Preparation of 9 Kinds of Volatile Organic Compounds Reference Material ZHANG Peng-hui1, WANG De-feng2, ZHANG Hui1, Yang Na1, YANG Jia-wei1, PAN Yi*1 (1. National Institute of Measurement and Testing Technology, Chengdu 610021, China; 2. Alxa Institute of Quality and Metrology, Alxa 750300)
Abstract: The preparation and isolation methods of 9 kinds of volatile organic compounds (VOCs) reference material were investigated and established. This method especially for multicomponent and low boil points of VOCs can ensure the process of preparation accurately and isolation of isomers absolutely. The purities of 9 kinds of reagents as the start materials of VOCs were determined by GC-FID concerning the effect of relative correction factors. The prepared value from weighting-volumetric method was defined as the characteristic value with the concentration of 1000 μg/mL. Within the 12 months, the reference material via the F and t examinations has good homogeneity and stability with the relative expanded uncertainty of 5% (k = 2). The 9 kinds of VOCs reference material was primarily used for the content analysis of VOCs and providing reference in the valuation transfer and traceability system.
Key words: volatile organic compounds; reference material; characteristic value; uncertainty
Li2Mn0.5Ti0.5O3的合成与锂离子交换研究
江津河*1，刘方旺2，马欣欣2
（1. 潍坊学院 化学化工学院，山东 潍坊 261061；2. 青岛科技大学 化工学院，山东 青岛 266042）
摘要：利用固相反应热结晶的方法合成尖晶石型复合金属氧化物Li2Mn0.5Ti0.5O3。具有尖晶石型结构的氧化物，可以在嵌入替代离子改变自身氧和锂化学计量数的同时，维持晶体结构的稳定性。这种特性能够用于离子交换研究，用来满足提取锂的需求。采用X射线衍射方法、原子吸收检测法、Kd值检测等方法对所合成的复合金属氧化物进行锂离子脱嵌性能测试。实验分析表明，离子交换机理是实现锂离子脱嵌的主要原因，用硝酸浸出锂离子后的实验样品，对锂离子的交换能力高达6.2 mmol/g。
关键词：Li2Mn0.5Ti0.5O3；金属氧化物；合成；离子交换
中图分类号：TQ 016.1 文献标识码：A 文章编号：0258-3283（2018）
Synthesis and Exchange on Spinel Phase Li2Mn0.5Ti0.5O3 JIANG Jin-he*1, LIU Fang-wang2, MA Xin-xin2(1. Department of Chemistry and Chemical Engineering, Weifang University, Weifang 261061, China; 2. Department of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China), Huaxue Shiji, 2018, 40(1)
Abstract：The spinel-type compound metal oxide Li2Mn0.5Ti0.5O3was synthesized using solid crystallization reaction. The oxide with spinel-type structure can insert alternative ions and change the stoichiometric number in lithium and oxygen, besides, it can keep spinel-type structure stability. This characteristic can be used for ion exchange to meet requirement of extracting lithium. The Li+ extraction/insertion performance of this material was investigated by X-ray, atomic absorption detection and Kd measurement. Data showed that the Li+ extraction/insertion be governed mainly by ion-exchange mechanism. Remarkably, the Li2Mn0.5Ti0.5O3samples which was leached Li+ by nitric acid showed an Li+ exchange capacity as large as 6.2 mmol/g.
Key words：Li2Mn0.5Ti0.5O3；metal oxide；synthesis；ion exchange
改性魔芋葡苷聚糖共振散射法测定铁含量
翟好英*，张金洋，吴烨梅
（内江师范学院 化学化工学院，四川 内江 641112）
摘要：在酸性介质中，次氯酸根离子氧化魔芋葡苷聚糖（KGM）使其发生降解而得到改性KGM。由于改性KGM中含有亲水性的羟基（-OH）、羧基（-COOH）等活性基团，从而使得改性后的KGM水溶性大大增加。实验结果表明，改性KGM分子中所含有的活性基团如羧基等能吸附Fe3+并与其配位形成铁基配合物，使得体系的共振散射信号明显增强，且在343 nm处产生1个显著的共振散射峰。在0.056 ～ 14 μg/mL浓度范围内，体系的共振散射强度变化值与Fe3+浓度之间具有良好的线性关系，建立了一种共振散射法测定铁含量的方法。并将该法运用于测定钢铁废渣中Fe3+ 含量，其加标回收率高达96.8%。
关键词：魔芋葡甘聚糖；改性；Fe3+；吸附；共振散射法
中图分类号: O657.3 文献标识码: A 文章编号:
Resonance Scattering Method for the Determination of Fe (Ⅲ) with Modified Konjac- glucomannan ZHAI Hao-ying*, ZHANG Jin-yang, WU Ye-mei (College of Chemistry and Chemical Engineering, Neijiang Normal University, Neijiang 641112)
Abstract：Konjacglucomannan (KGM) was oxidized by hypochlorite ion to obtain modified KGM in acidic medium. Dueto containing many active groups such as hydroxyl and carboxyl, the water-solubility of modified KGM is greatly increased. Moreover, the active groups of modified KGM can adsorb and coordinate with ferric ions to form coordination compound, which makes the resonance scattering intensity enhance distinctly and produces an obvious resonance scattering peak at 343 nm. In addition, there is a good linear relationship between the resonance scattering signal and the concentration of ferric ions in the range of 0.056 ～ 14 μg/mL. Therefore, the resonance scattering method to determine iron content was established and applied to measure ferric content in the steel slag with the recovery of 96.8% .
Key words：konjacglucanmannan; modification; Fe3+; adsorption; resonance scattering method
ZnS量子点荧光探针对Pb离子检测研究
张艺*，朱振华，黄珏欣
（伊犁师范学院 污染物化学与环境治理重点实验室 新疆凝聚态相变与微结构实验室，新疆 伊宁 835000）
摘要：以L-半胱氨酸修饰ZnS量子点为荧光探针，测定火腿肠中Pb2+离子含量。对ZnS量子点进行了UV、IR、荧光性能表征。研究了酸度、ZnS量子点浓度对体系荧光强度的影响，最佳条件为pH 8，L-半胱氨酸-ZnS量子点（L-ZnS量子点）浓度为1.0×10-6 mol/L。基于Pb2+浓度对体系的荧光猝灭效应，实现对Pb2+的定量检测，Pb2+浓度在1.0×10-7 ～ 4.5×10-5 mol/L范围内与体系的荧光强度线性关系良好，R2 = 0.9847，检出限（3σ/S）为3.7×10-8 mol/L。线性方程F0/F=88.14-14.05ρpb2+，RSD为5.4%（n = 6）。该方法简便、灵敏度高。
关键词：铅离子；荧光探针；ZnS量子点
中图分类号：O657.3；O614.43 文献标识码：A 文章编号：0258-3283（2018）
ZnSQuantum Dots as Fluorescent Probe in the Determination of Pb Ions ZHANG Yi*, ZHU Zhen-hua, HUANG Jue-xin (Xingjiang Laboratory of Phase Transitions and Microstructure in Condensed Matters, Key Laboratory of Pollutant Chemistry and Environmental Treatment, Yi Li Normal University, Yining 835000, China), Huaxue Shiji, 2018, 40(1)
Abstract: Determination of Pb2+ ion content in ham was conducted by a fluorescent probe made of L-cysteine modified ZnS quantum dots. ZnS Quantum dots were investigated by ultraviolet visible absorption (UV), infrared radiation (IR), fluorescence spectrum (FS). The effects of the system acidity and the concentration of ZnS quantum dots on the fluorescence intensity were investigated. Optimum condition was obtained as pH 8.0 and ρL-ZnS=1.0×10-6mol/L. Quantitative detection of Pb2+ was achieved according to the quenched luminescence extent of ZnS quantum dots by Pb2+. The fluorescence intensity of the whole system shows a good linear relationship with the concentration of Pb2+ in the range of 1.0×10-7 ～ 4.5×10-5mol/L. The linear regression equation can be described F0/F=88.14-14.05ρpb2+,and the correlation coefficient is calculated to be 0.9847. The limit of detection is 3.7×10-8 mol/L and RSD is 5.4%(n=6). The method is simple and sensitive, which can be applied for the determination of Pb2+ concentration in many actual systems.
Key words: lead ions; fluorescent probe; ZnS quantum dots
乙酸-3-氯-3-甲基丁酯的合成工艺研究
曾永明，魏婷*，何伟，耿莉莉，侯培桦
（昌吉学院 化学与应用化学系，新疆 昌吉 831100）
摘要：以MBOH和乙酰氯为原料，经酯化、亲电加成串联反应合成了乙酸-3-氯-3-甲基丁酯。通过单因素实验探讨了反应温度、反应时间、配料比对产物收率的影响。在此基础上，采用响应曲面法对实验条件进行最优化选择。结果表明，合成乙酸-3-氯-3-甲基丁酯的最佳实验条件为n(乙酰氯)∶n(3-甲基-3-丁烯-1-醇)= 1.17∶1、9 ℃下反应230 min，在此条件下产率达95.87%。采用红外光谱、气相色谱、核磁共振和气质联用色谱仪等对目标化合物的结构进行表征，并研究了其香气评价及稳定性研究。
关键词：乙酸-3-氯-3-甲基丁酯；香料；响应曲面法；合成工艺
中图分类号：TS264.3 文献标识码：B 文章编号：0258-3283（2017）
Preparation Technology of 3-Chloro-3-methyl Butyl Acetate ZENG Yong-ming, WEI Ting*, HE Wei, GENG Li-li, HOU Pei-hua(Department of Chemistry and Applied Chemistry, Changji University, Changji 831100, China)
Abstract: A simple, one-pot cascade reaction for the synthesis of 3-chloro-3-methyl butyl acetate has been developed by using MBOH and acetyl chloride as raw materials. The effect of the reaction time, temperature and feed ratio was investigated. Base on the single-factor experiments, the optimal synthetic conditions by using response surface methodology were obtained as follows : mole ratio of MBOH to acetyl chloride of 1.17 : 1 at 9 ℃ for 230 mins to give the target product with a maximum yield of 95.87%. The structures of the target compound were confirmed by IR , GC, GC/Ms and NMR, and its aroma evaluation and stability were investigated.
Key words: 3-chloro-3-methyl butyl acetate; spice; response surface methodology; preparation technology
5-氨基-7-氟喹啉的合成
赵啸颖，徐卫良，印晓星，徐炜政*
（徐州医科大学药学院，江苏徐州221004）
摘要：标题化合物是一个具有显著药用价值的医药中间体，但与其合成相关的报道较少且收率低。以2-氯-3-氟苯甲酸为起始原料，经取代、霍夫曼降解、关环、硝化、铁粉还原以及加氢脱8-氯6步反应得到标题化合物。该工艺路线成本低、易操作、总收率高达43%，适合工业化生产。
关键词：5-氨基-7-氟喹啉；喹啉；合成
中图分类号：TQ 文献标识码：A 文章编号：0258-3283（2018）
Synthesis of 5-Amino-7-fluoroquinolineZHAO Xiao-ying, XU Wei-liang, YIN Xiao-xing, XU Wei-zheng*(School of Pharmaceutical Science,Xuzhou Medical University, Xuzhou 221004,China), HuaxueShiji, 2018, 40(1)
Abstract：5-Amino-7-fluoroquinoline is a pharmaceutical intermediate with significant medicinal value, but the reports on its synthesis are particularly rare with lower yield. The process for the synthesis of 5-Amino-7-fluoroquinolinewas investigated. The target compound was prepared from 2-chloro-3-fluorobenzoic acid as the starting material via six steps includingsubstitution, Huffman degradation, ring closure, nitration, iron powder reduction and reduction of 8-cdechlorination. The synthetic route was low cost and easy to operatewith higher total yield(43%),and it is suitable for industrial production of 5-Amino-7-fluoroquinoline.
Key words：5-Amino-7-fluoroquinoline; quinoline;synthesis
微波辅助合成5-苯基取代的呋喃类化合物
骆焕泰1，杨浩2，洪伟*1
(1. 北方民族大学 化学与化学工程学院，宁夏 银川 750021；
2. 宁夏医科大学 药学院，宁夏 银川 750004)
摘要：呋喃为母核的化合物具有多种生物活性，如抑制蛋白质精氨酸甲基转移酶（PRMT）的活性。报道一种新型的呋喃为母核类化合物，N-甲基-(5-(4-腈基苯基)呋喃-2-基-甲基)-乙胺盐酸盐的合成方法。以5-溴糠醛为原料，经还原胺化反应，微波辅助的Suzuki反应和脱保护基反应的3步反应合成了5-苯基取代的呋喃类新化合物，其结构经1HNMR，13CNMR和HRMS表征，总收率为73%。
关键词：呋喃化合物；Suzuki反应；合成
中图分类号: O621.3 文献标识码: A 文章编号：0258-3283(2018)
Microwave-assisted Synthesis of 5-Phenyl Substituted Furan Derivative LUO Huan-tai1, YANG Hao2, HONG Wei*1 (1. School of Chemistry and Chemical Engineering, North Minzu University, Yinchuan 750021, China; 2.School of Pharmacy, Ningxia Medical University, Yinchuan 750004, China), Huaxue Shiji, 2018, 40(1)
Abstract: Furan core-based compounds have a variety of biological activities, such as inhibition of protein arginine methyltransferase (PRMT) activity. A synthetic method for a novel furan core-based derivative, N-methyl-(5-(4-nitrile-phenyl)furan-2-methyl)ethylaminehydrochloridewas reported. It was synthesized with the 5-bromofurfural as the raw material by a three-step reaction, which contains the reductive amination, microwave-assisted Suzuki reaction and deprotection reaction. The total yield is73% and the structure was confirmed by 1HNMR, 13CNMR and HRMS.
Key words: furan derivative; Suzuki reaction; synthesis
N-甲基吡咯烷酮促进布洛芬VC酯和布洛芬异VC酯的合成
祝显虹[1]，郑大贵，周安西，曹波强
（上饶师范学院 江西省普通高校应用有机化学重点实验室，江西 上饶 334001）
摘要：在N-甲基吡咯烷酮（NMP）的促进下，布洛芬与SOCl2反应得到酰氯后，再与加入的L-抗坏血酸（VC）或D-异抗坏血酸（异VC）反应合成布洛芬VC酯和布洛芬异VC酯。以布洛芬VC酯合成为例，考察了NMP用量、酰氯化反应时间、成酯反应时间和物料比对反应收率的影响。结果表明，5 mmol布洛芬、5 mL NMP、物料比n（布洛芬）∶n（SOCl2）∶n（VC）＝ 1.0∶1.2∶1.4，25 ℃酰氯化反应0.5 h，25 ℃成酯反应10 h，收率为86.20%。产物结构经1HNMR、13CNMR、IR和ESI-MS确证。
关键词：N-甲基吡咯烷酮；布洛芬VC酯；布洛芬异VC酯；合成；机理
中图分类号：O621.2 文献标识码：A 文章编号：0258-3283（2017）
N-Methyl Pyrrolidone-promoted Synthesis of AscorbicylIbuprofenate and IsoascorbicylIbuprofenate
ZHU Xian-hong*, ZHENG Da-gui, ZHOU An-xi, CAO Bo-qiang（Key Laboratory of Applied Organic Chemistry, Higher Institutions of Jiangxi Province, Shangrao Normal University, Shangrao 334001）
Abstract: Ascorbicylibuprofenate and isoascorbicylibuprofenate was synthesized via acyl chlorination of ibuprofen with SOCl2 in N-methyl pyrrolidone（NMP）, followed by esterification with ascorbic acid or isoascorbic acid. The effect of such factors as NMP amount, acyl chlorination time, esterification time and molar ratio of reactants on the yield of ascorbicyl 2-（4-isobutylphenyl）propanoate was investigated. It was found that the yield could reach 86.20% under the optimal reaction conditions 5 mmol of ibuprofen, 5 mL NMP, and n（ibuprofen）: n（SOCl2）: n（VC）= 1.0 : 1.2 : 1.4, acyl chlorination at 25 ℃ for 0.5 h, esterification reaction at 25 ℃ for 10 h. The title compound was characterized by 1HNMR, 13CNMR , IR and ESI-MS.
Key words: N - methyl pyrrolidone; ascorbicylibuprofenate; isoascorbicylibuprofenate; synthesis; mechanism
