中国分析测试协会
《化学试剂》2015年5月第37卷第5期中英文摘要
文章来源：《化学试剂》编辑部
螯合树脂及其在检测食品中重金属离子的应用
娄婷婷1 ，肖亚兵*1，何佳1，何健2
(1.天津出入境检验检疫局，天津 . 淮安出入境检验检疫局，江苏 淮安& 223001)
摘要：系统地介绍了新型螯合树脂的概念、分离富集金属离子的原理以及螯合树脂的分类，并对合成型螯合树脂的研究进展及其在食品分析检测领域中分离富集金属离子的应用情况进行了综述。
关键词：螯合树脂；金属离子；食品；应用
中图分类号：O652.6&&&&&&&&& 文献标识码：A&&&&&&&&&&&& 文章编号：15)05
Progress of Chelating Resin and Application for Metal Ions Detection in Food
LOU Ting-ting, XIAO Ya-bing, HE Jia, ZHOU Jin-fan (Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300461, China), Huaxue Shiji, ),
Abstract: This work described the adsorption principle of chelating resin for metal ions and common class. Also the progress on chelating resin was introduced and application on metal ions detection in food and water matrix was summarized.
Key words: application
含有苯并噁唑及吡啶基团的双杂芳基乙炔的合成
刘杰，庄俊鹏*，郝海军，张曙光，牛俊宇
（北京化工大学 理学院，北京& 100029）
摘要：标题化合物通过双杂芳基乙烯在加热回流的二氯甲烷中加溴，然后室温下在四氢呋喃溶液中由叔丁醇钾脱溴的方法进行制备。合成了8种未见文献报道的标题化合物。与过渡金属催化方法相比，此种制备方法原料易得，反应简便高效，不需要有昂贵金属参与。对所得产物进行了紫外和荧光光谱的检测，光化学测试表明，在紫外光照射下，标题化合物在有机溶剂或酸性水溶液中没有光化学活性。
关键词：二芳基乙炔；加溴和脱溴；紫外和荧光光谱；苯并噁唑；光化学性质
中图分类号：&&&&&&&&&&&& 文献标识码：A&&&&& &&&&&&文章编号：15)05
Synthesis of Diheteroarylacetylenes Containing Benzoxazole and Pyridine Groups
LIU Jie, ZHUANG Jun-peng*, HAO Hai-jun, ZHANG Shu-guang, NIU Jun-yu (Department of Organic Chemistry, Faculty of Science, Beijing University of Chemical Technology, Beijing 100029,China), Huaxue Shiji, ),
Abstract: Diheteroarylacetylenes containing benzoxazole and pyridine groups were synthesized from diheteroarylethenes in moderate yields by bromination with Br2 in refluxing dichloromethane and then debromination with KO-tBu in tetrahydrofuran at room temperature. Compared with the transition-metal-catalyzed methods, this procedure provides a metal-free, efficient and economical method with easily accessible starting materials for the synthesis of diheteroarylacetylenes. The UV and FL spectra were determined. The photochemical determination shows that these diheteroarylethenes are photoinert to UV irradiation in organic solvent or in acidic aqueous solution.
Keywords: d brominati UV and FL photochemical property
Schiff碱平面双核酞菁的合成及性能研究
朱白青，韩明亮，邓鹏飞，张学俊*
（中北大学 理学院，山西 太原& 030051）
摘要：以4-硝基邻苯二甲腈、叔丁醇、对苯二甲醛等为原料，合成不对称胺基锌酞菁(2(3)-胺基-9(10),16(17), 23(24)-(叔丁氧基)锌酞菁(APC))和一种新型平面双核酞菁(9(10),9&(10&),16(17),16&(17&),23(24),23&(24&)-叔丁氧基-2(3),2&(3&)-(对苯甲亚胺基)锌酞菁(bi-TPC))。通过FT-IR、UV-Vis、1HNMR、元素分析、循环伏安等手段对APC和bi-TPC的结构进行表征。结果表明，与无取代酞菁相比，APC和bi-TPC Q带的最大吸收峰具有明显红移；能级与纳米TiO2薄膜匹配，适用于制备太阳能电池。
关键词：酞菁；Schiff碱；双核；共轭
中图分类号：&&&&&&&&&&&& 文献标识码: A&&&&&&&&&&&& 文章编号：15)05
Synthesis and Characterization&of Schiff Base Planar Binuclear Phthalocyanine
ZHU Bai-qing, HAN Ming-liang, DENG Peng-fei, ZHANG Xue-jun* (College of Science, North University of China, Taiyuan 030051, China) , Huaxue Shiji, ),
Abstract 4-nitro-phthalonitrile, tert-butanol and 1,4-phthalaldehyde as the main raw materials were used to synthesis unsymmetrical amido zinc phthalocyanine(2(3)-amido-9(10), 16(17), 23(24)-(tert-butoxy) zinc phthalocyanine (APC)) and a new planar binuclear zinc phthalocyanine(9(10),9&(10&),16(17),16&(17&),23(24),23&(24&)-tert-butoxy-2(3),2&(3&)-(1,4-benzene methylene amine) zinc phthalocyanine (bi-TPC)). The compounds were characterized by FTIR, UV-Vis, 1H NMR, elemental analysis and cyclic and differential pulse voltammetry. The results show that the Q band maximum absorption peaks of APC and bi-TPC have red shift obviously, compared with the unsubstituted phthalocyanine (669 nm), APC and bi-TPC&level are matching with nano TiO2 thin film and suitable for the preparation of solar cell.
Key words: S conjugation
带有乙烯基苄基氯长链季铵盐的合成及抑菌性能研究
&&&&&&&&&&& &&&&&&&&&&&&&&杨万丽*，董艳丽，马荣华，李陆军，周超健
（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：以对乙烯基卞基氯（C9H9Cl）为原料分别与二甲基十二烷基叔胺（12DMA）、二甲基十四烷基叔胺（14DMA）、二甲基十六烷基叔胺（16DMA）进行亲核取代反应合成C9H9Cl-12DMA、C9H9Cl-14DMA 和C9H9Cl-16DMA 3种标题化合物，并用FT-IR、1HNMR、EA和TG等手段表征其结构。将3种新标题化合物采用抑菌圈法对大肠杆菌、金黄色葡萄球菌和枯草芽孢杆菌抑菌活性进行测试，结果表明杀菌活性大小顺序为：C9H9Cl-14DMA＞C9H9Cl-16DMA＞C9H9Cl-12DMA。
关键词：季铵盐；合成；表征；抑菌性&&&
中图分类号：O623.731&&&&&&&&&& 文献标识码：A　&&&&& 文章编号：15)04
Synthesis and Antibacterial Performance of Long Chain Quaternary Ammonium Salt with Vinyl and Benzyl
YANG Wan-li, DONG Yan-li, MA Rong-hua, LI Lu-jun, ZHOU Chao-jian (College of Chemical and Chemistry Engineering, Qiqihar University, Qiqihar 161006, China), Huaxue Shiji, )
Abstract: 1-(Chloromethyl)-4-vinylbenzene (C9H9Cl) as raw materials, three kinds of new type quaternary ammonium salt antibacterial monomers, namely C9H9Cl-12DMA, C9H9Cl-14DMA&and C9H9Cl-16DMA&were synthesized via nucleophilic substitution reaction with N, N-dimethyldodecylamine(12DMA), N, N-dimethyltetradecylamine&(14DMA), N, N-dimethylcetylamine (16DMA), respectively. The structures were confirmed by using&FT-IR, 1HNMR, EA and TG.&The antibacterial activities were tested for staphylococcus aureus, bacillus subtilis and escherichia coli by the inhibition zone method.&The bactericidal activity of quaternary ammonium salt monomer was tested via bacteriostatic circle diameter method and the bactericidal activity order was arranged as C9H9Cl-14DMA&C9H9Cl-16DMA&C9H9Cl-12DMA.
Key words: quat antibacterial performance
蒙药复方三子汤组分药材川楝子与栀子、诃子配伍
前后栀子苷含量的HPLC法测定及其小鼠急性肝毒性研究
王书妍*，包玉敏，王月英
（内蒙古民族大学 化学化工学院，内蒙古 通辽& 028000）
摘要：建立了蒙药复方三子汤组分药材川楝子、栀子与诃子配伍前后栀子苷含量变化的HPLC分析方法；三子汤组分药材川楝子与栀子、诃子配伍前后小鼠急性肝毒性分析方法。采用Hypersil ODS C18色谱分离柱，以V（乙腈）∶V（水）＝15∶85为流动相，流速1mL/min，检测波长238 nm，HPLC法测定栀子苷含量。小鼠给药，禁食12 h，采血，分离血清，测定血清中ALT（谷丙转氨酶）、AKP（碱性磷酸酶）、AST（天门冬氨酸氨基转移酶）含量。取小鼠肝脏，称重，制成匀浆，离心，取上清液，测定肝匀浆中LDH（乳酸脱氢酶）、AKP（碱性磷酸酶）含量。结果表明，栀子与川楝子、诃子按等质量比配伍后，栀子苷含量均比单味药材栀子中栀子苷含量降低，且对小鼠肝毒性明显降低。因此，三子汤三味药材等质量比配伍，能降低蒙药复方三子汤的毒性。
关键词：三子汤；栀子；栀子苷；肝中毒
中图分类号：&&&&&&&&&& 文献标识码: A&&&&&&&&&&& 文章编号：15)05
HPLC Measurement of the Content of Geniposide in Mongolia Medicine Complex Soup of Gardenia, Toosendan fruit and Terminalia Fruit and Effects of the Ingredients Proportion on Acute Toxicity in Mice Liver
WANG Shu-yan, BAO Yu-min, WANG Yue-ying (The College of Chemistry and Chemical Engineering, Inner Mongolia University for The Nationalities, Tongliao 028000, China), Huaxue Shiji, ),
Abstract: HPLC analysis has been applied to measure the content of geniposide in mongolia medicine complex soup of Gardenia, toosendan fruit and terminalia fruit. The effects of the ingredients proportion in the complex soup on the acute toxicity in mice liver are also examined. The analysis conditions for HPLC are Hypersil ODS C18 chromatographic separation column with acetonitrile and water (15: 85 V/V) as mobile phase, flow velocity of 1 mL/min and detector wavelength of 238 nm. The methods for the acute toxicity are tested by analyzing the content of ALT, AKP and AST in serum and LDH and AKP in liver. The amount of serum and liver are taken from the feeding medicine mice, and centrifuged to obtain upper clear solution. The results show that the content of toosendanin in complex soup with equal weight ratio of each ingredient is lower than that in toosendan fruit as the medicine. The acute toxicity for mice liver distinctly decreases. Therefore, the complex soup with equal weight ratio of toosendan fruit, gardenia and terminaliafruit has remarkable effects on reducing the toxicity of the complex soup.
Key words: liver toxicity
Gemini表面活性剂与月桂醇醚羧酸盐的复配性能研究
余鹏鸣1, 3，张 威*1, 2，王丰收1，董万田1
（1. 上海发凯化工有限公司，上海& . 华东理工大学&&&&& ，上海& 200237；
3. 中国日用化学工业研究院，山西 太原& 030001）
摘要：研究了Gemini阳离子表面活性剂双十二烷基季铵盐（12-3(OH)-12）与阴离子表面活性剂月桂醇聚氧乙烯醚羧酸钠（AE9C）复配体系的稳定性、表面活性、泡沫性能、润湿性和乳化性能。结果表明，12-3(OH)-12与AE9C复配体系稳定性好，表现出很好的协调增效作用。当n(12-3(OH)-12) : n(AE9C) = 1 : 2时，增效作用最为明显，其临界胶束浓度CMC为1.49 mmol/L，最低表面张力&CMC = 30.15 mN/m，都要低于任一单一组份。复配体系的泡沫、润湿和乳化性能均要优于任一单组分，并且都在n(12-3(OH)-12) : n(AE9C) = 1 : 2时，表现出最佳性能。
关键字：Gemini表面活性剂；月桂醇聚氧乙烯醚羧酸盐；复配体系；协同增效
中图分类号：&&&&&&&&&&& 文献标识码：A&&&&&&&&&& 文章编号：（2015）
MixedProperties&of&&Cationic&GeminiSurfactant&and&Laurinol&Ether&Carboxylate&Sodium&Anionic Surfactant
YU Peng-ming1,3, ZHANG Wei*1,2, WANG Feng-shou1, DONG Wan-tian1（1. Shanghai Fine Chemical Co., Ltd., Shanghai 201505, C 2. East China University of Science and Technology, Shanghai 200237, C 3. China Research Institute of Daily Chemical Industry, Taiyuan 030001, China）, Huaxue Shiji, )
Abstract: The surface activity, compatibility, foaming property, wetting power and emulsifying property were investigated for mixed Gemini surfactant 1,3-bis(dodecyl-N, N-dimethylammonium)-2-propanol(12-3(OH)-12) and laurinol ether carboxylate sodium (AE9C). These two surfactants show very good compatibility, and the strong synergic effect was shown by the mixture. When the molar ratio between 12-3(OH)-12 and AE9C was 1 : 2, i.e. the cationic and anionic head group charge were mixed in equal molar ratio, the mixed system showed the strongest synergic effect. The minimum values of critical micelle concentration (CMC) and the surface tension at cmc (&CMC) of mixed systems were 1.49 mmol/L and 30.15 mN/m, and the both were much lower than that of each surfactant. The foaming properties, wetting power and emulsifying property were also better than that of each component, and all these optimal results were shown while n(12-3(OH)-12) : n(AE9C) was 1 : 2.
Key words: G laurin synergic effect
无溶剂合成叔碳羟基膦酸酯及其表征
王储备*1，王威2，刘建枫3，周建伟1，褚亮亮1
(1. 新乡学院能源与燃料研究所，河南& 新乡& . 西安近代化学研究所，陕西& 西安& . 西北工业大学，陕西& 西安& 710000 )
摘要：发展了一种温和的磷酰化酮而得到标题化合物的方法。在碳酸钾催化无溶剂条件下，芳酮与亚磷酸酯形成羟基膦酸酯，该方法也适合对碱敏感的底物。在分离碱性催化剂（如三乙胺）过程中，常常伴随羟基膦酸酯发生重排反应，生成磷酸酯，磷酸酯影响产物纯度，增加产物分离难度；碳酸钾作为催化剂时，实验中未发现羟基膦酸酯发生重排反应。产物经核磁、红外、质谱等表征。
关键词：羟基膦酸酯；合成方法；路易斯碱；催化
中图分类号：&&&&&&&&&&&& 文献标识码：A&&&&&&&&&&& 文章编号：15)05
Solvent-free Synthesis and Characterization of Tertiary Hydroxy Phosphates
WANG Chu-bei*,a, WANG Weib , LIU Jian-fengc, ZHOU Jian-weia (a. Institute of Energy and Fuel, Xinxiang University, Xinxiang 453000, C b. Xi&an Modern Chemistry Research Institute, Xi&an710000, C c. School of Humanities, Northwestern Polytechnical University, Xi&an 710000,China), Huaxue Shiji, ),
Abstract: A benign synthesis method of tertiary hydroxyl phosphonates by hydro phosphonylation of unactivated ketones was developed. In the presence of potassium carbonate, aromatic or heteroaromatic ketones can react with phosphite to form tertiary hydroxy phosphonates under solvent-free and mild conditions. The proposed method was also suitable for base-sensitive ketone. Rearrangement of phosphonate to phosphate was carried out in many strong alkaline mediums, the rearrangement was not found in this work. The structures of products were confirmed by NMR, IR and MS.
Key words： L catalysis
拟除虫菊酯的电化学与生物传感器检测的研究进展
杜海军*，柳斌，罗乐，李玉美，班睿，吕昱
(贵州民族大学 电化学与储能材料研究所 化学与环境科学学院，贵州 贵阳& 550025)
摘要：电化学具有成本低、灵敏度高、仪器小巧等优点。近年来，构建基于检测拟除虫菊酯的电化学传感器已经成为一个热门的研究领域。简要评述了1996年以来检测拟除虫菊酯的电化学及生物传感器的研究进展，包括汞电极、修饰电极、分子印迹传感器、酶传感器、免疫传感器和DNA传感器等内容。
关键词：拟除虫菊酯；电化学检测；电化学传感器；电化学生物传感器；修饰电极；纳米材料
中图分类号：O657.1&&&&&&&&&&& 文献标识码：A&&&&&&&&&&&&&& 文章编号：（2015）
Electrochemical Sensors and Biosensors for Detection of Pyrethroids
DU Hai-jun *, LIU Bin, LUO Le, LI Yu-mei, BAN Rui, LV Yu (Institute of Electrochemistry and Energy Storage Material, College of Chemistry and Environmental Science, Guizhou Minzu University, Guiyang& 550025, China), Huaxue Shiji, )
Abstract: Electrochemical methods are well known for low cost, high sensitivity and miniature instruments. Recently, the design of electrochemical sensors for detection of pyrethroids has attracted remarkable attention in the field of sensors. This work mainly reviewed the developments of this field since 1996, including mercury electrodes, modified electrodes, , enzyme sensors, DNA sensors and molecular imprinting sensors.
Key words: elect ele electrochemical biosensors；modified electrodes；nanomaterials
水样中氨氮分析方法的研究
顾金凤，凌芳，曹丽丽，郭建国，刘征宙，郑琦，顾小焱*
（国药集团化学试剂有限公司，上海& 200002）
摘要：重点归纳总结了近年来在水样中氨氮分析方法的研究进展, 内容主要包括:氨氮的化学分析方法、仪器分析方法和水样的保存和预处理, 同时简述了氨氮测定的发展方向。
关键词：水样；氨氮；分析方法；预处理；
中图分类号：O661.1&&&&&&&&&& 文献标识码：A&&&&&&&&&&&& 文章编号：15)05
Analysis Method of Ammonia Nitrogen in Water
GU Jin-feng, LINGFang, CAO Li-li, GUO Jian-guo, LIU Zheng-zhou, ZHENGqi, GU Xiao-yan (Sinopharm Chemical Reagent Co.,Ltd.,Shanghai 200002,China), Huaxue Shiji, ),
Abstract: The progresses on the analysis methods of ammonia nitrogen in natural water were reviewed including analysis methods of ammonia nitrogen, existencestates of nitrogen, and the pre-treatment of the water samples. Simultaneity, this work has summarized the development direction of ammonia nitrogen.
Key words: pre-treatment of samples
并联双噻吩化合物的合成研究进展
袁勇，李雁武，李伦，朱太勇，袁建勇*
(重庆医科大学 药学院，重庆& 400016)
摘要：自从并联双噻吩环化合物在1886年被首次发现，该类化合物一直受到高度重视和广泛关注。作为一种重要的有机合成中间体，其在医药化工、材料化学及生物医学等领域应用尤为突出。重点从结构分类讲述其同分异构体的合成方法及应用研究进展，以期为未来研究者对该类化合物及其衍生物的合成研究提供有价值的参考。
关键词：并联双噻吩化合物；合成方法；研究进展
中图分类号：O626.12&&&&&&&&&& 文献标识码：A&&&&&&&& 文章编号：（2015）
Progress of Parallel Bithiophene Compound Synthesis
YUAN Yong, LI Yan-wu, LI Lun, ZHU Tai-yong, YUAN Jian-yong* (Institute of Pharmacy, Chongqing Medical University, Chongqing 400016, China), Huaxue Shiji, )
Abstract: Since parallel bithiophene compounds were first discovered in 1886, these compounds have received serious attention and broad concerns. As an important intermediate in organic synthesis, its application is prominent in the field of pharmaceutical chemistry, material chemistry and biomedicine. This work summarized the progress in synthetic method of isomers and application to provide a valuable reference for the future synthetic studies on those compounds and intermediate derivatives.
Key words: parallel
ICP-OES 法快速测定白头翁中21种矿物元素
赵庆帅1,2, 叶润蓉1, 周玉碧1, 王延花3, 卢学峰1, 孙胜男1,2, 舍莉萍1,2, 彭敏1, 孙菁 1
(1.中国科学院 西北高原生物研究所，青海省青藏高原特色生物资源研究重点实验室，青海 西宁& . 中国科学院大学，北京& . 青海省环境监测中心站，青海 西宁& 810007）
摘要：采用微波消解结合电感耦合等离子体发射光谱(ICP-OES)法对白头翁中21种元素含量进行了测定。所采用方法线性关系良好，r&0.9990，各元素检出限均低于0.0036 mg/L，加标回收率为88% ~ 105%，RSD均小于3.6%，具有良好的准确度和精密度。结果表明，白头翁中矿物元素含量丰富，重金属元素含量低于国家最低标准，符合安全用药标准。试验方法简单、快速、可靠、灵敏度高，可同时测定多种元素，满足样品分析要求。本研究结果可为开发利用白头翁药用资源提供基础资料。
关键词：白头翁；微波消解；ICP-OES；元素
中图分类号：O657.3&&&&&& 文献标识码：A&&&&&&&& 文章编号:15)
Elements Determination in Pulsatillachinensis by ICP-OES with Microwave Digestion
&ZHAO Qing-shuai1, 2, YE Run-rong1, ZHOU Yu-bi1, WANG Yan-hua3, LU Xue-feng1, SUN Sheng-nan1, 2, SHE Li-ping1,2, PENG Min1, SUN Jing* 1 (1. Qinghai Key Laboratory of Qinghai-Tibet Plateau Biological Resources, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810008, C 2. University of Chinese Academy of Sciences, Beijing 100049, C 3. Qinghai Environmental Monitoring Center Station, Xining 810007, China), Huaxue Shiji, )
Abstract: The contents of 21 elements in Pulsatillachinensis were determined by inductively coupled plasma optical emission spectrometer (ICP-OES) with microwave digestion. Linear correlation coefficient were larger than 0.9990 and excellent linear response were obtained. Recoveries obtained by standard addition ranged from 88% to 105% with RSD&3.6%.The results show that there are many elements in the Pulsatillachinensis, but the heavy metal element in Pulsatillachinensis is below the national minimum standard and meet the medication safety standards. The method is simple, fast, reliable, high sensitivity, and a variety of element can be determined simultaneously, meet the requirements of sample analysis. The results could provide a scientific basis for development of Pulsatillachinensis.
Keywords: P ICP-OES; elements
中兽药散剂中非法添加金刚烷胺的检测方法研究及应用
张立华1，周剑2，王敏
（中国农业科学院 农业质量标准与检测技术研究所，农业部农产品质量安全重点实验室，北京100081）
摘要：采用石英毛细管柱DB-5Ms（30m&0.3mm，0.25&m）、程序升温、FID检测器检测，建立了中兽药散剂中违规添加金刚烷胺的氢火焰离子化气相色谱(GC-FID)检测方法。该方法线性关系良好（R2=0.997，n=6），低、中、高3个浓度的添加平均回收率为95.2%。并运用方法对从12个省（市）购买的100个中兽药散剂药品进行检测。结果表明本方法准确可靠、简便易行，可用于中兽药散剂中非法添加金刚烷胺的含量检测。
关键词：中兽药散剂；金刚烷胺：GC-FID；检测
中图分类号：O657.7&&&&&&&&&& 文献标识码：A&&&&&&&&&&&&&& 文章编号：15)05
Determination Methods of Illegally Added Amantadine in Veterinary Traditional Chinese Medicine Powders by GC-FID
ZHANG Li-hua, ZHOU Jian, WANG Min
(Key Laboratory of Agrifood Safety and Quality, Ministry of Agriculture, Institute of Quality Standards and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China), Huaxue Shiji, ),
Abstract: A GC-FID chromatography method was established for effective detection on illegally added amantadine in veterinary traditional chinese medicine powders. The related substances were analyzed with programmed temperature in a DB-5Ms capillary column by FID. The results demonstrated that the linearity range of amantadine was 1.00~15.00 &g/mL,（r2=0.997，n=7）,the& mean recovery rate was 95.2%. And 100 samples of traditional chinese medicine powder from 12 province (city) were detected by this method. This method was accurate, reliable and suitable in the determination of amantadine added illegally in veterinary medicine powder.
Key words: veterinary traditional Chin GC-FID; determination
X-射线荧光光谱测定焊剂中硫、磷的方法研究
李颖，冯秀梅*，陈连芳，陈君
（江阴市产品质量监督检验所，江苏 江阴& 214431）
摘要：建立了X-射线荧光光谱对焊剂中硫、磷元素的快速检测方法。样品只需简单粉碎，直接压片进行测量，每个样品的测量时间短，仅为140 s。试样中硫、磷含量测定结果的相对标准偏差分别为0.78%和1.8%（n = 6），方法的准确度较好。用现有的国家标准分析方法进行对比试验，测量结果基本吻合。本法同其他检测方法相比，可对焊剂同时直接测定硫、磷两种元素，分析时间短，分析步骤少，结果稳定。
关键词：X-射线荧光；焊剂；硫；磷&&
中图分类号：TH744.11&&&&&&&& 文献标识码：A&&&&&&&& 文章编号：（2015）
Determination of Sulfur and Phosphorus in Flux by X-ray Fluorescence Spectrum
LI Ying, FENG Xiu-mei*, CHEN Lian-fang, CHEN Jun (Jiangyin Product Quality Supervision and Testing Institute, Jiangyin 214431, China), Huaxue Shiji, ),
Abstract: A rapid detection method for sulphur and phosphorus element in flux by X-ray fluorescence spectrum was established. The sample can be directly measured by simply crush and pressure. The test time of each sample is very short, only 140 s. The relative standard deviation of sulfur and phosphorus content in the sample were 0.78% and 1.8% (n = 6), respectively. The precision of the method is better than other methods. The test results were agreement with the results detected by the national standard method. The test accuracy of sulfur and phosphorus content in flux meet the test requirements. Compared with other detection methods, X-ray fluorescence spectrometry can be directly and simultaneously detect sulfur and phosphorus element with short analysis time, less analysis steps and stable results.
Key words: X- phosphorus
DSPE-UPLC-QTOF/MS法测定水中氨基甲酸酯类农药
蔡玺晨a，张占恩*a, b 张磊a, b
（苏州科技学院 a. 环境科学与工程学院，江苏 苏州& 215011；b. 江苏省环境科学与工程重点实验室，江苏 苏州& 215009）
摘要：研究建立分散固相萃取-超高效液相色谱-四极杆串联飞行时间质谱（DSPE-UPLC-QTOF/MS）法，测定水环境中3种氨基甲酸酯类农药（残杀威、仲丁威、速灭威）的分析方法。将萃取剂HC-C18颗粒直接投加到水样中，经过振荡后对目标物萃取，用空萃取柱进行过滤回收水样中的HC-C18颗粒，后经洗脱、氮吹浓缩后用UPLC-Q-TOF/MS检测器测定。实验中对萃取剂的选择、萃取时间、洗脱剂种类以及水样的pH等条件进行了优化，得到了最佳的萃取条件。3种氨基甲酸酯农药在0.5 ～ 100 &g/L范围内时，具有良好的线性（R & 0.9939），检出限介于6.40 ～ 11.3 ng/L之间。空白水样加标为1 &g/L时，相对标准偏差（RSD）为3.5% ～ 10.4%，加标回收率为77% ～ 105%。该方法可用于水体中氨基甲酸酯的分析测定。
关键词：氨基甲酸酯；分散固相萃取法；超高效液相色谱-四极杆串联飞行时间质谱；水样
中图分类号：X592&&&& &&文献标识码：A&&&&&& 文章编号：（2015）
Determination of Carbamate Pesticides in Water by DSPE-UPLC-QTOF/MS
CAI Xi-chena, ZHANG Zhan-en*a,b, ZHANG Lei a,b (a. College of Environmental Science and E b.; Suzhou University of Science and Technology, Suzhou 215009, China), Huaxue Shiji, )
Abstract：The dispersive solid-phase extraction and quadrupole ultra performance liquid chromatography tandem time-of-flight mass spectrometry (DSPE-UPLC-QTOF/MS) was established for the determination of three carbamate pesticides in aquatic environment (fenobucarb, propoxur, MTMC) analysis method. The extractant HC-C18 particle mixing to direct investment in water, after oscillation of object extraction, with the bottom is provided with a sieve plate extraction column polyethylene empty HC-C18 particles in water filtration and recovery, after elution, nitrogen blowing after concentration determined by UPLC-Q-TOF/MS detector. The selection of extraction agent, extraction time, eluent type and sample pH conditions were optimized and the best extraction conditions was obtained. Three kinds of carbamate pesticides in 0.5 ~ 100 g/L range, good linearity, limit of detection (R&0.9939) between 6.40 ~ 11.3 ng/L. Blank spiked water samples was at 1 &g/L, the relative standard deviation (RSD) ranged from 3.5% to 10.4%, the recovery is 77% ~ 105%. The method can be used for the determination of carbamates in water.
Key words:
dispersive solid- ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS)；water sample
同位素稀释-气相色谱-三重四级杆串联质谱（GC-MS/MS）法测定白酒中的塑化剂含量
王盛君1，雷雯2，杜晓宁*2，许旭1
(1. 上海应用技术学院，上海& . 上海化工研究院，上海& 200062)
摘要：以上海化工研究院研制的氘代邻苯二甲酸二甲酯（DMP-D6）和氘代邻苯二甲酸二乙酯（DEP-D10）为内标，利用三重四级杆气相色谱质谱联用仪（GC-MS/MS），建立了白酒中邻苯二甲酸二甲酯（DMP）和邻苯二甲酸二乙酯（DEP）的检测方法。其中，DMP和DEP的检测限分别为0.25和0.1 ng/mL，定量限为0.75和0.375 ng/mL，平均回收率96.5%和80.0%，精密度都小于5.4%，可满足白酒中DMP、DEP塑化剂的检测需求。
关键词：白酒；邻苯二甲酸二甲酯（DMP）；邻苯二甲酸二乙酯（DEP）；GC-MS/MS；同位素稀释质谱法
中图分类号：O657.63&&&&&& 文献标识码：A&&&&& 文章编号：（2015）
Determination of Phthalate Ester Residues in Liquor by Gas Chromatography Tandem Triple Quadruple Mass Spectrometry（GC-MS/MS）with Isotopic Internal Standards
WANG Sheng-jun1, LEI Wen2, DU Xiao-ning*2, XU Xu (1. Shanghai Institute of Technology, Shanghai 201418, C 2. Shanghai Research Institute of Chemical Industry, Shanghai 200062, China), Huaxue Shiji, )
Abstract: A method for analyzing dimethyl phthalate（DMP）and diethyl phthalate（DEP）in liquor by gas chromatography tandem triple quadruple mass spectrometry(GC-MS/MS) with isotopic internal standards, deuterated dimethyl phthalate(DMP-D6) and deuterated diethyl phthalate(DEP-D10), was established. The detection limit of DMP was 0.25 ng/mL, the quantification limit was 0.75 ng/mL, and the average recovery was 96.5%. The detection limit of DEP was 0.1 ng/mL, the quantification limit was 0.375 ng/mL, and the average recovery was 80.0%. The RSD was less than 5.4%, thus this method was suitable for phthalate esters detection in liquor.
Key words: dimethyl phthalate(DMP); diethyl phthalate(DEP); gas chromatography tandem triple quadruple mass spectrometry (GC-MS/MS); isotopic dilution mass spectrometry
含肉桂酸的聚丁二炔的合成及其可逆热致变色性能研究
张磊a，元以中*a, b, c，田晓慧*a, b, c，孙金煜a
（ 华东理工大学 a. 材料科学与工程学院；b. 超细材料制备与应用教育部重点实验室；c. 上海市先进聚合物材料重点实验室，上海& 200237）
摘要：将4-氨基肉桂酸和10, 12-二十五碳二炔酸的酰氯衍生物反应得到标题化合物，通过1HNMR、13CNMR、EI-MS和元素分析对其结构进行了表征。将单体超声分散，使其自主装形成囊泡，紫外光照之后得到聚丁二炔溶胶，其变色温度范围为20 ～ 90 ℃，颜色在紫色和红色之间可逆的变化。采用紫外可见光谱研究了其热致变色性能，实验结果表明，聚丁二炔溶胶具有完全可逆的、稳定的热致变色性能。
关键词：自主装；聚丁二炔溶胶；可逆热致变色
中图分类号：&&&&&&&&&&&&&&&& 文献标识码：A&&&&&&&&&&&& 文章编号：15)05
Synthesis and Reversible Thermochromic Properties of Polydiacetylenes with Cinnamic Acid Groups
ZHANG Leia, YUAN Yi-zhong*a, b, c, TIAN Xiao-hui* a, b, c, SUN Jin-yua (a. Schools of Materials Science and E b. Key Laboratory for Ultrafine Materials of Ministry of E c. Shanghai Key Laboratory of Advanced M China East University of Science and Technology, Shanghai 200237, China), Huaxue Shiji, )
Abstract: A diacetylene containing cinnamic acid as headgroup was synthesized by treating 4-aminocinnamic acid with 10, 12-pentacosadiynoic acid's chloride derivative and the structure was confirmed by 1HNMR, 13CNMR, EI-MS and elemental analysis. A suspension containing above diacetylene was dispersed by probe sonication, and then polymerized after UV irradiation forming a polydiacetylene sol. The heating-cooling cycle showed the reversible transformation between purple and red in the range of 20 ～ 70℃. The results suggest that the polydiacetylene containing cinnamic acid groups displayed completely reversibly thermochromic properties.
Key words: self- reversible thermochromism
吡啶-2,6-二[N-(1&-羟乙基)酰胺]的合成及其与金属离子的相互作用研究
罗世霞1，陈晓靓2，朱淮武1，顾曼琦1，卫钢3
（1. 贵州师范大学 化学与材料科学学院，贵州 贵阳& . 贵阳护理职业学院，贵州 贵阳& . CSIRO Manufacturing Flagship, PO Box 218, Lindfield, NSW 2070, Australia）
摘 要：合成了标题化合物 L，通过元素分析、1HNMR、13CNMR、IR及UV对其结构进行了表征，利用紫外光谱法考察了L对14种金属离子的识别性、萃取性和液膜传输性，讨论了它与金属离子之间的相互作用。结果表明，L对Cr3+、Pb2+离子具有良好的选择性识别作用及优良的萃取性和液膜传输性，它与两种金属离子均形成1:1型配合物，并可实现水样中Cr3+、Pb2+的含量分析。
关键词：吡啶酰胺；离子识别；萃取性；液膜传输
中图分类号：O626&&&&&&&&&&& 文献标识码：A&&&&&&&&&&&& 文章编号;15)05
Synthesis and Interaction of Metal Ions with Pyridine-2,6-bis[N-(1&-hydroxyethyl) carbamoyl]
LUO Shi-xia*1, CHEN Xiao-jing2 , ZHUHuai-wu1, GU Man-qi1, WEI Gang3 (1. School of Chemistry and Materials Science, Guizhou Normal University, Guiyang 550001, C 2. Guiyang Nursing Vocational College, Guiyang 550081, C 3. CSIRO Manufacturing Flagship, PO Box 218, Lindfield, NSW 2070, Australia), Huaxue Shiji, ),
Abstract: The pyridine amide molecule of pyridine-2, 6-bis[N-(1&-hydroxyethyl)carbamoyl] (L) has been synthesized and confirmedby using elemental analysis, 1HNMR, 13CNMR, IR and UV. The recognition, extraction and liquid membrane transport properties of L with fourteen metal ions had been investigated by the ultraviolet spectrophotometry, and followed by the discussions on& the interaction between L and metal ions. The results showed that L have a good selective recognition, extraction and liquid membrane transport properties for Cr(Ⅲ), Pb(Ⅱ) ions. The binding stoichiometry of L with two metal ions was 1:1, and the concentration of Cr(Ⅲ), Pb(Ⅱ) ions in water samples were determined.
Key words: P e liquid membrane transport
紫杉醇生物素标记衍生物的合成
巩凯*1，陈洁1，唐汝培*1, 2，陈敬华1
(1. 江南大学 药学院，江苏 无锡& . 安徽大学 生命科学学院，安徽 合肥& 230601)
&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&
摘要：以生物素、紫杉醇和6-氨基己酸为原料，经酰化反应、水解反应、酯化反应等步骤合成具有长臂连接的紫杉醇生物素标记物。在三乙胺催化下，生物素与N-羟基琥珀酰亚胺反应生成N-羟基琥珀酰亚胺生物素酯（a）。在氯化亚砜、甲醇反应体系下，由6-氨基己酸合成6-氨基己酸甲酯（b）。在三乙胺作用下，化合物a和化合物b反应生成生物素-氨基己酸甲酯（c）；化合物c在LiOH&H2O作用下，水解反应得到6-生物素氨基己酸（d）。以DMF为溶剂，在N, N'-二环己基碳二亚胺（DCC）、4-二甲氨基吡啶（DMAP）作用下，化合物d与紫杉醇反应，生成紫杉醇-连接臂-生物素衍生物（e）。目标化合物和重要中间体化合物采用IR、1HNMR、MS进行了表征。
关键词：紫杉醇；生物素；标记物；合成
中图分类号：O626.3&&&&&&& 文献标识码：A&&&&&&&& 文章编号：（2015）
Synthesis of Biotinylated Paclitaxel
GONG Kai*1, CHEN Jie1, TANG Ru-pei1,2, CHEN Jing-hua1 (1. School of Pharmaceutical Science, Jiangnan University, Wuxi 214122, C 2. School of Life Science, Anhui University, Hefei 230601, China), Huaxue Shiji, )
Abstract: A biotinylated paclitaxel with an extra-long chain spacer arm was synthesized via acylation reaction, hydrolysis reaction, esterification reaction steps from biotin, paclitaxel, and 6-aminohexanoic acid. The reaction of d-biotin with N-hydroxysuccinimide resulted in d-biotin N-succinimidyl ester (a) catalyzed by triethylamine. Methyl 6-aminohexanoate (b) was synthesized in thionyl chloride and CH3OH media. The reaction of d-biotin N-succinimidyl ester with methyl 6-aminohexanoate resulted in biotin-methyl 6-aminohexanoate (c) catalyzed by triethylamine. 6-Biotinamidohexanoic Acid (d) was prepared by the hydrolysis reaction of compound c under LiOH&H2O. With N, N&-dicyclohexylcarbodiimide (DCC) and 4-dimethylaminopyridine (DMAP), the reaction of compound d and paclitaxel resulted in the target compound (e). The structures were confirmed using IR, 1HNMR and MS.
Key words: synthesis
硫酸亚铁铵制备实验的研究
张婉佳﹡，李燕红，龚志强
（上饶师范学院 化学化工学院，江西 上饶& 334001）
摘要：设计了实验室制备硫酸亚铁铵的绿色化装置，计算出学生实验药品的基本用量，并从实验装置、反应液的pH控制、硫酸铵的反应状态和铁粉的用量等进行实验研究，归纳出实验异常结果与操作的对应关系表。
关键词：硫酸亚铁；硫酸亚铁铵；pH；硫酸铵
中图分类号：O611.66&&&&&&&&& 文献标识码：A&&&&&&&&&&& 文章编号：15)05
Preparation of Ferrous sulfate
ZHANG Wan-jia, LI Yan-hong, and Gong Zhi-qiang (College of Chemistry and Chemical Engineering, ShangraoNormalCollege, Shangrao 334001,China), Huaxue Shiji, ),
Abstract: In this work, the equipment for green chemistry is designed for the production of ferrous ammonium sulfate. The design is based on the chemistry theory of the production of ferrous ammonium sulfate. The amount of chemicals required for the experiment is calculated. The lookup table indicating the relation between the abnormal experiment result and the mistaken experiment operations is also derived. This lookup table is created based on the analysis of the equipment, the pH value of the solution, the status of the ammonium sulfate during reaction and the amount of the ferrous powder used in the reaction.
Key words: pH ferrous ammonium sulfate, ammonium sulfate
7-O-[&-(N-L-氨基酸甲酯)-烷基]-染料木素的合成与表征
杨雪梅*，杨宜球，麦桁棠，贾振斌
（广东医学院 药学院，广东 东莞& 523808）
摘要：染料木素具有多种生理活性，以染料木素和L-氨基酸为原料，经过染料木素烷基化、氨基酸酯化、两者偶联3步反应，合成了一系列新颖的7-O-[&-(N-L-氨基酸甲酯)-烷基]-染料木素，并对8个目标化合物进行了1HNMR、HRMS和IR结构表征。
关键词：染料木素；L-氨基酸甲酯；7-O-[&-(N-L-氨基酸甲酯)-烷基]-染料木素；合成
中图分类号：O621.3&&&&&&&& 文献标识码：A&&&&&&&&&& 文章编号：（2015）05
Synthesis and Characterization of 7-O-[&-(N-L-Amino Acid Methyl Ester)- Alkyl]-Genistein
YANG Xue-mei*, YANG Yi-qiu, MAI Heng-tang, JIA Zhen-bin &(School of Pharmacy, Guangdong Medical College, Dongguan 523808, China), Huaxue Shiji, ),
Abstract: Genistein has many biological activities, a series of novel 7-O-[&-(N-L-amino acid methyl ester)-alkyl]-genisteinderived from genistein and L-amino acidwas synthesized viathree-step reaction of the genistein alkylation, the amino acid esterification and the coupling reaction. The eight target compounds were confirmedby 1HNMR, HRMS and IR.
Key words: L-ami 7-O-[&-(N-L-amino acid methyl ester)-alkyl]- synthesis
3, 6-二氯水杨酸的合成研究
杜晓宇*,刘雁,陈芳,耿丽,牛彬波,刘伟
（河北工业大学& 化工学院，天津 &&&300130）
摘要：标题化合物是一种重要的医药中间体，也是合成高效、低毒除草剂麦草畏的关键中间体。以廉价易得的2, 5-二氯硝基苯为初始原料，经过水合肼还原、重氮化反应合成2, 5-二氯苯酚，再在高温高压下进行羧基化反应合成标题化合物。通过单因素实验，研究了以上反应的关键影响因素，得到了适宜的合成条件，标题化合物的收率为65.8%（以2, 5-二氯硝基苯计），纯度为99.24%，满足应用要求。该合成方法简单经济，产物纯度高，易于分离，收率较高。产物和中间体经过红外光谱和核磁共振波谱分析，表明其特征与标准物一致。
关键词：2, 5-二氯硝基苯；2, 5-二氯苯胺；2, 5-二氯苯酚；3, 6-二氯水杨酸；合成
中图分类号：&&&&&&&&&&&&&&&& 文献标识码：A&&&&&&&&&&&& &&&&文章编号：15)04
Synthesis of 3, 6-Dichlorosalicylic Acid
DU Xiao-yu*, LIU Yan, CHEN Fang, GENG Li, NIU Bin-bo, LIU Wei (School of Chemical Engineering, Hebei University of Technology, Tianjin 300130, China), Huaxue Shiji, )
Abstract: 3, 6-Dichlorosalicylic acid is a kind of important pesticide intermediate. It is also a key intermediate for production of herbicide dicamba. The route to synthesize the 3, 6-dichlorosalicylic acid is determined. The cheap and easy gained 2, 5-dichloronitrobenzene were choosed as initial raw materials. The intermediate 2, 5-dichlorophenol was obtained via the hydrazine hydrate reduction and the diazotization reaction. Then the target product 3, 6-dichlorosalicylic acid is obtained via carboxylation reaction by high temperature and pressure. The key reaction factors are investigated through single factor experiments, and optimum condition is obtained. The yield (calculated by 2, 5-dichloronitrobenzene) and the purity of 3, 6-dichlorosalicylic acid is 65.8% and 99.24%, respectively, and quality satisfies the commercial requirement. The synthetic method is simple and economic, and the target product has high purity and easy separated. The structure of 3, 6-dichlorosalicylic acid was confirmed via IR and NMR.
Key words: 2, 5- 2, 5- 2, 5- 3, 6-di&& synthesis
4-羟基吲哚的合成研究
王立中*，卞小琴，刘竺云，张文华，周晶晶
（泰州职业技术学院 制药与化学工程学院，江苏 泰州& 225300）
摘要：以2, 4-二硝基甲苯、多聚甲醛为起始原料首先合成2, 4-二硝基苯乙醇，然后经过还原、环合、脱氢3步合成获得4-羟基吲哚。考察了投料比的影响，得到了适宜的工艺条件，n(2, 6-二硝基甲苯)︰n(多聚甲醛)︰n(叔丁醇钾)＝1︰1.2 ︰0.16，n (2, 6-二硝基苯乙醇)︰n (85%水合肼) ＝1︰5，Pd/C催化剂为2 g。该反应路线操作简便，工艺路线可行。4步总收率达39.6%，产物经过熔点、IR、1HNMR、13CNMR等表征确证。
关键词：4-羟基吲哚；4-羟基吲哚啉；2, 4-二硝基苯乙醇；2, 4-二氨基苯乙醇
中图分类号：O626.13& &&&&&&&&&&&&&&&&&&文献标识码：A&& &&&&&文章编号：（2015）05
Synthesis of 4-hydroxyindole
WANG Li-zhong*, BIAN Xiao-qin, LIU Zhu-yun, ZHANG Wen-hua, ZHOU Jing-jing (Department of Pharmacy and Chemical Engineering, Taizhou Polytechnic College, Taizhou 225300,China), Huaxue Shiji, ),
Abstract：In order to explore the simple synthesis route of 4- hydroxyindole. 2,6-Dinitrophenylethanol was synthesized by 2,4-dinitrotoluene and formaldehyde as raw material, and then after reduction, cyclization, reduction of four step synthesis of the target product. Factors influencing the reaction yield were investigated，such as feed ratio．The optimum technical conditions： n(2,6-dinitrotoluene)：n (polyoxymethylene)：n (potassium tert-butoxide)=1：1.2 ：0.16, n (2,6-dinitrophenylethanol)：n (85% hydrazine hydrate)= 1：5 and Pd/C catalyst is 2g. The reaction route is simple, feasible process routes. After the four step reaction, the total yield was 39.6%, the product were confirmed via the melting point, IR, 1HNMR, 13CNMR.
Key words：4- 4- 2,6- 2,4-diaminophenylethanol
1, 1&-二甲基二茂铁合成新方法的研究
（承德石油高等专科学校，河北 承德& 067000）
摘要：近年来二茂铁及其衍生物的合成与应用研究成为金属有机化学界研究的热点问题，1, 1&-二甲基二茂铁就是一类重要的二茂铁衍生物，它在催化合成、生物学、医学等领域表现出越来越重要的作用。考察了1, 1&-二甲基二茂铁的几种合成路线，开发了一条反应条件温和、反应试剂易得、产率较高的新路线进行合成，成功地合成了目标产物，并对目标产物进行了熔点和1HNMR的分析。
关键词：二茂铁；1, 1&-二甲基二茂铁；合成
中图分类号：&&&&&& 文献标识码：A&&&&&&& 文章编号：（2015）05
Synthesis of 1,1&-dimethyl ferrocene
YANG Xi-qiang (Chengde Petroleum College, Chengde 067000, China), Huaxue Shiji, ),
Abstract: &In recent years, the synthesis and application of ferrocene and its derivatives have been a hot point in metal-organic chemistry. 1,1&-dimethyl ferrocene is an important& sort of ferrocene derivatives, it has showed its importance in fields such as& Catalytic synthesis, biology and medical, etc. the article studied several synthesis& routes of &1,1&-dimethyl ferrocene and developed a new synthesis route which has the advantage of& mild reaction condition, easy purchased reagents and high yield product. we synthesized& the goal product successfully and analysized its melt point and 1HNMR .
Key word: 1,1&- synthesis
曲酸双棕榈酸酯的合成
(徐州医药高等职业学校&&&&&& ，江苏 徐州& 221116)
摘要：以棕榈酸、氯化亚砜为原料，在60 ～ 65 ℃卤化合成棕榈酰氯；再以吡啶为催化剂、N, N-二甲基甲酰胺为溶剂，与曲酸酰化合成标题化合物，反应温度15 ～ 25 ℃，收率88.0%。该方法具有操作简单、成本低等优点，适合工业化生产。
关键词：曲酸双棕榈酸酯；棕榈酰氯；曲酸；棕榈酸；卤化；酰化
中图分类号：&&&&&&& 文献标识码：A&&&&&&& 文章编号：（2015）
Synthesis of Kojic Dipalmitate
SHEN Xin-an (Jiangsu Xuzhou Vocational College of Pharmaceutics, Xuzhou 221116, China), Huaxue Shiji, )
Abstract: Use palmitic acid, thionyl chloride as raw materials, palmitoyl chloride was synthesized in the halogenation reaction under the temperature of 60 ～ 65 ℃；and pyridine as catalyst, N, N-dimethyl formamide as solvent, 88.0% yield of kojic dipalmitate is synthesized with kojic acid in the acylation reaction under the temperature of 15 ～ 25 ℃. This method shows many advantages, such as easy operation and low cost, which can be feasible to large scale production.
Key words: acylation