全固态Z型Ag3PO4/RGO/Bi2WO6三元复合光催化剂可见光驱动高效降解四环素
姚慧*，孙海路，魏利民，高宝权，杨宏旭，庞春玲，李化
(辽源市食品质量安全检测中心，吉林 辽源 136200)
摘要：在日益增长的环境污染和能源短缺的情况下，光催化技术凭借其绿色、高效的特点，受到诸多科研工作者的关注。将Ag3PO4和Bi2WO6纳米晶体材料与氧化石墨烯相结合，构建全固态Z型Ag3PO4/RGO/Bi2WO6复合光催化剂，氧化石墨烯作为其中的电子传导介质，有效的将光生电子从Bi2WO6的导带转移到Ag3PO4的价带，从而有效的产生光生电子和空穴，较好的提高了光催化性能。实验结果发现，可见光照射下对四环素的降解率达91%。将为目前环境污染等相关领域提供一种有效的光催化剂的制备方法。
关键词：全固态Z型；石墨烯；光催化；四环素；磷酸银
中图分类号：TD33 文献标识码：A 文章编号：0258-3283（2018）
Synthesis of Ag3PO4/RGO/Bi2WO6 Composites with Highly Efficient Photocatalytic Activity: Efficient Visible-light Driven All-solid-state Z-scheme Photocatalyst YAO Hui*, SUN Hai-lu, WEI Li-min, GAO Bao-quan, YANG Hong-xu, PANG Chun-ling, LI hua （Food Quality Safety Inspection Center, Liaoyuan 136200, China）, Huaxue Shiji, 2018, 40(12)
Abstract: The photocatalytic technology as a kind of green and potential technology has been paid more and more attention in ever-increasing environmental pollution and energy shortage. In this work, a practical strategy is proposed to facilitate effectively the separation of photogenerated electrons and holes by addition of graphene oxide in Ag3PO4 and Bi2WO6 nanocrystals semiconductor composite. Compared with GO-single component, the three-component RGO-Ag3PO4/Bi2WO6 composites exhibited improved photocatalytic activity, with a degradation rate that reached up to 91% for tetracycline (TC) by visible light irradiation driven. Graphene oxide served as an electronic conduction medium is used to effectively transfer of the photogenerated electrons from the conduction band Bi2WO6 of to the valence band of Ag3PO4, the all-solid-state Z-Scheme photocatalytic mechanism was proposed. An effective method for development of pragmatic photocatalyst was provided in present environmental pollution, energy problems and other related fields.
Key words: all-solid-state Z-scheme; graphene; photocatalytic; tetracycline; Ag3PO4
“由下而上”一步水热法制备二硫化钼量子点及性能研究
李菁菁*1, 2, 郁莉婷2, 万法广2, 董超2, 郭鹏2, 郭红根2, 顾莹2
（1. 徐州医科大学附属医院 影像科，江苏 徐州 221006; 2. 徐州医科大学 医学影像学院，江苏 徐州 221004）
摘要：二硫化钼量子点（MoS2 QDs）因其优越的性能近年来备受关注。然而其制备方法和量子产率仍有改进空间。以L-半胱氨酸为硫源、钼酸铵为钼源，利用“由下而上”一步水热法制备二硫化钼量子点，制备得到的二硫化钼量子点单分散，粒径大小平均为5.3 nm。以硫酸奎宁为标准物，荧光量子产率为7.75%。同时，二硫化钼量子点表现出良好的光稳定性和溶液稳定性以及细胞生物相容性，可用于肿瘤细胞的荧光成像。
关键词：L-半胱氨酸；一步水热法；由下而上；二硫化钼量子点
中图分类号：R445.2 文献标识码：A 文章编号：0258-3283(2018)12--
Preparation and Performance of Molybdenum Disulfide (MoS2) Quantum Dots by One Pot “Bottom-up” Hydrothermal Approach LI Jing-jing*1,2, YU Li-ting2, WAN Fa-guang2, DONG Chao2, GUO Peng2, GUO Hong-gen2, GU Ying2 (1.Department of Radiology, Affiliated Hospital Xuzhou, Xuzhou 221006, China; 2.School of Medical Imaging, Xuzhou Medical University, Xuzhou 221004, China), Huaxue Shiji, 2018, 40(12)
Abstract: Molybdenum disulfide quantum dots (MoS2 QDs) have attracted much attention in recent years due to their superior properties. However, there is room for improvement in its preparation and quantum yield. Molybdenum disulfide quantum dots (MoS2 QDs) were prepared by a one pot “bottom-up” hydrothermal approach with L-cysteine as S source and ammonium molybdate as Mo source. Obtained MoS2 QDs were monodispersed with the average size of 5.3 nm and their photoluminescence quantum yield was estimated to be 7.75% using quinine sulfate as a fluorescent standard. Additionally, the excellent photo stability and solution stability as well as cell biocompatibility favored their applications in tumor cell fluorescence imaging.
Key words: L-cysteine; one pot hydrothermal approach; bottom-up; MoS2 quantum dots
新型碳纳米管接枝聚丙烯酸二茂铁甲酰氧丁酯纳米复合材料的制备及表征
旦智多杰1，张森2，徐峰*2，罗延龄2，张瑞乾2
（1.青海师范大学 民族师范学院 青海 西宁 810008，
2.陕西师范大学 化学化工学院 陕西省大分子重点实验室，陕西 西安 710062）
摘要：多壁羟基纳米管（MWCNTs-OH）在材料科学的各个领域显出了优异的物理、化学、机械等性能，已经成为纳米科学技术的重要组成部分之一。首先将多壁羟基纳米管与2-溴异丁酰溴（BIB）发生反应制备原子转移自由基聚合引发剂，然后采用ATRP法引发二茂铁基衍生物丙烯酸二茂铁甲酰氧丁酯（ABFC）聚合，制备得到标题化合物（MWCNTs-g-PABFC）纳米复合材料。采用红外光谱、拉曼光谱、热重法、紫外-可见吸收光谱、扫描电镜等一系列测试手段对纳米复合材料的结构及形貌进行表征。研究表明，聚丙烯酸二茂铁甲酰氧丁酯在碳纳米管表面的接枝有效地改善了碳纳米管在二氯甲烷中的分散稳定性，同时表现出显著的氧化还原电化学特性。
关键字：多壁羟基纳米管; 纳米复合材料; ATRP; 电化学性能
中图分类号：O646.1 文献标识码：A 文章编号：0258-3283(2018)12--
Preparation and Characterization of a New Type of Carbon Nanotube Graft Poly(4-acryloyloxybutyl ferrocene carboxylates) Nanocomposites DAN-ZHI Duo-jie1, ZHANG Sen2, XU Feng*2，LUO Yan-ling2, ZHANG Rui-qian2 (1. , Qinghai Normal University, Xining 810008, China; 2. Key Laboratory of Macromolecular Science of Shaanxi Province, School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi'an 710062, China), Huaxue Shiji, 2018, 40(12)
Abstract：Hydroxylated multi-walled carbon nanotubes (MWCNTs-OH) have become one of the important parts in nanoscience and nanotechnology due to their excellent physical, chemical and mechanical properties in various fields of material science. In this work , an atom transfer radical polymerization (ATRP) initiator was first obtained via the acylation reaction of MWCNTs-OH with 2-bromoisobutyryl bromide (BIB), and then a novel nanocomposite, multi-walled carbon nanotubes grafted poly(4-acryloyloxybutyl ferrocenecarboxylates) (MWCNTs-g-PABFC), was prepared by atom transfer radical polymerization of 4-acryloyloxybutyl ferrocene carboxylates (PABFC). The structure and morphology of the nanocomposites were confirmed by FTIR, Raman, TGA, UV-vis and FESEM. The experimental results showed that the grafting of PABFC on the surface of MWCNTs effectively improved the dispersion stability of MWCNTs in dichloromethane. Cyclic voltammetry (CV) determination showed that the novel MWCNTs-g-PABFC nanocomposites have an obvious redox electrochemical property.
Key words：multi-walled carbon nanotubes; nanocomposites; ATRP; electrochemical properties
水溶性黄绿色荧光硅量子点合成及对miRNA-21的检测
李春荣，孟铁宏*，余跃生，胡先运，赵鸿宾
（黔南民族医学高等专科学校 公共课教学部 贵州 都匀 558000）
摘要：相对于传统的Ⅱ/Ⅵ族、Ⅲ/V族族量子点，硅量子点以其良好的生物相容性和优越的光学性能在生物传感、荧光探针及医学诊断等领域受到广泛应用。以氨基乙基氨基异丁基甲基二甲氧基硅烷为硅前体，抗坏血酸钠和抗坏血酸为还原剂，水热法合成了水溶性黄绿色荧光的硅量子点。并利用红外光谱仪、X-射线光电子能谱仪、透射电子显微镜对硅量子点进行结构表征。对反应的影响因素如水浴反应时间、水浴温度、反应物的摩尔比、还原剂比例进行了考察和优化。制备的硅量子点对Cy5具有明显的淬灭行为。基于硅量子点对Cy5的淬灭行为，建立了Cy5标记单链DNA用于检测肿瘤标志物miRNA-21的方法。结果表明，该方法的检出范围为0.5 ～ 20 nmol/L，检出限为0.15 nmol/L，并具有良好的区分单碱基错配的能力。
关键词：硅量子点；miRNA-21；水热法；荧光检测
中图分类号：O657.3 文献标识码：A 稿件编号：0258-3283(2018)12--
Synthesis of Yellow-Green Water-Soluble Silicon Quantum Dots and Detection of miRNA-21
LI Chun-rong, MENG Tie-hong*, YU Yue-sheng, HU Xian-yun, ZHAO Hong-bin (Chemistry Teaching-Research Section of Basic Department, Qiannan Medical College for Nationalities, Duyun 558000, China ), Huaxue Shiji, 2018, 40(12)
Abstract: Compared with traditionalⅡ-Ⅵ, Ⅲ- V quantum dots, silicon quantum dots have been widely used in biosensing, fluorescence probe, medical diagnosis and other domains because of their good biocompatibility and excellent optical performance. A yellow-green fluorescent water-soluble silicon quantum dots was synthesized by hydrothermal method with N-(3-(Dimethoxy methylsilyl)isobutyl)-ethylenediamine as silica precursor, sodium ascorbic acid and ascorbic acid as reducing agents. The structures of silicon quantum dots were confirmed by IR, XPS and TEM. The water bath calefaction time, reaction temperature, reaction molar ratio and reductant ratio were optimized. Silicon quantum dots have prominent quenching character to Cy5. A analysis method of detection tumor marker miRNA-21 has been established based on the quenching efficiency of silicon quantum dots to Cy5. The results show that the detection linearity range is 0.5 ～ 20 nmol/L, LOD is 0.15 nmol/L, and the method has a good ability to distinguish single base mismatch.
Key words: silicon quantum dots; miRNA-21; hydrothermal method; fluorescent detection
含香豆素结构小分子有机胶凝剂的合成及胶凝行为研究
姜祎，徐虹，张化为，王乐，翁强，邓翀，赵鹏，宋小妹
（陕西中医药大学 药学院，陕西 咸阳 712046）
摘要：为探索含香豆素结构小分子有机胶凝剂在药剂领域中的应用，采用Williamson反应、酯化反应合成3个含香豆素结构的胆固醇类小分子胶凝剂，最高收率为83%。探讨了三苯基膦促进Williamson反应的机理。测试胶凝剂在10种溶剂中的胶凝能力，结果显示，3个小分子胶凝剂均有一定的胶凝能力，并且对于小极性溶剂（60-90石油醚、液体石蜡和植物油）表现出良好的胶凝能力，其中胆固醇-[3-（7-氧基香豆素）正丙基]碳酸酯和胆固醇-[3-（4-氧基香豆素）正丙基]碳酸酯的胶凝能力好于胆固醇-[3-（4-甲基-7-氧基香豆素）正丙基]碳酸酯，2%的胆固醇-[3-（7-氧基香豆素）正丙基]碳酸酯和胆固醇-[3-（4-氧基香豆素）正丙基]碳酸酯可以胶凝60-90石油醚、液体石蜡和植物油；5%的胆固醇-[3-（7-氧基香豆素）正丙基]碳酸酯还可以胶凝乙酸乙酯、DMF、乙醇、丙酮和甲苯；5%的胆固醇-[3-（4-氧基香豆素）正丙基]碳酸酯还可以胶凝乙酸乙酯、DMF、乙醇和丙酮；向5%的胆固醇-[3-（7-氧基香豆素）正丙基]碳酸酯/液体石蜡体系中加入1%的红霉素能显著缩短胶凝时间。SEM形貌观察研究表明，胶凝剂形成明显的自组装结构，不同浓度的胶凝剂形成的凝胶结构也不相同。为含香豆素结构小分子有机胶凝剂在药剂领域中的应用提供了依据。
关键词 香豆素；小分子有机胶凝剂；胆固醇；固-液互变
中图分类号：0648．1 文献标识码：A 文章编号：0258-3283（2018）
Synthesis and Gelation Behaviors of Coumarin-based Low Molecular Mass Organic Gelators JIANG Yi*, XU Hong, ZHANG Hua-wei, WANG Le, WENG Qiang, DENG Chong, ZHAO Peng, SONG Xiao-mei (College of Pharmacy, Shaanxi University of Chinese Medicine, Xianyang 712046, China), Huaxue Shiji, 2018, 40(12)
Abstract: To explore the application of coumarin containing small molecule organic gelling agent in the pharmacy, three new coumarin-based cholesterol low molecular mass organic gelators were synthesized via Williamson reaction and esterification reaction with yeild of 83%. The mechanism of Williamson reaction promoted by three phenyl phosphine was investigated. The gelation abilities were tested in 10 solvents. The results showed that these three gelators exhibited gelling ability,especial in small polar solvent(petroleum ether (60-90), liquid paraffinthe and plant oil). Compound 1 and 3 showed better gelling ability than compound 2 and could gel petroleum ether (60-90), liquid paraffinthe and plant oil with mass concentration of 2%. Compound 1 could futher gel ethyl acetate, DMF, ethanol, acetone and toluene with mass concentration of 5%. Meanwhile, compound 3 could futher gel ethyl acetate, DMF, ethanol and acetone with same mass concentration. The erythromycin could significantly shorten the gelation time of 5% of the compound 1-liquid paraffin system to 30 s. SEM showed that the gelators formed obvious self-assembling structure and the gel structure was different in different solvents. This work provides the basis for the application of coumarin containing small molecule organic gelling agent in pharmacy.
Key words: coumarin; low molecular mass organic gelator; cholesterol; liquid-solid phase transition
银纳米线的制备及应用研究进展
王成 许秋瑾*
（中国环境科学研究院，北京 100012）
摘要：银纳米线由于其优异的导电性和良好的延展性，被广泛研究并应用于制备透明导电薄膜。对已报到的银纳米线的制备方法进行系统总结，包括模板法和液相合成法，分析对比了两种方法的优缺点，并对目前研究较多的液相合成法中涉及的表面活性剂、成核缓释剂的作用做了详细阐述，为银纳米线的可控合成提供了参考。银纳米线作为最有可能替代传统ITO透明电极的材料，相关研究表明银纳米线的长度、直径对透明电极的性能有很大的影响，为后续优化银纳米线的制备指明了方向。
关键词：银纳米线; 制备方法; 透明导电薄膜
中图分类号：0622.4 文献标识码：A 文章编号：0258-3283(2018)12--
Recent Progress in Synthesis and Application of Silver Nanowires Wang Cheng, Xu Qiu-jin* (Chinese Research Academy of Environmental Sciences, Beijing 100012, China), Huaxue Shiji, 2018, 40(12), Abstract：Silver nanowires (Ag NWs) have sparked an immense interest from both academic and industrial researches due to the excellent optical, electric, and malleable properties. The common preparation methods of Ag NWs are summarized, including template method and liquid phase synthesis method and the advantages and disadvantages are comparably analyzed. The functions of surfactants and the nucleation slow-release agents used in liquid phase synthesis method are summarized in detail. The limitation of their wide use are deeply discussed in this work in order to provide the powerful support for the further study of Ag NWs. At current, the most important and promising application of Ag NWs is in the field of flexible transparent conductive films (TCFs), where they serve as the essential raw materials. Relevant studies show that the length and diameter of silver nanowires have great influence on the performance of transparent electrodes, which points out the direction for further optimization of the preparation of silver nanowires.
Key words：Silver nanowires; preparation methods; transparent conductive films
全球太阳能光伏政策研究及其产业发展趋势
王维利
（内蒙古财经大学 节能监管中心，内蒙古 呼和浩特 010051）
摘要：随着全球能源形势趋紧，使用可再生、可持续的太阳能能源取代传统化石能源，于近年得到迅速发展，不同的国家制定了一系列政策、法规用以鼓励太阳能及太阳能相关产业的发展，例如强制光伏上网电价，税收减免政策，贸易制度等，用以提高可再生资源的利用率，为了使光伏产业在激烈竞争中持续健康发展，满足国际可持续发展战略的需要。详细介绍了不同国家的太阳能扶持政策，并对产业发展趋势进行了分析。
关键词：太阳能；全球；政策；趋势
中图分类号：TM914 文献标识码：A 文章编号：0258-3283（2018）
Policy and Industrial Development Tendency of Global Solar Energy WANG Wei-li（Center of Energy Conservation and Supervision, Inner Mongolia University Finance and Economics, Hohhot 010051, China）, Huaxue Shiji, 2018, 40(12)
Abstract: As the global energy supply is facing severe constraint，Solar energy, as a new durative energy, has been developed rapidly in recent years. Different countries have formulated Solar energy policies to reducing dependence on fossil fuel and increasing domestic energy production by Solar energy. A variety of policies like feed-in-tariff (FIT), tax credits, trading systems etc. have been developed and implemented to promote the use of renewable energy. For global industry developing healthily and continually in intense competition and meeting the need of international sustainable development strategy, This work provides details on Solar energy policies implemented on the different countries of the world, and Solar energy industry development tendency is also analyzed in this work as well.
Key words: Solar energy; global; policies; tendency
芳香族氨基酸二肽金属配合物与DNA作用研究
杜秀红*1，崔节虎2，刘隽1，行书丽1
（1.河南医学高等专科学校 检验系，河南 郑州 451191；2.郑州航空工业管理学院 环境功能材料重点实验室，河南 郑州 450015）
摘要：芳香族氨基酸二肽类配体，具有特殊的芳香性侧链结构、良好的理化性质及生理相容性等优势，使芳香族氨基酸二肽金属配合物成为新型金属配合物抗癌药物研究的热点。通过系统研究芳香族氨基酸二肽金属配合物与DNA作用，可为设计、开发新型抗癌药物奠定基础。重点综述芳香族氨基酸直链二肽类金属配合物、芳香族氨基酸环二肽类金属配合物和芳香族氨基酸二肽有机金属配合物与DNA作用的研究进展。
关键词：抗癌药物；芳香族氨基酸二肽；芳香族氨基酸二肽金属配合物；DNA
中图分类号: O641.4 文献标识码：A 文章编号：0258-3283（2018）
Study on the interaction of metal complexes of aromatic amino acid dipeptide with DNA
DU Xiu-Hong*1, CUI Jie-Hu2, LIU Jun1, XING Shu-Li1 (1.Department of Laboratory Medicine, Henan Medical College, Zhengzhou 451191, China; 2. Key Laboratory of Environment Functional Materials, Zhengzhou University of Aeronautics, Zhengzhou 450015, China), Huaxue Shiji, 2018, 40(12)
Abstract：The aromatic amino acid dipeptide ligand has the advantages of special aromatic side-chain structure, good physical and chemical properties and physiological compatibility. By virtue of these advantages, the aromatic amino acid dipeptide metal complexes become a hotspot in the research of new anticancer drugs. Through systematically studying the interaction of aromatic amino acid dipeptide metal complexes with DNA, it can lay a good foundation for the design and development of new anticancer drugs. The research progress of the metal complexes of linear chain aromatic amino acids dipeptide, the metal complexes of cyclic chain aromatic amino acids dipeptide and organic metal complexes of aromatic amino acids dipeptide interacting with DNA are reviewed.
Key words：anti-cancer drug; aromatic amino acid dipeptide; metal complex of aromatic amino acid dipeptide; DNA
大叶藜指纹图谱研究及相似度分析
武芸*a，王春林b，胡浩斌a，张腊腊a，韩明虎a
（陇东学院 a. 化学化工学院，b. 生命科学与技术学院，甘肃 庆阳 745000）
摘要: 通过大叶藜紫外指纹图谱（UVFP）、红外指纹图谱（IRFP）结合化学计量学方法建立快速鉴别大叶藜药材的多维指纹图谱。采集10个不同产地的大叶藜样品190~700 nm的UVFP和4 000~400 cm-1的IRFP，分别反映中药化学组分中π→π*、n→π*、n→σ*化学信息和多种化学单键、双键、三键等化学振动（转动）对中红外线的吸收，建立其共有模式，并结合聚类分析和相似度分析构建多维指纹图谱。结果显示，UVFP、IRFP相结合构建的多维指纹图谱技术可实现对中药化学成分的全面检测。多维指纹图谱技术是一种综合鉴别中药质量的有效可行的方法，较任何单一方法更能准确揭示中药复杂系统的真实本源。
关键词：大叶藜；紫外指纹图谱；红外指纹图谱；相关系数；聚类分析
中图分类号：R 284.1 文献标识码：A 文章编号：0258-3283（2018）
Fingerprint Spectrum and Similarity Analysis of Chenopodium hybridum L. WU Yuna, WANG Chun-linb, HU Hao-bina , MA Shi-rongb, HAN Ming-hua (a. College of Chemistry and Chemical Engineering, b. College of Life Science and Technology, Longdong University, Qingyang 745000, China), Huaxue Shiji, 2018, 40(12)
Abstract： An evaluation method of Chenopodium hybridum L. from different areas was established by adopting the ultraviolet spectrum fingerprints (UVFP) and infrared spectrum fingerprints (IRFP) and with the stoichiometry. UVFP(199 ～ 700 nm) includes the chemical information of the chemical constituents (π→π*、n→π* and n→σ*) and IRFP in the range of 4000 ～ 400 cm-1 includes the absorption capacity to mid-infrared of chemical bond vibration (rotation) including single bond, double bond and triple bond were all recorded of Ch- enopodium hybridum L. Samples from ten different areas of China, established common pattern combining with the stoichiometry and similarity analysis to identify Chenopodium hybridum L. The combination of UVFP and IRFP achieved the overall monitoring of traditional Chinese medicine. The multidimensional fingerprints method was an effective and feasible method to comprehensively identify and objectively quantify traditional Chinese medicine quality, which can more accurately reflect the origin of the complex system of traditional Chinese medicine than any single method.
Key words：Chenopodium hybridum L.; UVFP; IRFP; correlation coefficient; clustering analysis
超声-微波协同萃取-液相色谱法检测口红中的4种色素
李军德a，王亚楠b，宋吉英*a
（青岛农业大学 a. 校医院，b. 化学与药学院，山东 青岛 266109）
摘要：采用超声-微波协同萃取法提取了口红中的苋菜红、胭脂红、诱惑红和罗丹明B这4种色素，并采用液相色谱法检测其含量。结果表明，用丙酮作提取剂、提取温度20 ℃、微波功率300 W、萃取时间为30 min时，提取效果最佳；色谱分析采用Eclipse Plus C18柱，甲醇和0.02 mol/L乙酸铵溶液(pH 4)为流动相进行梯度洗脱，流动相流速1.0 mL/min，柱温30 ℃，检测波长510 nm。在以上条件下提取检测，目标产物线性关系良好，平均回收率范围为91.7% ～ 103.5%，相对标准偏差为1.7% ～ 4.6%。
关键词：超声-微波协同萃取法；液相色谱法；口红；色素
中图分类号:O657 文献标识码: A 文章编号：0258-3283（2018）
Determination of Four Pigments in Lipstick by Ultrasonic-microwave Synergistic Extraction withLiquid Chromatography LI Jun-dea, WANG Ya-nanb, SONG Ji-ying*a (a. Hospital of Qingdao Agricultural University, b. College of Chemistry &Pharmacy, Qingdao Agricultural University, Qingdao 266109, China), Huaxue Shiji, 2018, 40(11),
Abstract：In this work, ultrasound-microwave synergistic extraction forfour pigmentswhichincluded amaranth, carmine, allura red andrhodamine B was used to extract from the pigment. A method based on liquid chromatography enabling determination of the pigment contents was developed. The results indicated that the optimal extractant, extractiontemperature, microwave power and extraction time wereacetone, 20 ℃,300 watt and 30 minutes, respectively. Liquid chromatography analysis was performed on Eclipse Plus C18 column. Methanol and 0.02 mol/L ammonium acetate was mobile phase in gradient elution. The flow rate was 1.0 mL/min, the column temperature was 30 ℃ and the detection wavelength located at 510 nm. Under the optimal conditions, the calibration curves of the targets showed good linearity. The average recoveries ranged from 91.7% to 103.5% with RSDs of 1.7%～4.6%.
Key words: ultrasound-microwave synergistic extraction; liquid chromatography; lipstick; pigment
邻苯二甲酸二丁酯-D4制备及其溶液标准物质均匀性稳定性研究
孙雯1, 2，邓晓军3，李美华*1, 2
(1.上海化工研究院有限公司，上海 200062；2.国家同位素工程技术研究中心 上海分中心，上海 200062；3.上海市检验检疫科学技术研究院，上海 200135)
摘要：采用质谱（MS）、红外光谱（IR）及核磁共振（NMR）对所制备原料邻苯二甲酸二丁酯-D4进行定性分析，优化并建立了邻苯二甲酸二丁酯-D4纯度及同位素丰度的测定方法，以液相色谱和气相色谱两种方法进行纯度定值，以电喷雾离子源（ESI）和电子轰击离子源（EI）两种方法进行丰度定值。以甲醇作为基体溶液，采用重量-重量法制备邻苯二甲酸二丁酯-D4溶液标准物质，分别采用方差分析法和直线拟合法对所制备溶液标准物质的浓度及同位素丰度进行了均匀性检验和稳定性监测。经检验，所研制的邻苯二甲酸二丁酯-D4溶液标准物质满足均匀性和稳定性要求。
关键词：邻苯二甲酸二丁酯-D4；标准物质；均匀性；稳定性
中图分类号：0652.1 文献标识码：A 文章编号：0258-3283（2018）
Study on Preparation of Dibutyl Phthalate-D4 and Uniformity and Stability of the Solution Reference Materials SUN Wen1, 2, DENG Xiao-jun3, LI Mei-hua*1, 2 (1.Shanghai Research Institute of Chemical Industry CO.,LTD., Shanghai 200062, China; 2.National Isotope Engineering Technology Research Center-Shanghai Sub-Center, Shanghai 200062, China; 3.Shanghai Research Institute of Inspection and Quarantine Science and Technology, Shanghai 200135, China), Huaxue Shiji, 2018, 40 (11),
Abstract：Mass spectrometry (MS), infrared (IR) and nuclear magnetic resonance (NMR) were used to confirm the structure of dibutyl phthalate-D4. The analytical method of the isotope abundance and chemical purity of dibutyl phthalate-D4 was developed, the purity was certified by liquid chromatography (HPLC) and gas chromatography (GC), the isotopic abundance was certified by electron spray ionization (ESI) and electron impact ion source (EI). Dibutyl phthalate-D4 solution reference was prepared in methanol according to weight- weight method. The uniformity test and stability monitoring of the concentration of the standard substance and the isotopic abundance of the prepared solution were carried out by the method of variance analysis and the linear fitting method. The dibutyl phthalate-D4 solution reference materials was tested to meet the requirements of the state for the uniformity and stability of the reference materials.
Key words：dibutyl phthalate-D4; reference material; uniformity; stability
霍乱弧菌核酸标准物质定值方法：ICP-MS法和数字PCR法
梁文*,李妍,许丽,李兰英,闻艳丽,杨雪,罗超,刘刚
（上海市计量测试技术研究院 化学与电离辐射所生物计量实验室, 上海 201203）
摘要：霍乱弧菌是人类霍乱的病原体，霍乱是一种古老且流行广泛的烈性传染病之一。曾在世界上引起多次大流行，主要表现为剧烈的呕吐、腹泻、失水，死亡率甚高，属于国际检疫传染病。霍乱弧菌定量检测质粒标准物质，霍乱弧菌的外膜蛋白编码基因ompW为靶基因，可作为霍乱弧菌核酸扩增（PCR）荧光检测试剂盒中的阳性物质替代物。构建霍乱弧菌质粒DNA标准样品，采用电感耦合等离子体质谱（ICP-MS）方法和数字PCR两种方法定值，最终定值结果为（79.2±5.2）ng/μL，可为霍乱弧菌核酸检测的量值准确性、可比性和有效性提供保障。
关键词：霍乱弧菌；ICP-MS；数字PCR
中图分类号：Q819文献标识码：A文章编号：0258-3283(2018)12--
Quantification of Plasmid DNA Reference Material for Vibrio choleraebyusingICP-MS and Digital PCR LIANG Wen*, LI Yan, XU Li, LI Lan-ying, WEN Yan-li, YANG Xue, LUO Chao, LIU Gang (Lab of Biometrology, Chemical and Ionizing Radiation Metrolology Institute, Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China), Huaxue Shiji, 2018, 40(12)
Abstract: Vibrio cholerae is the pathogen of human cholera, and cholera is an ancient and widespread infectious disease. It as an international quarantine infectious disease has caused many pandemics in the world, and mainly manifested as severe vomiting, diarrhea, dehydration, and high mortality rate. Vibrio cholerae plasmid reference material (RM), containing a target gene coding the outer-membrane protein ompW of Vibrio cholerae. It can be used as a positive substance substitute in polymerase chain reaction (PCR) fluorescence detection reagent kit for Vibrio Cholerae. Plasmid DNA reference material for Vibrio cholerae analysis and performed the quantification by using two different methods: inductively coupled plasma mass spectrometry (ICP-MS) and digital PCR. The result was (79.2±5.2) ng/μL. Reference material will play important role for the accuracy, comparability, and effectiveness of the Vibrio cholerae quantification.
Key words: Vibrio cholerae; ICP-MS; digital PCR
基于咔唑和间苯二甲酸的荧光配体合成及性能
姜涛，郭崇伟，邱文革*，白广梅，张桂臻，何洪
（北京工业大学 环境与能源工程学院 绿色催化与分离北京市重点实验室，北京 100124）
摘要：以咔唑、5-羟基-1,3-苯二甲酸二乙酯和1,4-二溴丁烷为原料，经缩合、水解等步骤合成了一种新型荧光配体N-[4-(3,5-二羧基苯氧基)-丁基]咔唑，并利用傅立叶变换红外光谱、核磁共振氢谱及单晶X-射线衍射对其结构进行了表征。该目标化合物具有强的荧光特性。在乙醇/水混合介质中，Fe3+的存在会导致目标化合物的荧光强度显著降低，显示出高效的Fe3+选择性“开-关”行为。最大淬灭率达到86 %，这种强的荧光猝灭效应是目标化合物和Fe3+离子发生配位作用的结果。荧光滴定实验和体系红外光谱数据表明，在溶液中目标化合物与Fe3+ 之间的结合是一种多分子的协同配位模式。
关键词：咔唑衍生物；荧光配体；三价铁离子；配位作用
中图分类号：O626.13 文献识别码：A 文章编号: 0258-3283(2018)12--
Synthesis and Property of Fluorescent Ligand Based on Carbazole and Isophthalic Acid JIANG Tao, GUO Chong-wei, QIU Wen-ge*, BAI Guang-mei, ZHANG Gui-zhen, HE Hong (Beijing Key Laboratory for Green Catalysis and Separation, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124, China), Huaxue Shiji, 40(12),
Abstract: A new fluorescent ligand，N-[4-(3,5-dicarboxylphenoxy)-butyl]-carbazole, was synthesized from carbazole, diethyl 5-hydroxyisophthalate and 1,4-dibromobutane through condensation and hydrolysis. And its molecular structure was confirmed by Fourier transform infrared spectroscopy, nuclear magnetic resonance spectra and X-ray single-crystal diffraction. This compound has strong fluorescence property. In ethanol/water solution, the fluorescence intensity at 352 nm decreased significantly in the presence of Fe3+ due to the coordination with Fe3+ ion, indicating an efficient Fe3+-selective “on–off” behavior. The quenching rate was up to 86 %. The results of fluorescence titration experiment and infrared spectroscopy of the system indicated a polymolecular cooperative coordination binding mode between compound and Fe3+.
Key words: carbazole derivative; fluorescent ligand; ferric iron; coordination
甲基苯偶氮芳香醛液晶异构化动力学及光电性能
郑敏燕*，侯雅慧，张国伟，郭妮，贾瑶，袁戈
（咸阳师范学院 化学与化工学院，陕西 咸阳 712000）
摘要：以偶氮类液晶化合物4-(4-(4-甲基苯酰氧)苯偶氮)苯甲醛为目标化合物，研究了在不同溶剂（甲醇、四氢呋喃）条件下，紫外光（365 nm）照射一定时间，其反-顺光异构化反应的动力学过程。并通过电化学方法，在两种溶剂（无水四丁基高氯酸铵或KCl水溶液为电解质）条件下，测定了样品在无水和水体系中反-顺光异构化过程中电化学性质的变化。结果表明，该化合物在甲醇、四氢呋喃两种溶剂条件下光异构化反应均为一级速率过程，且在四氢呋喃中的转化率高于甲醇中的转化率；循环伏安曲线表明在不同体系中，该偶氮化合物反-顺光异构化反应的HOMO和LUMO轨道能量及能级差（能隙）也在不断变化，且反式结构的能隙高于光稳态结构。
关键词：动力学；异构化；光电性能；偶氮芳香醛液晶
中图分类号：O625.4 文献标识码：A 文章编号：0258-3283（2018）
Isomerization Kinetics and Photo-electric Properties of Methyl Phenyl Azo Aromatic Aldehyde ZHENG Min-yan*, HOU Ya-hui, ZHANG Guo-wei, GUO Ni, JIA Yao, YUAN Ge（College of Chemistry and Chemical Engineering, Xianyang Normal University, Xianyang 712000, China), Huaxue Shiji, 2018, 40(12)
Abstract: The reaction kinetics of trans-cis photoisomerization of the methyl benzoyl azo aryl aldehyde in different solvents(methanol and tetrahydrofuran) under irradiation of UV light of 365 nm at a certain time was investigated in this work. Electrochemical methods were used to determine the electrochemical properties of the sample in the process of isomerization by using methanol and tetrahydrofuran as solvents with anhydrous ammonium tetrabutyl perchlorate (anhydrous ) or KCl solution(aqueous system) as electrolytes. The photoisomerization reaction of the compound is a first order rate process in each of the solvents, and the conversion rate of the compound in THF is higher than that in the methanol. The energy level curve of the cyclic voltammetry curve showed the HOMO, LUMO and energy gap（Eg）were changed during the isomerization process. The energy gap of the trans isomer is higher than that of photostabilization structure.
Key words: kinetics; isomerization; photo-electric properties; azo aromatic aldehyde
含羟基氧杂蒽荧光染料的合成及其荧光成像应用
曾红，吴洁，李媛艳，范小林，吴勇权*
（赣南师范大学 化学化工学院 江西省有机药物化学重点实验室，江西 赣州 341000）
摘要：近年来，氧杂蒽类荧光染料具有很多优点而被广泛应用。由于近红外荧光染料用于荧光成像，具有光损伤小、组织穿透性大和背景荧光干扰小的优点。设计与合成了具有羟基的氧杂蒽衍生物染料NIR-1和NIR-2。通过核磁共振谱和质谱确认了荧光染料的结构。利用紫外可见吸收光谱和荧光光谱对其光谱性能进行研究，结果表明NIR-1和NIR-2最大吸收波长分别为642 nm和607 nm，其最大发射波长分别为748 nm和752 nm。最后，对含羟基氧杂蒽荧光染料用于细胞和活体的荧光成像标记进行研究，结果表明NIR-1具有良好的细胞和活体荧光标记成像效果。
关键词：氧杂蒽；紫外-可见吸收光谱；荧光光谱；荧光成像
中图分类号: O625.15 文献标识码: A 文章编号：0258-3283(2018)12--
Synthesis of Hydroxy-substituted Xanthene Fluorescent Dyes for Fluorescence Imaging
ZENG Hong, WU Jie, LI Yuan-yan, FAN Xiao-lin, WU Yong-quan* (Key Laboratory of Organo-pharmaceutical Chemistry，School of Chemistry and Chemical Engineering, Gannan Normal University, Ganzhou 341000，China)，Huaxue Shiji, 2018, 40(12)
Abstract: In recent years, xanthene-based organic fluorescent dyes have been widely used because of their many advantages. Due to the strong penetration property of near-infrared (NIR) light, NIR dyes have been used for fluorescence imaging. Xanthene dyes NIR-1 and NIR-2 were synthesized with hydroxyl group. Meanwhile, their structures were confirmed by 1HNMR and HR-MS. The photophysical properties of xanthene NIR-1 and NIR-2 were investigated by UV-vis spectroscopy and fluorescence spectroscopy. The maximum absorption wavelength of NIR-1 is 642 nm; the maximum emission wavelength is 748 nm. The maximum absorption wavelength of NIR-2 is 607 nm, and the maximum emission wavelength is 752 nm. At last, the fluorescence labeling effect of xanthene derivatives for imaging was tested. The results indicated that the NIR-1 can be used for fluorescence imaging in living cells and in vivo.
Key words: Xanthene; UV-visible absorption spectrum; fluorescence spectrum; fluorescence imaging
黄酮衍生物的设计、合成及抗2型糖尿病活性
黄元政1，朱盼虎1，李家明*1, 2，刘万冬1，杨雨1
(1.安徽中医药大学 药学院，安徽 合肥 230038；2.安徽省中医药科学院 药物化学研究所，安徽 合肥 230038)
摘要：合成新型黄酮衍生物，并研究其抗2型糖尿病活性。以氯乙酸乙酯、对羟基苯甲醛为起始原料，经烃化、水解、Claisen-Schmidt缩合、环合等步骤，得到6个黄酮类化合物。采用高脂饮食+ STZ（链脲佐菌素）诱导2型糖尿病模型检测化合物对TG、TC、Glu含量的影响。目标化合物结构经1HNMR、13CNMR、MS确证。药理结果显示：黄酮衍生物表现出一定的的降低血清中TG、TC、Glu含量的作用。该新型黄酮衍生物具有一定的抗2型糖尿病活性。
关键词：黄酮；糖尿病；合成；链脲佐菌素
中图分类号：R916 文献标识码：A 文章编号：0258-3283（2018）
Design, Synthesis and Biological Evaluation of Flavonoid Derivatives against Type 2 Diabetes HUANG Yuan-zheng1, ZHU Pan-hu1, LI Jia-ming*1, 2, LI wan-dong1, YANG Yu1 (1.College of Pharmacy, Anhui University of Chinese Medicine, Hefei 230038, China; 2.Department of Medicinal Chemistry, Anhui Academy of Chinese Medicine, Hefei 230038, China), Huaxue Shiji, 2018, 40 (11),
Abstract: To synthesize a series of new flavonoid derivatives and evaluate their against type 2 diabetes, six novel flavonoid derivatives were synthesized by utilizing ethyl chloroacetate, p-hydroxybenzaldehyde as starting material, subsequently undergoing alkylation, hydrolysis, Claisen-Schmidt, cyclization, and so on. The antidiabetic biological evaluation in high-fat diet and streptozotocin (STZ) induced type 2 diabetes animal model. The structure of target compounds was characterized by 1HNMR, 13CNMR and MS. The results of antidiabetic activities showed that flavonoid derivatives exhibited potential reduction in serum Glu, TG, TC levels. The novel flavonoid derivatives have potential activitives against type 2 diabetes.
Key words: flavonoid; diabetes; synthesize; streptozotocin
5-磺基水杨酸中SO42-的去除研究
张路家，顾学峰，韩国清，戴惠明*
(永华化学科技（江苏）有限公司，江苏 常熟 215538)
摘要：提供了一种降低5-磺基水杨酸中硫酸根的方法。将5-磺基水杨酸结晶后的剩余母液加入至5-磺基水杨酸粗品内，常温搅拌0.5 h。由于5-磺基水杨酸母液为饱和溶液，对5-磺基水杨酸的粗品溶解度较小，而对附着在粗品表面的硫酸溶解度较大，所以通过过滤可将粗品中的硫酸大部分去除。再将母液洗涤后的粗品加纯水溶解，过D345阴离子交换柱，进一步降低5-磺基水杨酸中残留的硫酸，然后加活性炭过滤，经浓缩、冷却结晶、离心、干燥，所得产品的硫酸根含量与常规工艺相比大幅度降低，合格品的收率远远高于传统工艺。浓缩结晶后的母液可以循环再利用，此方法节约了生产成本，提高了产品质量，是一种比较经济可行的处理方法。
关键词：5-磺基水杨酸；硫酸根；水杨酸
中图分类号： TQ 216 文献标识码：A 文章编号：0258-3283（2018）
Reducing of SO42- from 5-Sulfosalicylic Acid ZHANG Lu-jia, GU Xue-feng, HAN Guo-qing, DAI Hui-ming (Yonghua Chemical Technology (Jiangsu) Co., Ltd., Changshu 215538, China), Huaxue Shiji, 2018, 40(12)
Abstract：This work provides a method for reducing sulfate in 5-sulfosalicylic acid. After crystallization of 5-sulfosalicylic acid, the mother liquor was added to the crude 5-sulfosalicylic acid and stirred at room temperature for 0.5 h. Since the 5-sulfosalicylic acid mother liquor is a saturated solution, the solubility of the crude product of 5-sulfosalicylic acid is small, and the solubility of sulfuric acid attached to the surface of the crude product is relatively large. Therefore, most of the sulfuric acid in the crude product is removed by filtration. The crude product washed with the mother liquor is then dissolved in purified water and passed through a D315 anion exchange column to further reduce the residual sulfuric acid of 5-sulfosalicylic acid, and then the activated carbon is filtered, concentrated, cooled and crystallized, centrifuged, and dried. The sulfate content of the product is greatly reduced compared with the conventional process. The yield of qualified products is much higher than traditional processes. The concentrated and crystallized mother liquor can be recycled and reused. This method saves production costs and improves product quality. It is a more economical and feasible treatment method.
Key words：5- sulfonylsalicylic acid; sulfate; salicylic acid
聚乙二醇水溶液中无配体钯催化的Suzuki反应
李新民*，陈正军，胡庆红，张玉婷，王征琴，袁泽利*
(遵义医学院 药学院，贵州 遵义 563000)
摘要：以聚乙二醇水溶液为反应介质，70 mol% K2CO3为碱，0.3 mol% Pd(OAc)2为催化剂，在空气氛围下实现了含有多种官能团溴代（杂环）芳烃与芳基硼酸的高效Suzuki偶联反应，合成了30个联芳环化合物。该体系仅需加入少量碱且无需加入对空气敏感的膦配体，即降低了实验操作的难度又避免了因副产物较多而造成的分离困难。该体系底物官能团兼容性好，产品分离收率最高达98%；且该方法可用于制备克级的药物中间体沙坦联苯。
关键词：聚乙二醇；无配体；Suzuki 反应；少量碱
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283（2018）
Palladium Catalyzed Ligand-Free Suzuki Reaction in Polyethylene glycol/H2O LI Xin-min*, CHEN Zheng-jun, HU Qing-hong, ZHANG Yu-ting, WANG Zheng-qin, YUAN Ze-li* (College of Pharmacy, Zunyi Medical University, Zunyi 56300, China), Huaxue Shiji, 2018, 40(12)
Abstract：In the presence of 0.3 mol% Pd(OAc)2 and 70 mol% K2CO3, various hetero/aryl bromides coupled with arylboronic acids in aqueous polyethylene glycol to afford biaryl products with excellent yields. This protocol shows tolerate to a diverse array of functionalized aryl bromides and boronic acids, and the highest biaryl product yield up to 98% without using any phosphine ligands. Moreover, this method allows the preparation of the core intermediate of valsartan in gram quantities in good yield.
Key words：polyethylene glycol; ligand-free; Suzuki reaction; reducing base
无溶剂加成酯化法合成羧酸环己酯的研究
李鑫1，朱鑫东1，洪永如1，李心忠*1,2,3
(1.闽江学院 海洋学院 化工与材料系，福建 福州 350108；2.绿色染整福建省高校工程研究中心，福建 福州 350108；3.福建省中国漆新型材料工程研究中心，福建 福州 350108 )
摘要：以两种磺酸基官能化季铵盐、Keggin构型杂多酸为构建单元，通过分子自组装合成的具有类核壳结构多磺酸基官能化杂多酸阴离子杂化体8S3SiIH、6S2PIH为非均相催化剂，采用一锅法在无溶剂反应条件下，由环己烯与碳数从1~4的直链脂肪酸经一步直接加成酯化反应合成了系列羧酸环己酯。确定的最佳反应条件为，n（环己烯）∶n（羧酸）∶n（杂化体）=1∶2.5∶0.015，反应温度 95~130 ℃，反应时间4 h，目标酯分离产率44%~93%。离子杂化体经过滤、乙醚洗涤、真空干燥即可再生循环使用，循环使用5次后催化活性基本保持不变。
关键词：杂多酸；离子杂化体；加成酯化；羧酸环己酯
中图分类号：TG225.52 文献标识码：A 文章编号：0258-3283（2018）
Synthesis of Cyclohexyl Carboxylic Esters by Direct Addition Esterification under Solvent-
free Conditions LI Xin1, ZHU Xin-dong 1, HONG Yong-ru1, LI Xin-zhong*1,2,3 (1.Department of Chemical and Materials of Ocean College, Minjiang University, Fuzhou 350108,China; 2. Green Dyeing and Finishing Eingineering Research Centre of Fujian University, Fuzhou 350108, China; 3. Fujian Engineering Research Center of New Chinese Lacqure Material, Fuzhou 350108), Huaxue Shiji, 2018, 40(12)
Abstract：Addition esterification of cyclohexene with aliphatic catalyzed by two multi-SO3H functionalized multi-heteroplyanion-based ionic hybrids with core-shell structure under solvent-free conditions was investigated. Under optimum conditions of n（cyclohexene）：n（acid）：n（ionic hybrid）=1：2.5：0.015, the reaction range from 95-130 ℃ within 4 hours, the corresponding cyclohexyl carboxylic esters was obtained with yields of 44% to 93%. Two ionic hybrids could be easily recycled after filtration, washed with diethyl ether and reused five times with keeping in the catalytic activity.
Key words：polyoxometalate; ionic hybrids; addition esterification; cyclohexyl carboxylic esters
苯甲酸阿格列汀合成工艺的改进
韩在褀1，刘颖1，马晶杰1，时元泰1，董琳琳1，尹树铸1，梁承武1，王锰*2，昌盛*1
(1. 吉林医药学院 药学院，吉林 吉林 132013；2.北华大学 药学院，吉林 吉林 132013)
摘要：以3-甲基-6-氯尿嘧啶、2-氰基溴苄为起始原料，在碱性条件经亲核取代反应得到2-(6-氯-3-甲基-2,4-二氧代-3,4-二氢-2H-嘧啶-1-基甲基)-苄腈，再与(R)-3-氨基哌啶二盐酸盐取代得到(R)-2-[(6-(3-氨基哌啶-1-基)-3-甲基-2,4-二氧代-3,4-二氢嘧啶-1(2H)-基)甲基]苄腈，最后与苯甲酸成盐以69.61%的总收率得到苯甲酸阿格列汀，纯度＞99.5%。该合成工艺反应条件温和、成本低廉，适用于工业化生产。
关键词：苯甲酸阿格列汀；合成；改进
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283（2018）
Improved synthesis of alogliptin benzoate HAN Zai-qi1, LIU Ying1, MA Jing-jie1, SHI Yuan-tai1, DONG Lin-lin1, YIN Shu-zhu1, LIANG Cheng-wu, WANG Meng*2, CHANG Sheng*1 (1. College of Pharmacy, Jilin Medical University, Jilin 132013, China; 2. College of Pharmacy, Beihua University, Jilin 132013, China), Huaxue Shiji, 2018, 40(11),
Abstract: Alogliptin was synthezied by reacted with (R)-3-aminopiperdine dihydrochloride and 2-(6-chloro-3-me-thyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl)-benzo-nitrile which was produced by the nucleophilic substitution reaction of 3-methyl-6-chloro-uracil and 2-bromomethyl-benzonitrile. Alogliptin was reacted with benzoic acid to yield alogliptin benzoate in total yield of 69.61% as well as purity more than 99.5%. The optimized synthetic conditions were mild, low cost, and was suitable for industrial production.
Key words: alogliptin benzoate; synthesis; improvement
3-甲基戊酸糠醇酯的合成研究
张改红，杨静，程传玲，毛多斌，张月丽，白冰*
（郑州轻工业学院 食品与生物工程学院，河南 郑州 450002）
摘要：以3-甲基戊酸为原料，经酰氯化、酯化反应，合成了香料3-甲基戊酸糠醇酯。考察了催化剂用量、反应物配比、反应时间、反应温度等对目标化合物收率的影响，结果表明：最佳合成工艺条件为：n（3-甲基戊酰氯）: n（吡啶） ＝ 1：2，n（糠醇）:n（3-甲基戊酰氯） ＝ 1：1.2，反应时间4 h，反应温度50 ℃，收率达87.8%。利用IR、1HNMR、13CNMR对目标化合物结构进行了表征。
关键词：3-甲基戊酸；糠醇；3-甲基戊酸糠醇酯；香料
中图分类号：0626.11 文献标识码：A 文章编号：0258-3283(2018)12--
Synthesis of Furfuryl 3-Methylpentanoate ZHANG Gai-hong, YANG Jing, CHENG Chuan-ling, MAO Duo-bin, BAI Bing* (School of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 45002, China) , Huaxue Shiji, 2018, 40(12)
Abstract: Furfuryl 3-methylpentanoate as a flavor was synthesized from 3-methylpentanoic acid by chlorination and esterification reactions．The reaction process was optimized by adjusting the catalyst dosage, reactant ratio, reaction time, reaction temperature to reveal the effects of these factors on yield of the targeted product. And the optimum conditions were as follows: the mole ratio of 3-methylvaleryl chloride to catalyst pyridine was 1.0 : 2.0, mole ratio of furfuryl alcohol to 3-methylvaleryl chloride was 1.0:1.2, reaction time was 4h, and reaction temperature was 50 ℃, the yield of compound 3 was up to 87.8%. The product was confirmed by IR, 1HNMR,13C NMR．
Key words: 3-methylpentanoic acid；furfuryl alcohol；furfuryl 3-methylpentanoate；flavor
