多菌灵与3种环糊精的识别研究  

Study on Inclusion Behavior of Carbendazim with Cyclodextrins

作　　者：孙伟[1] 厍梦尧[1] 马思悦 陈娇 史真[1] 李剑利[1] 

机构地区：[1]西北大学化学与材料科学学院合成与天然功能分子化学教育部重点实验室,西安710127

出　　处：《分析化学》2018年第2期246-253,共8页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.21572177;21673173;J1210057);陕西省自然科学基金项目(Nos.2015J003;2016JZ004)资助~~

摘　　要：利用溶液法制备了疏水性药物分子多菌灵与β-环糊精、2-羟丙基-β-环糊精和2,6-二甲基-β-环糊精的包合物,在25℃时,通过核磁共振实验氢谱、二维ROESY和扩散排序DOSY的实验方法对多菌灵与3种环糊精的识别进行研究,得出了包合物的可能包合形式和3种环糊精与多菌灵包合后的扩散系数分别为D_(β-CD)=2.516×10^(-10)m^2/s,D_(2-Hp-β-CD)=1.676×10^(-10)m^2/s,D_(Me-β-CD)=2.046×10^(-10)m^2/s;通过X-射线粉末衍射、热重分析、红外光谱和扫描电镜发现,形成包合物后,环糊精和多菌灵的特征衍射峰均发生了变化,多菌灵的特征衍射峰10.4°,21.2°,25.8°,31.5°(2θ)消失或减弱;多菌灵热分解温度197.5℃,形成包合物后热分解温度提高到260℃以上;红外光谱的结果也表明,形成包合物后,环糊精空腔内的水峰振动明显减弱,说明环糊精的疏水空腔中水分子位置被多菌灵分子占据;扫描电镜的结果表明,包合物的外观不同于单体,说明有新的物相生成。Hydrophobic medicine carbendazim,come into inclusion compounds with β-cyclodextrin( β-CD),2-hydroxypropyl-β-CD( 2-Hp-β-CD) and 2,6-dimethyl-β-CD( Me-β-CD),were made by solvent method. By investigating the inclusion behaviors of these three cyclodextrins combined with carbendazim using 1H NMR,2D rotating frame overhause effect spectroscopy( ROESY) and diffusion ordered spectroscopy,the possible ways of combinations and the recognition ratio of this three inclusion compounds,D_(β-CD)=2.516×10^(-10)m^2/s,D_(2-Hp-β-CD)=1.676×10^(-10)m^2/s,D_(Me-β-CD)=2.046×10^(-10)m^2/s,were obtained. According to X-ray power diffraction, thermogravimetric analysis, infrared spectroscopy and scanning electron spectroscopy characterization,it was found that the characteristic diffraction peaks changed after carbendazim and cyclodextrin formed into inclusion compounds,and the characteristic diffraction peak of carbendazim at 10.4°,21.2°,25. 8°,31. 5°( 2θ) lost or disappear. The pyrolysis temperature of carbendazim was 197. 5℃,and would be higher than 260℃ after it formed inclusion complex. The infrared spectrum also showed that the oscillation peaks of inner cyclodextrin cavum apparently reduced after carbendazim combined, which demonstrated that the position of water molecules inside cyclodextrin cavum were occupied by the carbendazim molecules. With the help of SEM,the appearances of inclusion were different from a single carbendazim molecule,which manifested a new structure appeared.

关 键 词：多菌灵 环糊精 核磁共振 包合物 

分 类 号：TQ455[化学工程—农药化工]