在酸性条件下,将自制的葫芦[7]脲均匀地涂覆到102白色硅藻土担体上,制得葫芦[7]脲气相色谱固定相.采用红外光谱、质谱、元素分析和热重分析表征了葫芦[7]脲在载体表面的结构.利用相关探针测定了新固定相的麦氏常数,表征了其基本色谱性能.考察了葫芦[7]脲气相色谱固定相填充柱对芳香烃、卤代烃、醇、酮、酯及硅氧烷的分离能力.结果表明,葫芦[7]脲固定相热稳定性高,柱色谱性能稳定,对较广泛的化合物尤其对高沸点的酯类及硅氧烷类化合物显示出良好的色谱分离能力(7 min内分离),作为气相色谱固定相有较好的应用前景.初步讨论了葫芦[7]脲固定相对上述化合物的分离机理.
参考文献
| [1] | Lehn J M.Supramolecular Chemistry-Scope and Perspective.Molecules,Supramolecules and Molecular Derives[J].Angew Chem Int Ed,1988,27:89-112. |
| [2] | Lee J W,Samal S,Selvapalam N,et al.Cucurbituril Homologues and Derivatives:New Opportunities in Supramolecular Chemistry[J].Acc Chem Res,2003,36(8):621-630. |
| [3] | LIU Simin,WU Chengtai.Recent Progress in Studies of Cucurbituril[J].Prog Chem,2005,17 (1):143-150(in Chinese).刘思敏,吴成泰.葫环联脲新进展[J].化学进展,2005,17(1):143-150. |
| [4] | Xu L,Liu S M,Wu C T,et al.Separation of Positional Isomers by Cucurbit[7]uril Mediated Capillary Electrophoresis[J].Electrophoresis,2004,25:3300-3306. |
| [5] | LI Laisheng,WANG Shangwen,LIU Chao,et al.Preparation of Glycoluril and Perhydroxycucurbit[6]uril GC Stationary Phase and Comparative Studies on Their Separation Performances[J].Acta Chim Sin,2007,65 (17):1855-1862 (in Chinese).李来生,王上文,刘超,等.甘脲和羟基葫芦[6]脲气相色谱固定相的制备及其色谱分离性能比较研究[J].化学学报,2007,65(17):1855-1862. |
| [6] | Li L S,Wang S W,Chen X Q,et al.Studies on Chromatographic Properties of Perhydroxycucurbit[6]uril as a New Type of Gas Chromatographic Column Packing Material[J].Chinese J Chem,2008,26 (2):307-314. |
| [7] | XING Songmin,WANG Yilu.Synthesis of Silicone and Product Applications[M].Beijing:Chemical Industry Press,2000:271 (in Chinese).幸松民,王一璐.有机硅合成工艺及产品应用[M].北京:化学工业出版社,2000:271. |
| [8] | QU Changling.Progress in Pyridylazo Reagents[J].Chem Reag,1986,8 (4):211-221(in Chinese).曲长菱.吡啶偶氮试剂的进展[J].化学试剂,1986,8(4):211-221. |
| [9] | LIU Xiaomei,WU Beiyan,YAN Jinlian.GC Analysis of γ-Aminopropyl-triethoxysilane[J].Silicone Mater,2003,17(6):18-20(in Chinese).刘晓梅,吴北阳,颜金莲.γ-氨丙基三乙氧基硅烷的气相色谱分析[J].有机硅材料,2003,17(6):18-20. |
| [10] | ZHOU Tingting,CHEN Guanxi,WU Qingzhou,et al. Separation and Analysis of Low-boiling Residues of Methylchlorosilanes[J].J Instrum Anal,2009,28(12):1448-1451 (in Chinese).周婷婷,陈关喜,吴清洲,等.甲基氯硅烷低沸物的分离分析[J].分析测试学报,2009,28(12):1448-1451. |
| [11] | SHEN Yiwen,QU Jichuan,ZHANG Hongdu.Gas Chromatography Analysis of Chlorosilanes[J].Chinese J Chromatogr,1997,15(13):246-247(in Chinese).沈怡文,曲吉川,张洪度.氯硅烷的气相色谱分析[J].色谱,1997,15(13):246-247. |
| [12] | XIA Yuzheng,JIAO Shuke.Synthesis and Characterization of Glycoturil[J].J Beijing Univ Chem Technol(Nat Sci Ed),1990,17(3):73-76(in Chinese).夏宇正,焦书科.甘脲的合成与鉴定[J].北京化工学院学报(自然科学版),1990,17(3):73-76. |
| [13] | ZHANG Guiling,LUO Xuqiang.Synthesis and Continuous Separation of Cucurbit[n]uril[J].Chinese J Synth Chem,2008,16(3):322-324(in Chinese).张桂玲,罗绪强.瓜环的合成及其连续分离[J].合成化学,2008,16(3):322-324. |
| [14] | Day A,Arnold A P,Blanch R J,et al.Controlling Factors in the Synthesis of Cucurbituril and Its Homologues[J].J Org Chem,2001,66(24):8094-8100. |
| [15] | LUO Xuqiang,ZHANG Guiling,XUE Saifeng,et al.Progress in Synthesis and Separation Method of a New Family Function Material Compounds-Cucurbit[n]urils[J].Guizhou Chem Ind,2003,28 (24):1-4 (in Chinese).罗绪强,张桂玲,薛赛凤,等.一类新型功能材料化合物——瓜环的合成与分离研究进展[J].贵州化工,2003,28(24):1-4. |
| [16] | Meschke C,Buschmann H J,Schollmeyer E.Synthesis of Mono-,Oligo-and Polyamide-Cucurbituril Rotaxanes[J].Macromol Rapid Commun,1998,19 (1):59-63. |
| [17] | WANG Shangwen.Study on Applications of Cucurbituril and Its Derivatives in Chromatography[D].Nanchang:Nanchang University,2007:41-42(in Chinese).王上文.葫芦脲及其衍生物在色谱中的应用[D].南昌:南昌大学,2007:41-42. |
| [18] | LIU Guoquan,YU Zhaolou.Chromatographic Column Technology[M].2nd Edition.Beijing:Chemical Industry Press,2006:46-48(in Chinese).刘国诠,余兆楼.色谱柱技术[M].第2版.北京:化学工业出版社,2006:46-48. |
| [19] | YU Zhongjian,LONG Yicheng,LUO Chongjian.Investigation on a New Porous Polymer Bead[J].Acta Chim Sin,1990,48(3):287-294(in Chinese).余仲健,龙义成,罗崇健.一种新型的高分子小球的研究[J].化学学报,1990,48(3):287-294. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%