β-环糊精类（CDs）高效液相色谱手性分离材料的制备及应用
摘要
本论文分五部分：
1．概述了β—环糊精类衍生物作为高效液相色谱固定相和添加剂的合成和应用，对分离机理及协同效应进行了初步探讨。并介绍了农药样品的分析技术。
2．合成了β—环糊精键合硅胶手性柱填料，并自己装柱，考察了它的色谱性能。实验表明，它对手性化合物有较好的分离作用。实验中发现，不同的流动相、温度及pH值对分离产生不同的影响，通过多次实验，确定了它的最佳色谱分离条件。以β—环糊精、2，6-二甲基-β—环糊精和2，3，6-三甲基-β—环糊精为流动相添加剂，对“两相协同效应”做了初步探讨。
3．首次合成了新型二异氰酸酯桥连β—环糊精键合硅胶手性柱填料，并自己装柱，讨论了不同合成方法的利弊。考察了柱子的色谱性能。实验表明，它分离手性化合物的能力比β—环糊精柱的好。通过多次实验，确定了它的最佳色谱分离条件。同样以β—环糊精、2，6-二甲基-β—环糊精和2，3，6-三甲基-β—环糊精为流动相添加剂，对“两相协同效应”做了初步探讨。
4．首次合成了新型丁二酰氯桥连β—环糊精手性柱填料，并自己装柱。考察了柱子的色谱性能。实验表明，它对手性化合物有良好的分离能力。通过多次实验，确定了它的最佳色谱分离条件。同样以β—环糊精、2，6-二甲基-β—环糊精和2，3，6-三甲基-β—环糊精为流动相添加剂，对“两相协同效应”做了初步探讨。
5．我们使用自制的新型高效液相色谱柱(二异氰酸酯桥连β—环糊精柱)对环境样品——蔬菜上的残留农药进行测试，建立了番茄上两种农药残留的分析方法。结果表明，其具有操作简便、分析速度快、灵敏度高等优点。
This paper divides into 5 parts:
1. The article has stated β - cyclodextrin derivatives as the static phase of the high performance liquid chromatography and the composition of the chiral selector, at the same time we have discussed phenomenon of the mechanism and synergism preliminarily. And the analysis technology of the sample of agricultural chemical have also been introduced.
2. The synthesis of β - cyclodextrin chiral bounded static phase has been finished and packed column in our lab. we have investigated its performance of chromatography. Our results show that it is better in the selection of chiral chemical commpound. In the experiment we know, for different factors such as : mobile phase , temperature or pH has different effect. By large of magnitude experiments we have founded the best chromatographic conditions. So we selected β -cyclodextrin, 2, 6-dimethyl - β -cyclodextrin and 2, 3, 6-trimethyl - β -cyclodextrin as the chiral selector, and for " two-phase synergism " we make a further discussion.
3. We synthesized disocyanute bridged β- cyclodextrin as chiral bounded static phase for the first time, and packed column in our lab. We discussed different methods of synthesis, we have investigated its performance of chromatography. Our results show that it is better than β-cyclodextrin as chiral static phase in the selection of chiral chemical compounds. By large of magnitude experiments we have founded the best chromatographic conditions. So we selected β -cyclodextrin, 2,6-dimethyl - β -cyclodextrin and 2,3,6-trimethyl - β - cyclodextrin as the chiral selector, and for" two-phase synergism" we make a further discussion.
4.. We synthesized succinyl chloride bridged β - cyclodextrin as chiral static phase for the first time, and packed column in our lab. We discussed different length of the bridged linkage have done affect on the performance of the column. And we investigated its performance of chromatography. By large of magnitude experiments we have founded the best chromatographic conditions. So we selected β -cyclodextrin, 2, 6-dimethyl - β -cyclodextrin and 2 - oxygen - (2-hydroxypropyl) - β - cyclodextrin as the chiral selector, and for " two-phase synergism " we make a further discussion.
5. By using the high performance liquid chromatography which was packed in our lab (disocyanute bridged β - cyclodextrin column) to do the detective work on environmental sample -remaining agricultural chemical on vegetable , on the base of this we established the detective methods of two kinds of the remaining agricultural chemicals on tomato. As a result, show that it has operating and simple and convenient, analysis speed rapid, sensitivity high and other advantages.
1．概述了β—环糊精类衍生物作为高效液相色谱固定相和添加剂的合成和应用，对分离机理及协同效应进行了初步探讨。并介绍了农药样品的分析技术。
2．合成了β—环糊精键合硅胶手性柱填料，并自己装柱，考察了它的色谱性能。实验表明，它对手性化合物有较好的分离作用。实验中发现，不同的流动相、温度及pH值对分离产生不同的影响，通过多次实验，确定了它的最佳色谱分离条件。以β—环糊精、2，6-二甲基-β—环糊精和2，3，6-三甲基-β—环糊精为流动相添加剂，对“两相协同效应”做了初步探讨。
3．首次合成了新型二异氰酸酯桥连β—环糊精键合硅胶手性柱填料，并自己装柱，讨论了不同合成方法的利弊。考察了柱子的色谱性能。实验表明，它分离手性化合物的能力比β—环糊精柱的好。通过多次实验，确定了它的最佳色谱分离条件。同样以β—环糊精、2，6-二甲基-β—环糊精和2，3，6-三甲基-β—环糊精为流动相添加剂，对“两相协同效应”做了初步探讨。
4．首次合成了新型丁二酰氯桥连β—环糊精手性柱填料，并自己装柱。考察了柱子的色谱性能。实验表明，它对手性化合物有良好的分离能力。通过多次实验，确定了它的最佳色谱分离条件。同样以β—环糊精、2，6-二甲基-β—环糊精和2，3，6-三甲基-β—环糊精为流动相添加剂，对“两相协同效应”做了初步探讨。
5．我们使用自制的新型高效液相色谱柱(二异氰酸酯桥连β—环糊精柱)对环境样品——蔬菜上的残留农药进行测试，建立了番茄上两种农药残留的分析方法。结果表明，其具有操作简便、分析速度快、灵敏度高等优点。
This paper divides into 5 parts:
1. The article has stated β - cyclodextrin derivatives as the static phase of the high performance liquid chromatography and the composition of the chiral selector, at the same time we have discussed phenomenon of the mechanism and synergism preliminarily. And the analysis technology of the sample of agricultural chemical have also been introduced.
2. The synthesis of β - cyclodextrin chiral bounded static phase has been finished and packed column in our lab. we have investigated its performance of chromatography. Our results show that it is better in the selection of chiral chemical commpound. In the experiment we know, for different factors such as : mobile phase , temperature or pH has different effect. By large of magnitude experiments we have founded the best chromatographic conditions. So we selected β -cyclodextrin, 2, 6-dimethyl - β -cyclodextrin and 2, 3, 6-trimethyl - β -cyclodextrin as the chiral selector, and for " two-phase synergism " we make a further discussion.
3. We synthesized disocyanute bridged β- cyclodextrin as chiral bounded static phase for the first time, and packed column in our lab. We discussed different methods of synthesis, we have investigated its performance of chromatography. Our results show that it is better than β-cyclodextrin as chiral static phase in the selection of chiral chemical compounds. By large of magnitude experiments we have founded the best chromatographic conditions. So we selected β -cyclodextrin, 2,6-dimethyl - β -cyclodextrin and 2,3,6-trimethyl - β - cyclodextrin as the chiral selector, and for" two-phase synergism" we make a further discussion.
4.. We synthesized succinyl chloride bridged β - cyclodextrin as chiral static phase for the first time, and packed column in our lab. We discussed different length of the bridged linkage have done affect on the performance of the column. And we investigated its performance of chromatography. By large of magnitude experiments we have founded the best chromatographic conditions. So we selected β -cyclodextrin, 2, 6-dimethyl - β -cyclodextrin and 2 - oxygen - (2-hydroxypropyl) - β - cyclodextrin as the chiral selector, and for " two-phase synergism " we make a further discussion.
5. By using the high performance liquid chromatography which was packed in our lab (disocyanute bridged β - cyclodextrin column) to do the detective work on environmental sample -remaining agricultural chemical on vegetable , on the base of this we established the detective methods of two kinds of the remaining agricultural chemicals on tomato. As a result, show that it has operating and simple and convenient, analysis speed rapid, sensitivity high and other advantages.
引文
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2．刘国铃，余兆楼，柱色谱技术，北京：化学工业出版社，2000：198～203
3．陈慧，王琴孙，色谱[J]，1999(6)：533～538
4．陈国亮，张道道，化学通报[J]，1988(7)：1～6
5. Gunther K .Martens J. , Schickedan Z M, [J] Angew. Chem, Imt. Ed, Engl., 1984,23:506～518
6. Alak A, Armstrong D W.[J] Anal. Chem., 1986,58:582～599
7. Pitha J, Irie T, Sklar P B et al. Life Science, 1988,43(6):493～508
8. Szejtli J. J. Inclusion Phenom. Mol. Recognit. Chem., 1992,14(1): 25～30
9. Armstrong D W, Ward T J.[J]M 2:9 Chromatogr. 1986, 9:407～423
[10] 史坚，邵芸，邹公伟，色谱[J]，1995(6)443～446
11. C. Bichi, G. Artuffo, A. D. Amato, G. M. Nano. JHRC, 1991, 14:301～306
12. W. Keim, A. Khne, W. Meltzow. JHRC, 1991, 14:507～508
13．刘育，张毅民，孙世新等，高等学校化学学报。1995，16：1567～1568
14. X. Y. Shi, Y. Q. Zhang, J. H. Han, R. N. Fu. J Chromatogr, 2000, 52:200～204
15．童林荟．环糊精化学．基础与应用．北京：科学出版社，2001，33～36
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