建立了超临界流体色谱快速分析吴茱萸中吲哚类生物碱的方法。以标准品混合物和复杂样品为对象比较4种色谱柱的分离效果，进行色谱柱的筛选；考察了进样体积、改性剂、添加剂、温度和背压对保留行为的影响。结果表明，进样体积对峰形影响显著；添加剂对保留时间和色谱峰形影响有限；改变改性剂能使保留时间显著改变；降低温度，升高背压，保留时间减小。经过优化，确定采用 Waters ACQUITY UPC2 BEH 色谱柱，以甲醇为改性剂，在35℃柱温和2.07×107 Pa背压条件下，15 min内完成复杂样品的分析。同时采用超高效液相色谱完成复杂样品的快速分析。结果表明，超临界流体色谱可用于天然产物的高效快速分析，同时该方法与超高效液相色谱在分离选择上的差异有助于天然产物分析方法的拓展。
A fast chromatographic separation of indole alkaloids from Evodiae fructus was developed by supercritical fluid chromatography( SFC). The initial screening of four stationary phases was investigated with a standard mixture of evodiamine and rutaecarpine,and a com-plex sample of indole alkaloids prepared from Evodiae fructus as probes. Later,the effects of chromatographic parameters on separation were studied including injection volume,organic modifier,additive,temperature and back pressure. The injection volume had significant impact on the peak shape. With the additives in the mobile phase,slight changes in peak shape and retention time were observed in separation. Variation in organic modifier led to dramatic change in chromatographic behavior. Both decreased temperature and increased back pressure short-ened the retention time. Finally,a fast analytical method using SFC,on a Waters ACQUITY UPC2 BEH column,methanol as modifier,under 35 ℃ and 2. 07×107 Pa,was developed to sep-arate a complex sample of indole alkaloids in less than 15 min. Another rapid approach for the separation of a complex sample of indole alkaloids was developed by using ultra-high perform-ance liquid chromatography( UHPLC). As a result,SFC can be used in the separation of natu-ral products,giving high performance,good resolution and fast analysis speed. The difference in selectivity with UHPLC can be used to the development of natural product separation.
参考文献
| [1] | 杨长龙;胡浩权;张维冰.[J].分析科学学报,200521(04):444. |
| [2] | 郭亚东.[J].天然产物研究与开发,200113(03):61. |
| [3] | 张怡评;洪专;方华.[J].中医药导报,201218(07):89. |
| [4] | 王学军;赵锁奇;王仁安.[J].色谱,200119(04):344. |
| [5] | 徐雪峰;沈爱金;郭志谋.[J].色谱,201331(03):185. |
| [6] | Taylor L T .LCGC North America[OL].http://www.chromatographyonline.com/lcgc/Misc/Separa-tion-of-Ionic-Analytes-via-Supercritical-Flu/ArticleStandard/Article/detail/605649,2009-06-01. |
| [7] | Miller L.[J].Journal of Chromatography A,20121250:250. |
| [8] | 张进治;汪瑗;陈惠.[J].光谱学与光谱分析,200727(05):944. |
| [9] | 张雪琴;周欣;王道平.[J].分析化学,200533(02):241. |
| [10] | Sun J;Baker A;Chen P.[J].Rapid Communications in Mass Spectrometry,201125(18):2591. |
| [11] | Okunji C O;Iwu M M;Ito Y.[J].Journal of Liquid Chromatography and Related Technologies,200528(05):775. |
| [12] | Liu R M;Chu X;Sun A L.[J].Journal of Chromatography A,20051074:139. |
| [13] | 杨敏;周萍;徐路.[J].分析测试学报,201029(07):743. |
| [14] | 邱时祎 .[D].上海:华东理工大学,2013. |
| [15] | Perrenoud A G G;Boccard J;Veuthey J L.[J].J Chrom-atogr A,20121262:205. |
| [16] | Chou F M;Wang W T;Wei G T.[J].Journal of Chromatography A,20091216:3594. |
| [17] | 张云;杜振霞;于文莲.[J].色谱,201432(01):52. |
| [18] | West C;Bouet A;Routier S.[J].Journal of Chromatography A,20121269:325. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%