反相液相制备色谱法结合超临界流体制备色谱法分离纯化海风藤中的化合物

引用本文: 辛华夏, 彭子悦, 江大森, 傅青, 金郁, 梁鑫淼. 反相液相制备色谱法结合超临界流体制备色谱法分离纯化海风藤中的化合物[J]. 色谱, 2018, 36(5): 474-479. doi: 10.3724/SP.J.1123.2017.11054 shu

Citation: XIN Huaxia, PENG Ziyue, JIANG Dasen, FU Qing, JIN Yu, LIANG Xinmiao. Separation and purification of compounds from piper kadsura using preparative reversed-phase liquid chromatography and preparative supercritical fluid chromatography[J]. Chinese Journal of Chromatography, 2018, 36(5): 474-479. doi: 10.3724/SP.J.1123.2017.11054 shu

反相液相制备色谱法结合超临界流体制备色谱法分离纯化海风藤中的化合物

辛华夏 ^1, ,
彭子悦 ^1, ,
江大森 ^1, ,
傅青 ^1, ,
金郁 ^1, ,
梁鑫淼 ^1,2,

1.
华东理工大学药学院, 上海 200237;
2.
中国科学院分离分析化学重点实验室, 中国科学院大连化学物理研究所, 辽宁大连 116023
基金项目:
中央高校基本科研业务费专项基金（222201717016）.

摘要: 建立了基于反相液相制备色谱和超临界流体制备色谱的组合方法，用于分离纯化醇提水沉后石油醚层中的海风藤。首先以甲醇作为改性剂，采用醇提水沉法去除海风藤甲醇提取物中的叶绿素，加入硅藻土后用石油醚回流富集目标成分。选用反相C18制备色谱柱将其分为18个组分，然后将组分在SFC模式下进行制备。选用酰胺色谱柱，以甲醇为改性剂，在柱温30℃、背压15.0 MPa的条件下进行分离。基于反相色谱和超临界流体色谱不同的分离选择性，最后分离得到6个高纯度化合物。该法展示了反相制备色谱和超临界流体制备色谱在海风藤分离纯化方面的优势，特别是超临界流体色谱在天然产物的分析和制备方面的巨大潜力。

关键词:

English

Separation and purification of compounds from piper kadsura using preparative reversed-phase liquid chromatography and preparative supercritical fluid chromatography

1.
School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China;
2.
Key Laboratory of Separation Science for Analytical Chemistry(CAS), Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
Received Date: 26 November 2017
Fund Project:
Fundamental Research Funds for the Central Universities (No. 222201717016).

Abstract: A method based on preparative reversed-phase liquid chromatography (prep-RPLC) and preparative supercritical fluid chromatography (prep-SFC) was developed for the separation and purification of compounds from piper kadsura. A pretreatment method was first developed, including methanol extraction, water precipitation, petroleum ether extraction, etc. Chlorophyll and other strong polar impurities were removed from the piper kadsura samples, and the target components were enriched in petroleum ether extracts. The piper kadsura samples were separated into 18 fractions on a Unitary C18 column (250 mm×20 mm, 5 μm) with water and methanol as the mobile phases. Then, the SFC parameters, including the column, modifier, temperature, and backpressure were optimized. The optimized conditions for prep-SFC were as follows:XAmide column (250 mm×20 mm, 5 μm), methanol as the modifier, 30℃ column temperature, and 15.0 MPa backpressure. Because of the good orthogonality of RPLC and SFC, six highly pure compounds were isolated, including kadsurenone, wallichinine, denudatin B, pellitorine, 2E-decenoic acid N-isobutylamide, and futoxide.

Key words:

supercritical fluid chromatography (SFC)
/ reversed-phase liquid chromatography (RPLC)
/ preparative (prep) chromatography
/ separation and purification
/ piper kadsura

1. [1] Song J L, Yuan L, Liu Y J, et al. Journal of Hubei University of Chinese Medicine, 2007, 9(3):70 宋敬丽, 袁林, 刘艳菊, 等. 湖北中医学院学报, 2007, 9(3):70
2. [2] Ma Y, Han G Q, Liu Z J. Acta Pharmaceutica Sinica, 1993, 28(3):207 马迎, 韩桂秋, 刘志坚. 药学学报, 1993, 28(3):207
3. [3] Ma Y, Han G Q, Wang Y Y. Acta Pharmaceutica Sinica, 1993, 28(5):370 马迎, 韩桂秋, 王银叶. 药学学报, 1993, 28(5):370
4. [4] Lin L C, Shen C C, Shen Y C, et al. J Nat Prod, 2006, 69, 842
5. [5] Li X M, Wang D Y, Liu H Q. Chinese Traditional Paten Medicine, 2005, 27(10):1199 李晓蒙, 王定勇, 刘慧琼. 中成药, 2005, 27(10):1199
6. [6] Kim K H, Choi J W, Ha S K, et al. Bioorg Med Chem Lett, 2010, 20, 409
7. [7] Zhang S X, Liu X K, Zhang L, et al. Natural Product Research and Development, 1992, 4(3):1 张顺祥, 刘星楷, 张莉, 等. 天然产物研究与开发, 1992, 4(3):1
8. [8] Yuan L.[MS Dissertation]. Hubei:Hubei University of Chinese Medicine, 2008 袁林.[硕士学位论文]. 湖北:湖北中医药大学, 2008
9. [9] Xin H X, Fu Q, Yuan Y, et al. J Supercrit Fluid, 2017, 127:9
10. [10] Kalikova K, Slechtova T, Vozka J, et al. Anal Chim Acta, 2014, 821:1
11. [11] Miller L. J Chromatogr A, 2012, 1250:250
12. [12] Zhang J, Chen X D, Li L Q, et al. Chinese Journal of Chromatography, 2016, 34(3):321 张晶, 陈晓东, 李丽群, 等. 色谱, 2016, 34(3):321
13. [13] Li D Y, Wu X, Hao F L, et al. Chinese Journal of Chromatography, 2016, 34(1):80 李冬艳, 吴锡, 郝芳丽, 等. 色谱, 2016, 34(1):80
14. [14] Desfontaine V, Guillarme D, Francotte E, et al. J Pharm Biomed Anal, 2015, 113:56
15. [15] Lemasson E, Bertin S, West C. J Sep Sci, 2016, 39(1):212
16. [16] Bernal J L, Martin M T, Toribio L. J Chromatogr A, 2013, 1313:24
17. [17] Hartmann A, Ganzera M. Planta Med, 2015, 81(17):1570
18. [18] Li Z Y, Fu Q, Li K Y, et al. Chinese Journal of Chromatography, 2014, 32(5):506 李振宇, 傅青, 李奎永, 等. 色谱, 2014, 32(5):506
19. [19] Yuan Y, Xin H X, Peng Z Y, et al. Chinese Journal of Chromatography, 2017, 35(7):683 袁云, 辛华夏, 彭子悦, 等. 色谱, 2017, 35(7):683
20. [20] Miller L. J Chromatogr A, 2014, 1363:323
21. [21] Miller L. J Chromatogr A, 2012, 1256:261
22. [22] Sarrut M, Corgier A, Cretier G, et al. J Chromatogr A, 2015, 1402:124
23. [23] Yang B C, Xin H X, Wang F E, et al. J Sep Sci, 2017, 40(16):3231
24. [24] Tarafder A, Hill J F. J Chromatogr A, 2017, 1482:65
25. [25] Tarafder A, Hudalla C, Iraneta P, et al. J Chromatogr A, 2014, 1362:278
26. [26] Duan S T.[MS Dissertation]. Shanghai:Fudan University, 2009 段书涛.[硕士学位论文]. 上海, 复旦大学, 2009
27. [27] Jochen R, Xiao P G, Rudolf B. J Ethnopharmacol, 2001, 75:133
28. [28] Chen Z N, Xu P J. Acta Pharmaceutica Sinica, 1993, 28(11):876 陈泽乃, 徐佩娟. 药学学报, 1993, 28(11):876
29. [29] Molina-Torres J, Salazar-Cabrera C, Armenta-Salinas C, et al. J Agric Food Chem. 2004, 52:4700

扫一扫看文章

计量

PDF下载量: 4
文章访问数: 862
HTML全文浏览量: 60

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

反相液相制备色谱法结合超临界流体制备色谱法分离纯化海风藤中的化合物

English

Separation and purification of compounds from piper kadsura using preparative reversed-phase liquid chromatography and preparative supercritical fluid chromatography

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

反相液相制备色谱法结合超临界流体制备色谱法分离纯化海风藤中的化合物

English

Separation and purification of compounds from piper kadsura using preparative reversed-phase liquid chromatography and preparative supercritical fluid chromatography

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs