通过逆流色谱法依次结合等度制备反相高效液相色谱法对印楝（Azadirachta indica）种子中的七种四降三萜类化合物进行纯化。

Purification of the seven tetranortriterpenoids in neem (Azadirachta indica) seed by counter-current chromatography sequentially followed by isocratic preparative reversed-phase high-performance liquid chromatography.

作者信息

Silva Júlio César T, Jham Gulab N, Oliveira Rosângela D'arc L, Brown Leslie

机构信息

Universidade Federal de Viçosa, Laboratório de Pesquisas de Produtos Naturais, Departamento de Química, Viçosa MG 36570-000, Brazil.

出版信息

J Chromatogr A. 2007 Jun 1;1151(1-2):203-10. doi: 10.1016/j.chroma.2007.03.086. Epub 2007 Mar 30.

DOI:10.1016/j.chroma.2007.03.086

PMID:17428489

Abstract

Counter-current chromatography (CCC) sequentially followed by isocratic preparative reversed-phase high-performance liquid chromatography was used to isolate the seven bio-actives (azadirachtin A, azadirachtin B, azadirachtin H, desacetylnimbin, desacetylsalannin, nimbin and salannin) from the seed concentrate (NSC) of the neem tree (Azadirachta indica A. Juss). Reproducible, narrow polarity range, high purity fractions were obtained from repeated injections of the NSC (700 mg loadings/injection), on to a relatively small volume CCC coil (116 mL). The CCC biphasic solvent system chosen was hexane:butanol:methanol:water (1:0.9:1:0.9, v/v). A mass balance of injected material showed that 95+% were recovered.

摘要

采用逆流色谱（CCC），随后进行等度制备反相高效液相色谱，从印楝（Azadirachta indica A. Juss）种子浓缩物（NSC）中分离出七种生物活性成分（印楝素A、印楝素B、印楝素H、脱乙酰印楝苦素、脱乙酰印楝素、印楝苦素和印楝素）。通过将NSC（每次进样量700 mg）重复进样到相对较小体积（116 mL）的CCC柱上，获得了可重现、极性范围窄、高纯度的馏分。所选用的CCC双相溶剂体系为己烷：丁醇：甲醇：水（1:0.9:1:0.9，v/v）。注入物质的质量平衡表明回收率为95%以上。