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液-液逆流色谱和超高压液相色谱:两种快速互补的分离方法,用于制备分离和分析芳香-massoia 内酯。

Hydrostatic countercurrent chromatography and ultra high pressure LC: Two fast complementary separation methods for the preparative isolation and the analysis of the fragrant massoia lactones.

机构信息

Laboratory of Pharmacognosy and Natural Products Chemistry, Department of Pharmacy, University of Athens, Panepistimiopolis-Zografou, Athens, Greece.

出版信息

J Sep Sci. 2010 May;33(9):1198-203. doi: 10.1002/jssc.200900818.

Abstract

Using a one-step preparative hydrostatic countercurrent chromatography method, the fragrant massoia lactones were purified from the crude massoia bark oil, in less than 3 h. The fractionation was performed with the biphasic solvent system c-hexane-methanol-water (10:9:1, v/v/v), leading to target compounds with purity over 96%, as determined by GC-MS and ultra high pressure LC-MS analyses. Together with C-10, C-12 and C-14 massoia lactones, two other aromatic compounds used in perfumes, benzyl benzoate and benzyl salicylate, were also obtained as pure compounds. In parallel, an easy and efficient ultra high pressure LC method was developed for the ultra-fast analysis of massoia lactones, as an alternative to long GC-MS methods.

摘要

采用一步制备性超高压逆流色谱法,从粗巴戟天树皮油中不到 3 小时即可纯化出芳香的密花巴戟素。通过两相溶剂系统正己烷-甲醇-水(10:9:1,v/v/v)进行分级,通过 GC-MS 和超高压 LC-MS 分析确定目标化合物的纯度超过 96%。与 C-10、C-12 和 C-14 密花巴戟素一起,还获得了两种用于香水的其他芳香化合物,即苯甲酸苄酯和水杨酸苄酯,均为纯化合物。同时,还开发了一种简单高效的超高压 LC 方法,用于超快速分析密花巴戟素,作为替代长 GC-MS 方法。

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