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采用水蒸气蒸馏提取和一步高速逆流色谱法从斑鸠菊 essential oil 中制备分离生物活性化合物。

Preparative separation of bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze using steam distillation extraction and one step high-speed counter-current chromatography.

机构信息

State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Chaoyang District, Beijing, China.

出版信息

J Sep Sci. 2012 Oct;35(19):2608-14. doi: 10.1002/jssc.201200266. Epub 2012 Aug 21.

Abstract

In order to utilize and control the invasive weed, bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze were studied. Steam distillation extraction and one step high-speed counter-current chromatography were applied to separate and purify the caryophyllene oxide, 7,11-dimethyl-3-methylene-1,6,10-dodecatriene, and caryophyllene from essential oil of Flaveria bidentis (L.) Kuntze. The two-phase solvent system containing n-hexane/acetonitrile/ethanol (5:4:3, v/v/v) was selected for the one step separation mode according to the partition coefficient values (K) of the target compounds and the separation factor (α). The purity of each isolated fraction after a single high-speed counter-current chromatography run was determined by high performance liquid chromatography. A 3.2 mg of caryophyllene oxide at a purity of 92.6%, 10.4 mg of 7,11-dimethyl-3-methylene-1,6,10-dodecatriene at a purity of 99.1% and 5.7 mg of caryophyllene at a purity of 98.8% were obtained from 200 mg essential oil of Flaveria bidentis (L.) Kuntze. The chemical structures of these components were identified by GC-MS, (1) H-NMR, and (13) C-NMR.

摘要

为了利用和控制入侵杂草,对斑鸠菊(L.)挥发油中的生物活性化合物进行了研究。采用水蒸气蒸馏提取和一步高速逆流色谱法从斑鸠菊挥发油中分离和纯化石竹烯氧化物、7,11-二甲基-3-亚甲基-1,6,10-十二碳三烯和石竹烯。根据目标化合物的分配系数(K)和分离因子(α),选择含有正己烷/乙腈/乙醇(5:4:3,v/v/v)的两相溶剂系统用于一步分离模式。通过高效液相色谱法确定单次高速逆流色谱运行后每个分离馏分的纯度。从 200mg 斑鸠菊(L.)挥发油中获得了 3.2mg 纯度为 92.6%的石竹烯氧化物、10.4mg 纯度为 99.1%的 7,11-二甲基-3-亚甲基-1,6,10-十二碳三烯和 5.7mg 纯度为 98.8%的石竹烯。这些成分的化学结构通过 GC-MS、(1)H-NMR 和(13)C-NMR 进行了鉴定。

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