Separation of an Effective Component of Ligustilide from Volatile Oil of Angelica Sinensis by High Speed Countercurrent Chromatography and Its Analysis and Identification by GC-MS
摘 要
提出了应用高速逆流色谱从当归挥发油中分离有效成分藁本内酯,探索这一分离条件的关键是两相溶剂体系的选择。根据分离目标物的极性以及选择两相溶剂应满足的3个条件(1分层时间不超过30 s;2对样品不引起分解;3目标成分的分配系数在0.5~2.0之间),经薄层色谱法及高效液相色谱法预选,最终从几种溶剂体系中筛选得到两相溶剂体系为正己烷-乙酸乙酯-乙醇-水(1+1+1+1)体系。采用这一溶剂体系,一次进样500 mg当归挥发油,可达到目标组分与其他杂质完全分离,目标组分回收后得到48 mg藁本内酯。对此分离所得组分经气相色谱-质谱法(GC-MS)分析,其纯度达到98.5%以上,GC-MS还对此组分进行结构鉴定,证明其确为藁本内酯。
Abstract
High speed countercurrent chromatography (HSCC) was applied to the separation of an effective component of ligustilide from volatile oil of Angelica sinensis. The key to the success of this separation was the choice of the bi-phase solvent system. Based on the polarity of the target component and on the 3 essential requirements (i.e. 1 time of phase separation should be less than 30 s; 2 without leading to decomposition of the sample; 3 values of distribution coefficient K of the targent components should be in the range of 0.5-2.0) which should be followed in the choice of the bi-phase solvent system, the solvent system of n-hexane-ethylacetate-ethanol-water (1+1+1+1) was sieved among some other candidate solvent systems in the preliminary screening by TLC and HPLC. By using the selected bi-phase solvent system in the HSCC separation, when a portion of the oil sample (500 mg) was introduced, 48 mg of ligustilide was obtained after separation. As shown by the results found in the GC-MS study on the separated ligustilide, its purity attained to a high value of more than 98.5%, and through structural study, the compound was identified to be ligustilide.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201810009
所属栏目 工作简报
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收稿日期 2017/10/26
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备注金晶,讲师,主要从事色谱分析工作
引用该论文: JIN Jing,TONG Shengqiang. Separation of an Effective Component of Ligustilide from Volatile Oil of Angelica Sinensis by High Speed Countercurrent Chromatography and Its Analysis and Identification by GC-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(10): 1163~1167
金晶,童胜强. 高速逆流色谱法分离当归挥发油中有效成分藁本内酯及其气相色谱-质谱法的分析和鉴别[J]. 理化检验-化学分册, 2018, 54(10): 1163~1167
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【9】YAN J Z, CHEN G, TONG S Q, et al. Preparative isolation and purification of germacrone and curdione from the essential oil of the rhizomes of Curcuma wenyujin by high-speed counter-current chromatography[J]. Journal of Chromatography A, 2005,1070(1/2):207-210.
【10】TONG S Q, LU M X, CHU C, et al. Selective isolation of components from natural volatile oil by countercurrent chromatography with cyclodextrins as selective reagent[J]. Journal of Chromatography A, 2016,1444:99-105.
【11】XIONG Y K, ZHU G H, ZHANG J Q, et al. Purification of ferulic acid, senkyunolide I and senkyunolide H from the volatile oil of Rhizoma Chuanxiong using high-speed countercurrent chromatography and preparative liquid chromatography[J]. Advanced Materials Research, 2014,1033/1034:259-264.
【12】QUEIROGA C L, CAVALCANTE M Q, FERRAZ P C, et al. High-speed countercurrent chromatography as a tool to isolate nerolidol from the Baccharis dracunculifolia volatile oil[J]. Journal of Essential Oil Research, 2014,26(5):334-337.
【13】WEI Y, DU J, LU Y. 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[J]. Journal of Separation Science, 2012,35(19):2608-2614.
【14】LI X C, ZHANG Q W, YIN Z Q, et al. Preparative separation of patchouli alcohol from patchouli oil using high performance centrifugal partition chromatography[J]. Journal of Essential Oil Research, 2011,23(6):19-24.
【15】CHEN Q Q, HU X F, LI J M, et al. Preparative isolation and purification of cuminaldehyde and p-menta-1,4-dien-7-al from the essential oil of Cuminum cyminum L. by high-speed counter-current chromatography[J]. Analytica Chimica Acta, 2011,689(1):149-154.
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【17】谢贵香,王兵,梁逸曾,等.高速逆流色谱法对当归中石油醚萃取部位化学成分的分离纯化[J].分析测试学报, 2010,29(10):1063-1067.
【18】曾志,谢润乾,张涛,等.川芎中内酯类化合物的质谱学规律[J].质谱学报, 2011,32(5):293-300.
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