Chen Fengli, Jia Jia, Zhang Qiang, Gu Huiyan, Yang Lei
Key Laboratory of Forest Plant Ecology, Ministry of Education, Northeast Forestry University, Harbin 150040, China.
Pharmacy & Medical Laboratory Department, Daqing Medical College, Daqing 163312, China.
J Chromatogr A. 2017 Nov 17;1524:254-265. doi: 10.1016/j.chroma.2017.10.008. Epub 2017 Oct 7.
In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs.
在本研究中，开发了一种改进技术，即采用微波辅助水蒸馏串联液液萃取（MHD-LLE）从紫穗槐果实中分离精油。新装置由两个串联的用于分离精油的分离柱组成，一个是传统的油水分离柱，另一个是使用有机溶剂从水溶胶中萃取成分的萃取柱。因此，该装置可以同时收集在水溶胶顶部分离出的精油和使用有机溶剂从水溶胶中萃取的成分。基于第一和第二分离柱中精油的产率，通过单因素实验和Box-Behnken设计研究了参数的影响。在最佳条件下（第二分离柱中使用2mL乙醚作为萃取溶剂，液固比为12mL/g，匀浆时间为4.0min，微波辐照时间为35min，微波辐照功率为540W），第一分离柱中精油的产率令人满意（10.31±0.33g/kg），第二分离柱中精油的产率也令人满意（0.82±0.03g/kg）。与传统方法相比，所开发的方法在更短的时间内获得了更高的精油产率。此外，精油的GC-MS分析表明，在两个分离柱中获得的精油中各挥发性成分的相对含量存在显著差异。因此，这里开发的MHD-LLE技术是从紫穗槐果实以及其他草药中分离精油的良好替代方法。
