正交试验优选当归挥发油的超临界CO_2流体萃取工艺

Optimization of Supercritical CO_2 Fluid Extraction Process of Volatile Oil from Angelicae Sinensis Radix by Orthogonal Test

目的:优选当归挥发油的超临界CO2流体萃取工艺,为当归挥发油的进一步研发提供参考。方法:建立UPLC同时测定当归挥发油中阿魏酸松柏酯和藁本内酯含量的方法,流动相乙腈-水(50∶50),检测波长320 nm,流速0.4 m L·min-1,柱温35℃,样品室温度4℃,进样量2μL;以阿魏酸松柏酯及藁本内酯的提取量为指标,采用正交试验考察萃取温度、萃取压力、萃取时间对当归挥发油萃取工艺的影响。结果:阿魏酸松柏酯和藁本内酯的线性范围依次为0.006 2~0.777 6,0.017 9~2.238μg,加样回收率在96.67%~102.08%。当归挥发油最佳萃取工艺为萃取温度40℃,萃取压力25 MPa,萃取时间2 h;阿魏酸松柏酯和藁本内酯的平均提取量分别为1.62,10.28 mg·g-1。结论:建立的UPLC含量测定方法重复性好、简便易行,可用于当归挥发油的质量控制;优化的萃取工艺稳定可行,适用于当归挥发油的提取。

Objective： To optimize supercritical CO2 fluid extraction process of volatile oil from Angelicae Sinensis Radix and provide reference for its further research and development. Method： UPLC was adopted to determine the contents of coniferyl ferulate and ligustilide in volatile oil from Angelicae Sinensis Radix with mobile phase of acetonitrile-water（ 50 ∶ 50）, detection wavelength at 320 nm and the flow rate of0. 4 m L·min^-1. With extracting amounts of coniferyl ferulate and ligustilide as indexes, extraction parameters including temperature, pressure and time were optimized by orthogonal test. Result： Coniferyl ferulate and ligustilide showed good linearity at 0. 006 2-0. 777 6 μg and 0. 017 9-2. 238 μg,respectively; their recoveries were between 96. 67%-102. 08%. Optimum extraction parameters were as follows： extraction temperature at40 ℃,extraction pressure of 25 MPa and extraction time of 2 h; average extracting amounts of coniferyl ferulate and ligustilide were 1. 62,10. 28 mg·g^-1,respectively. Conclusion： This UPLC is repeatable and simple,it can be used for quality control of volatile oil from Angelicae Sinensis Radix. Optimum extraction process is stable and feasible for extraction of volatile oil from Angelicae Sinensis Radix.