用微波萃取-HPLC法测定不同产地辛夷药材中木兰脂素的含量

Determination of the content of magnolin in Flos Magnoliae by microwave-assisted extraction and HPLC method

目的：采用微波萃取-HPLC法测定木兰脂素的含量,并考察4个不同产地辛夷药材中木兰脂素的含量差异。方法：采用微波萃取法,以75%乙醇为溶剂,在76℃恒温800 s萃取辛夷药材中的木兰脂素。Shim-Pack VP-ODS柱（150 mm×4.6 mm,5μm）,流动相：乙腈-水（40∶60）,流速：0.8 ml/min;柱温：室温,检测波长：238 nm,采用HPLC法测定木兰脂素的含量。结果：以峰面积（A）对浓度（c）作线性回归,回归方程为A=2.922 7×104c-3 617.4（r=0.999 9）,在5.6~240.8μg/ml浓度范围内,木兰脂素的峰面积与浓度呈良好线性关系。该法的精密度、重现性和稳定性良好,低、中、高浓度（104.87、127.42和172.51μg/ml）的加样回收率分别为（100.39±1.58）%（、103.82±4.04）%和（103.74±0.13）%（n=3）。采用该法测得河南、河北、湖南、湖北4地所产的辛夷药材中木兰脂素含量分别为（6.59±0.39）%（、3.44±0.48）%、（2.73±0.28）%和（4.18±0.25）%（n=3）。其中河南产辛夷药材中木兰脂素含量最高。结论：本方法简便、准确、稳定、重复性好,可作为辛夷药材及相关制剂质量控制的定量方法。

Objective： To establish a microwave-assisted extraction and HPLC method for determinination of the content of magnolin in Flos Magnoliae from four different origins.Methods： The magnolin in Flos Magnoliae herbs was extracted by 75% ethanol in microwave for 800 s at the temperature of 76 ℃.HPLC was performed on a Shim-Pack VP-ODS column（150 mm×4.6 mm,5 μm） with mixture of acetonitrile and water（40∶60） as mobile phase.The flow rate was 0.8 ml/min.The column temperature was room temperature.The detection wavelength was 238 nm.Results：The regression equation was A=2.922 7×104 c-3 617.4（r=0.999 9）,where A was the peak areas and c was the concentration of magnolin.The concentrations of magnolin in the range of 5.6-240.8 μg/ml were in good linearity with chromatographic peak areas.The precision,reproducibility and stability were all good.The average recovery rates of low,middle and high concentrations（104.87,127.42,172.51 μg/ml） of magnolin were（100.39±1.58）%,（103.82±4.04）% and（103.74±0.13）%（n=3）,respectively.This method was used to determine the contents of magnolin in Flos Magnoliae from four different origions： He＇nan,Hebei,Hunan and Hubei provinces and the contents were（6.59±0.39）%,（3.44±0.48）%,（2.73±0.28）% and（4.18±0.25）%（n=3）,respectively.Flos Magnoliae herbs from He＇nan province was found to have the highest content of magnolin.Conclusion： The method is simple,accurate,stable and can be used as a quantitative method for quality control of Flos Magnoliae herbs and its preparations.