不同产地连翘中挥发油及其β-蒎烯含量的比较研究

Comparative study on the contents of volatile oil and β-pinene of Fructus Forsythiae in different origins

目的:建立连翘挥发油中β-蒎烯的毛细管气相色谱含量测定方法,并比较不同产地连翘中挥发油及β-蒎烯的含量。方法:用水蒸气蒸馏法提取连翘中的挥发油,毛细管气相色谱法测定挥发油中β-蒎烯的含量。色谱条件:采用HP-5(15 m×0.53 mm×1.5μm)弹性石英毛细管色谱柱;载气N2;程序升温,初始温度40℃,以1℃.min-1速率升温至50℃,保持1min,以5℃.min-1升温至70℃,保持1 min,最后以20℃.min-1升温至205℃,保持3 min;进样口温度250℃;检测器(FID)温度280℃。结果:在本文色谱条件下,β-蒎烯与其他组分能得到良好分离;β-蒎烯线性范围为0.12～1.8 mg.mL-1(r=0.9995);精密度、稳定性和重复性试验的RSD(n=6)分别为1.3%,1.5%,1.2%;平均回收率(n=9)为101.1%。结论:本方法简便、准确,可用于连翘中挥发油的提取和β-蒎烯的含量测定。不同产地连翘中挥发油及β-蒎烯的含量,青翘大多高于老翘,山西绛县的青翘又高于其他产地样品。

Objective： To establish a capillary gas chromatography（CGC） method for the determination of β-pinene of volatile oil in Fructus Forsythiae,and to compare the contents of volatile oil and β-pinene of Fructus Forsythiae in different origins.Methods：Vapour-distilation was employed in extracting volatile oil of Fructus Forsythiae.The contents of β-pinene of volatile oil in Fructus Forsythiae were determined by CGC.The CGC system consisted of an HP-5 capillary column（15 m×0.53 mm×1.5 μm）,nitrogen as the carrier gas.Temperature program was the initial temperature was 40 ℃,increased temperature at a rate of 1 ℃·min-1 to 50 ℃ and retained for 1 min,again increased at a rate of 5 ℃·min-1 to 70 ℃ and retained for 1 min,finally at a rate of 20 ℃·min-1 to 205 ℃ and retained for 3 min.The inject temperature was 250 ℃,FID as the detector at 280 ℃.Results：β-pinene in Fructus Forsythiae was separated from other constituents under the chromatographic condition;The linear range of β-pinene was 0.12-1.8 mg·mL-1（r=0.9995）;The RSDs（n=6） of precision,stabilization and reproducibility were 1.3%,1.5% and 1.2%,respectively.Average recoveries（n=9） of the method were 101.1%.Conclusion：This method is simple,accurate and suitable for the extraction of volatile oil and the determination of β-pinene in Fructus Forsythiae.The contents of volatile oil and β-pinene in Qingqiao are almost higher than those in Laoqiao.Qingqiao in Jiangxian Shanxi have higher contents than samples collected in other origins.