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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 method for the determination of β-pinene in volatile oil from Forsythia suspensa by capillary gas chromatography and to compare the content of volatile oil and β-pinene in forsythia from different habitats. Methods: Volatile oil from Forsythia suspensa was extracted by steam distillation. The content of β-pinene in volatile oil was determined by capillary gas chromatography. Chromatographic conditions: using HP-5 (15 m × 0.53 mm × 1.5 μm) elastic silica capillary column; carrier gas N2; temperature programmed, the initial temperature 40 ℃, 1 ℃ .min-1 rate heating to 50 ℃, hold 1min , And the temperature was raised to 70 ℃ for 1 min at 5 ℃ .min-1. Finally, the temperature was raised to 205 ℃ for 3 min at 20 ℃ .min-1. The inlet temperature was 250 ℃. The detector temperature was 280 ℃. Results: Under the chromatographic conditions, β-pinene and other components were well separated. The linear range of β-pinene was 0.12 ~ 1.8 mg.mL-1 (r = 0.9995). The precision, stability and reproducibility The test’s RSD (n = 6) was 1.3%, 1.5%, 1.2%, respectively; the average recovery (n = 9) was 101.1%. Conclusion: The method is simple and accurate and can be used for the extraction of volatile oil and determination of β-pinene in Forsythia suspensa. The content of volatile oil and β-pinene in Forsythia suspensa from different habitats was mostly higher than that of the former, while that of Qiangxian County in Shanxi Province was higher than that of other origin samples.