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目的:应用气相色谱-质谱(GC-MS)联用法对淫羊藿挥发油进行指纹图谱研究。方法:采用水蒸气蒸馏法提取巫山淫羊藿和粗毛淫羊藿中的挥发油,利用GC-MS对其化学成分进行分析,通过GC-FID建立了淫羊藿挥发油指纹图谱的分析方法。气相色谱条件为HP-INNOWAX色谱柱,进样口温度260℃,分流比5∶1;程序升温(初始温度60℃,保持10 min,以2℃·min-1升至250℃,保持13 min)。GC-MS参数为柱流速1.0 m L·min-1,MS电子能量70 e V,离子源温度230℃,四级杆温度180℃,传输线温度280℃,全离子扫描,扫描质量范围m/z 40~550,溶剂延迟3 min。GC-FID参数:柱流速1.5 m L·min-1,FID检测器温度260℃,氢气流量30 m L·min-1,空气流量300 m L·min-1,尾吹氮气30 m L·min-1。结果:获得了20份不同产地淫羊藿的指纹图谱峰。结论:该方法的精密度、稳定性和重复性均良好。为淫羊藿药材的质量控制提供了有效手段。
Objective: To study the fingerprint of volatile oil from Epimedium by gas chromatography-mass spectrometry (GC-MS). Methods: Volatile oil was extracted from the leaves of Epimedium wadima and Epimedium wadgeshanensis by steam distillation. The chemical constituents were analyzed by GC-MS. The fingerprint of volatile oil from Epimedium sagittatum was established by GC-FID. Gas chromatographic conditions were HP-INNOWAX column with inlet temperature of 260 ℃ and split ratio of 5:1. The temperature was programmed (the initial temperature was 60 ℃ and kept for 10 min, and the temperature was raised to 250 ℃ at 2 ℃ · min-1 for 13 min ). The GC-MS parameters were column flow rate 1.0 m L · min-1, MS electron energy 70 e V, ion source temperature 230 ℃, quadrupole temperature 180 ℃, transmission line temperature 280 ℃, total ion scan, mass scan range m / z 40 ~ 550, solvent delay 3 min. GC-FID parameters: column flow rate 1.5 m L · min-1, FID detector temperature 260 ℃, hydrogen flow rate 30 m L · min-1, air flow rate 300 m L · min- -1. Results: Fingerprints of Epimedium from 20 different areas were obtained. Conclusion: The method has good precision, stability and repeatability. For the quality control of Epimedium herbs provides an effective means.