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[摘要]
目的 采用气相色谱(GC)法建立养血清脑颗粒指纹图谱,并用GC-MS法对其中化学成分进行分析鉴定。方法 采用DB-5MS(30 m×0.25 mm,1 μm)石英毛细管色谱柱进行分离,氢火焰离子化检测器检测,进样口温度为250 ℃,分流比为50∶1;分离过程中采用程序升温方式:以10 ℃/min从150 ℃升至210 ℃,平衡5 min,再以3 ℃/min升温至240 ℃,平衡10 min;载气为高纯氮气,体积流量1 mL/min,进样量1 μL。结果 10批养血清脑颗粒得到的共有指纹图谱选定了10个共有峰,通过质谱鉴定出10个共有峰的化学成分,并考察了制剂与中间体和药材的相关性。结论 该方法准确、重现性好,可以作为养血清脑颗粒质量评估和控制的依据。
[Key word]
[Abstract]
Objective To establish GC fingerprint of Yangxue Qingnao Granula and identify the chemical components by GC-MS method. Methods The analysis was performed on a DB-5MS (30 m × 0.25 mm, 1 μm) capillary gas chromatography column and the split ratio was 50:1, while the temperatures of FID and inlet were set at 250 ℃; The programmed column temperature was set during the separation: 150 ℃ to 210 ℃ (10 ℃/min, 5 min) then 240 ℃ (3 ℃/min, 10 min); The high pure nitrogen was used as the carrier gas and the flow rate was set at 1 mL/min, and the injection volume was 1 μL. Results Ten common peaks were contained according to the common fingerprint of 10 batches of Yangxue Qingnao Granula and the 10 chemical components were identified by a GC-MS method. The comparison of the chromatograms showed good relativity among the medicinal material, intermediate, and preparation. Conclusion The analysis method is so precise and repeatable that the chromatogram could to be used as characteristic fingerprint for the quality evaluation and control of Yangxue Qingnao Granula.
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