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目的建立HPLC同时测定瑞香狼毒中瑞香素、伞形花内酯和东莨菪内酯含量的方法。方法样品经无水乙醇回流。采用Synergi 4u Polar-RP 80R柱(4.6 mm×250 mm,5μm),流动相为甲醇-1%冰醋酸溶液,等度洗脱,流速:1.0 m L·min-1,检测波长:324 nm,柱温:30℃。结果瑞香素在0.012~0.250μg(r=0.999 9)、伞形花内酯在0.149~2.981μg(r=0.999 9)、东莨菪内酯在0.012~0.239μg(r=0.999 9)均呈良好的线性关系;瑞香素、伞形花内酯和东莨菪内酯的加样回收率分别为99.0%(RSD=0.94%),98.7%(RSD=0.77%)和98.3%(RSD=1.16%)。结论 3种香豆素成分在35 min内达到基线分离,该方法分析时间短、稳定性和回收率良好,对瑞香狼毒药材的质量控制具有一定的参考价值。
Objective To establish a method for simultaneous determination of daphnetin, umbelliferone and scopoletin in Stellera chamaejasme by HPLC. Methods Samples were refluxed with absolute ethanol. A Synergi 4u Polar-RP 80R column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase consisted of methanol-1% glacial acetic acid and wasocratically eluted at a flow rate of 1.0 mL · min-1. The detection wavelength was 324 nm, Column temperature: 30 ℃. Results Daphnetin was found to be good at 0.012-0.250 μg (r = 0.999 9), ursolide at 0.149-2.981 μg (r = 0.999 9) and scopoletin at 0.012-0.239 μg (r = 0.999 9) (RSD = 0.94%), 98.7% (RSD = 0.77%) and 98.3% (RSD = 1.16%) of the daphnetin, umbelliferone and scopoletin respectively. . Conclusion The results showed that the three coumarins achieved baseline separation within 35 min. The analysis time was short, and the stability and recovery rate were good. The results showed that the three coumarins could be used as reference for the quality control of Stellera chamaejasme material.