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目的建立RP-HPLC法测定瑞香狼毒药材中伞形花内酯和狼毒色原酮的含量。方法采用反相高效液相色谱法,PDA检测器,选用Hypersil GOLDaQ-C_(18)(250mm×4.6mm,5μm),色谱柱;流动相为乙腈(A)-0.1%磷酸水溶液(B),进行梯度洗脱;检测波长伞形花内酯为327 nm,狼毒色原酮为297nm;流速1.0ml/min;进样量10μl,柱温25℃。结果2种活性成分在13 min内实现良好分离,伞形花内酯、狼毒色原酮的线性范围分别为1.22~19.6μg·ml~(-1)(r=0.9998)、20.0~320μg·ml~(-1)(r=0.9997),平均回收率分别为100.5%,101.8%,RSD分别为1.2%,1.5%。13批不同产地瑞香狼毒药材中伞形花内酯的含量范围为:0~0.57mg/g;狼毒色原酮的含量范围6.46~30.92mg/g。结论该方法操作简便、重现性好、结果准确可靠,可用于中药瑞香狼毒的质量控制。
OBJECTIVE To establish a RP-HPLC method for the determination of Ursolvin and Stellate ketone in Stellera chamaejasme L. herbs. Methods A reversed phase high performance liquid chromatography (HPLC) and PDA detector were used. The column was Hypersil GOLDaQ-C 18 (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-A 0.1% phosphoric acid solution B, Gradient elution; detection wavelength umbelliferone was 327 nm, eradication of ketone was 297nm; flow rate 1.0ml / min; injection volume 10μl, column temperature 25 ℃. Results The two active components were well separated within 13 min. The linear ranges of ursovalein and promaninone were 1.22-19.6μg · ml -1 (r = 0.9998) and 20.0-320μg · ml ~ (-1) (r = 0.9997). The average recoveries were 100.5% and 101.8%, respectively. The RSDs were 1.2% and 1.5% respectively. The contents of ursolate in 13 batches of Stellera chamaejasme herbs were ranged from 0 to 0.57 mg / g, and the content of Stellera chamaejasme was 6.46 to 30.92 mg / g. Conclusion The method is simple, reproducible, accurate and reliable, and can be used for the quality control of Stellera chamaejasmel L.