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目的:建立超高效液相色谱(UPLC)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:超高效液相色谱法,Waters BEH C18(2.1 mm×100 mm,1.7μm)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297 nm;流速0.3 mL·min~(-1);进样量2μL,柱温25℃。结果:伞形花内酯、狼毒色原酮的线性范围分别为0.74~19.64μg·mL~(-1)(r=0.999 9)、14.70~352.8μg·mL~(-1)(r=0.999 8),平均回收率分别为99.20%,99.63%,RSD分别为1.81%,1.65%。13批瑞香狼毒药材中伞形花内酯的含量范围为0~0.602 mg·g~(-1),狼毒色原酮的含量范围6.08~33.37 mg·g~(-1)。结论:该方法操作简便、快速、重复性好、结果准确可靠,可用于中药瑞香狼毒的质量控制。
OBJECTIVE: To establish a method for the determination of ursosteon and lancinone in Stellera chamaejasme by UPLC. METHODS: The mobile phase consisted of acetonitrile (A) - 0.1% phosphoric acid solution (B) with gradient elution on a Waters BEH C18 column (2.1 mm × 100 mm, 1.7 μm) The lactone was 327 nm, the concentration of eplerenone was 297 nm, the flow rate was 0.3 mL · min -1. The injection volume was 2 μL and the column temperature was 25 ℃. Results: The linear ranges of ursovalein and eplerenone were 0.74 ~ 19.64μg · mL -1 (r = 0.999 9), 14.70 ~ 352.8μg · mL -1 (r = 0.999 8). The average recoveries were 99.20% and 99.63%, respectively. The RSDs were 1.81% and 1.65% respectively. The content of ursolate in 13 batches of Stellera chamaejasmelon was 0 ~ 0.602 mg · g ~ (-1), and the content of Stellera chamaejasme was 6.08 ~ 33.37 mg · g ~ (-1). Conclusion: The method is simple, rapid, reproducible and accurate. It can be used for the quality control of Stellera chamaejasme.