HPLC-DAD-ELSD测定蒺藜中5个活性成分含量

HPLC-DAD-ELSD determination of five active components in Tribulus terrestris L.

目的:建立同时测定蒺藜中5个活性成分含量的方法。方法:采用HPLC-DAD-ELSD法,色谱柱为Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm),流动相为甲醇(A)-0.5%醋酸溶液(B),梯度洗脱,流速1.0 mL·min-1,柱温30℃,DAD检测波长为369 nm,ELSD漂移管温度100℃,载气流速2.5 L·min-1。结果:在此色谱条件下,各组分在55 min内均得到较好分离。槲皮素、山柰酚、异鼠李素、海柯皂苷元和替告皂苷元的浓度分别在0.829～20.73μg·mL-1,0.4051～10.13μg·mL-1,0.5176～12.94μg·mL-1,33.76～211.0μg·mL-1,17.12～107.0μg·mL-1范围内呈良好线性关系;其平均回收率分别为99.1%,98.5%,98.4%,98.8%,97.7%,RSD均小于2.0%。结论:所建立的分析方法简便、可靠,可用于蒺藜药材的质量控制。

Objective：To establish a quantitative method for the determination of five anti-tumor active components in Tribulus terrestris.Method：The determination was performanced on a Zorbax SB-C18 column（250 mm×4.6 mm,5 μm） with the mobile phase consisting of methanol（A） and 0.5% acetic acid solution（B） with gradient elution mode at a flow rate of 1.0 mL·min-1.Detection wavelength was 369 nm,the column temperature was 30 ℃,the drift tube temperature of ELSD was set at 100 ℃,and flow-rate was 2.5 L·min-1.Results：The calibration curves of quercetin,kaempferol,isorhamnetin,hecogenin and tigogenin were linear in the ranges of 0.829-20.73μg·mL-1,0.4051-10.13 μg·mL-1,0.5176-12.94 μg·mL-1,33.76-211.0 μg·mL-1,and 17.12-107.0 μg·mL-1,respectively.The average recoveries of quercetin,kaempferol,isorhamnetin,hecogenin and tigogenin were 99.1%,98.5%,98.4%,98.8%,97.7%,respectively.Conclusion：The method is simple and accurate,and is suitable for evaluating the quality of Tribulus terrestris.