HPLC法测定益肝康胶囊中华蟾酥毒基与脂蟾毒配基的含量

Determination of Cinobufagin and Resibufogenin in Yigankang Capsule by HPLC

目的:建立以高效液相色谱法测定益肝康胶囊中华蟾酥毒基与脂蟾毒配基含量的方法。方法:色谱柱为SpherigelODSC18(150mm×4.6mm,5μm),流动相为0.5%磷酸二氢钾-乙腈(50∶50,用磷酸调pH3.2),流速为1.0mL·min-1,检测波长为296nm,柱温为40℃。结果:华蟾酥毒基、脂蟾毒配基的进样量分别在0.22～1.09μg(r=0.9998)、0.26～1.30μg(r=0.9999)范围内与各自峰面积积分值呈良好的线性关系;二者平均回收率分别为99.4%(RSD=1.9%,n=9)和98.7%(RSD=1.4%,n=9)。结论:本法灵敏度高、操作简便、结果准确、专属性强,可用于益肝康胶囊的质量控制。

OBJECTIVE： To establish an HPLC method for the determination of the contents of cinobufagin and resibu-fogenin in Yigankang capsule. METHODS： The samples were separated on Spherigel ODS C18（150 mm x 4.6 ram, 5 μm） chromatographic column with 0.5% KH2PO4-acetonitrile （50 ： 50, pH was adjusted to 3.2 by phosphoric acid） used as a mobile phase at a flow rate of 1.0 mL·min^-1. The detection wavelength was set at 296 nm and the column temperature was kept at 40℃.RESULTS： The linear ranges of cinobufagin and resibufogenin were 0.22--1.09μg （r = 0.999 8） and 0.26-1.30μg （r = 0. 999 9）, respectively, and the average recoveries of cinobufagin and resibufogenin were 99.4% （RSD = 1.9%, n = 9） and 98.7% （RSD = 1.4%, n = 9）, respectively. CONCLUSION： This method is proved to be sensitive, simple, accurate and specific, and it is applicable for the quality control of Yigankang capsule.