RP-HPLC法测定狼毒中狼毒乙素和岩大戟内酯B的含量

RP-HPLC determination of 2,4-dihydroxy-6-methoxy-3-methylacetophenone and jolkinolide B in Euphorbiae Ebracteolatae Radix

目的：建立同时测定狼毒药材中狼毒乙素和岩大戟内酯B的HPLC定量分析方法。方法：采用Lichrospher C18（4.6 mm×250 mm,5μm）色谱柱,以乙腈（A）-水（B）为流动相梯度洗脱（0-5 min,40%A;5-10 min,40%A→50%A;10-30 min,50%A→55%A;30-40 min,55%A→60%A;40-45 min,60%A→70%A）,流速1.0 mL·min^-1;检测波长226 nm,柱温30℃。结果：狼毒乙素线性范围为0.005-0.863μg（r=0.9999）,平均回收率为96.4%（RSD=1.4%,n=6）;岩大戟内酯B线性范围为0.003-0.496μg（r=0.9999）,平均回收率为96.0%（RSD=2.1%,n=6）。结论：本方法专属性强,结果准确,简便可行,可用于狼毒药材的质量控制。

Objective：To develop an HPLC method for the determination of 2,4-dihydroxy-6-methoxy-3-methylacetophenone and jolkinolide B in Euphorbiae Ebracteolatae Radix.Methods：A Lichrospher C18（4.6 mm ×250 mm,5 μm） column was adopted.The mobile phase consisted of acetonitrile and water with gradient elution（0-5 min,40%A;5-10 min,40%A→50%A;10-30 min,50%A→55%A;30-40 min,55%A→60%A;40-45 min,60%A→70%A）,at the flow rate of 1.0 mL·min^-1.The detection wavelength was set at 226 nm and column temperature was 30 ℃.Results：The linear range of 2,4-dihydroxy-6-methoxy-3-methylacetophenone was 0.005-0.863 μg（r=0.9999）,the mean recovery was 96.4%（RSD=1.4%,n=6）;the linear range of jolkinolide B was 0.003-0.496 μg（r=0.9999）,the mean recovery was 96.0%（RSD=2.1%,n=6）.Conclusion：The method is specific,accurate and convenient,and can be used for the quality contro1 of Euphorbiae Ebracteolatae Radix.