高效液相色谱-二极管阵列-电化学联用技术测定八角莲中3种成分的含量

HPLC-DAD-ECD determination of 3 components in Dysosma pleiantha(Hance)Woods

目的:建立高效液相色谱-二极管阵列-电化学联用技术同时测定八角莲中鬼臼毒素、山萘酚和槲皮素3种成分含量的新方法。方法:采用 Zorbax SB-C_(18)(150 mm×4.6 mm,5.0 μm)色谱柱;以甲醇(A)-0.2%醋酸(B)为流动相,采用梯度洗脱:0 min 时 A-B(50:50),12 min 时 A-B(70:30);流速为0.8 mL·min^(-1);柱温为25℃;二极管阵列检测波长为290 nm;单安培检测器的工作电位为+0.4 V。结果:鬼臼毒素、山萘酚及槲皮素的线性范围分别为46.9～469μg·mL^(-1)(r=0.9992),17.2～172μg·mL^(-1)(r=0.9991),8.44～84.4μg·mL^(-1)(r=0.9994);回收率分别为98.04%～98.51%(RSD<1.0%),96.30%～97.28%(RSD<1.5%),95.81%～97.72%(RSD<2.2%)。结论:本法简便,重复性好,适用于八角莲中鬼臼毒素、山萘酚和槲皮素3种成分的同时测定。

Objective： To establish an HPLC - DAD - ECD new method for determination of the contents of podophyllotoxin, kaempferol and quercetin in Dysosma pleiantha（Hance） Woods. Method：The samples were separated on Zorbax SB- C18 column（150 mm 4. 6 mm,5.0μm） by gradient elution with methanol -0. 2% acetic acid （0 min, 50：50; 12 min, 70： 30） as the mobile phase at a flow rate of 0. 8 mL·min^-1. The DAD detection was used at 290 nm and 25℃, and the ECD detection potential was set at ＋ 0. 4 V. Results： The linear ranges of podophyllotoxin, kaempferol and quercetin were 46. 9 - 469μg·mL^-1 （ r = 0. 9992） , 17.2 - 172μg·mL^-1 （ r = 0. 9991 ）, 8.44 - 84. 4μg·mL^-1 （ r = 0. 9994） respectively. The average recoveries were 98.04% - 98.51% （ RSD 〈 1.0% ）, 96. 30% -97.28% （ RSD 〈 1.5% ）, 95.81% -97.72% （ RSD 〈2.2% ） respectively. Conclusion ： The method is simple with good reproducibility, suitable for the determination of the contents of podophyllotoxin, kaempferol and quercetin in Dysosma pleiantha（Hance） Woods.