HPLC-CAD法测定芪蛭通络胶囊中苷类成分的含量

目的 建立高效液相色谱-电喷雾检测器方法(HPLC-CAD)同时测定芪蛭通络胶囊中人参皂苷Rb₁和黄芪甲苷的含量。方法 采用色谱柱为Waters XSclectHss T3-C₁₈(4. 6 mm×250 mm,5 μm),水(A)-乙腈(B)为流动相,梯度洗脱(0 min,15% B;0～10 min,15%~25%B;10～15 min,25%B~31%B;20～50 min,31%B),流速1 mL·min^{- 1},柱温25 ℃,进样量为20 μL。电喷雾检测器(CAD)雾化器温度为35 ℃,功能参数(power function,PF)为1.0。结果 芪蛭通络胶囊中人参皂苷Rb₁和黄芪甲苷均具有良好的线性关系(r＞0.999 0),定量限(LOQ)分别为0.013和0.015 μg,精密度、重复性、24 h稳定性实验的相对标准偏差(RSD)值均小于3.0%,平均加样回收率分别为91.74%和100.09%。结论 本研究建立的HPLC-CAD法可同时对芪蛭通络胶囊中人参皂苷Rb₁和黄芪甲苷进行含量测定,为芪蛭通络胶囊的检测分析和质量控制提供了新的方法。

Determination of Saponins in Qizhitongluo Capsules by HPLC-CAD

OBJECTIVE To develop a HPLC-CAD method for simultaneous determination of ginsenoside Rb₁ and astragaloside Ⅳ in Qizhitongluo Capsules. METHODS HPLC analysis was performed on a WatersXSclectHss T3-C₁₈ column (4.6 mm×150 mm, 5 μm), with mobile phase consisting of water solution (A) -acetonitrile (B) at a flow rate of 1.0 mL· min^-1 (0 min, 15% B; 0-10 min, 15%-25%B; 10-15 min, 25%-31%B; 20-50 min,31%B),and column temperature was 25 ℃.The injection volume was 20 μL. The nebulizer chamber temperature for the CAD system was maintained at 35 ℃ and the power function (PF) was 1.0. RESULTS The HPLC-CAD approach developed showed good linearity for ginsenoside Rb₁ and astragaloside Ⅳ, and the correlation coefficients for calibration curves were both more than 0.9990. The limits of quantitation (LOQ) were found to be 0.013 and 0.015 μg, respectively. The RSDs of precision, repeatability, stability in 24 h were all less than 3.0%. The average recovery rates of ginsenoside Rb₁ and astragaloside Ⅳ were 91.74% and 100.09%, respectively. CONCLUSION The established HPLC-CAD method can simultaneously determine ginsenoside Rb₁ and astragaloside Ⅳ in Qizhitongluo capsules, which provides a new approach for the analysis and quality control of Qizhitongluo capsules.