HPLC-CAD法同时测定注射用芪红脉通中的7个黄芪皂苷类成分

目的: 建立高效液相色谱-电喷雾检测(HPLC-CAD)法同时测定注射用芪红脉通中7个黄芪皂苷(黄芪甲苷、黄芪皂苷Ⅱ、异黄芪皂苷Ⅱ、cyclocephaloside Ⅱ、黄芪皂苷Ⅰ、异黄芪皂苷Ⅰ、cycloastragenol-3-O-β-D-(3",4"-di-O-acetyl)-xylopyranosyl-6-O-β-D-glucopyranoside)的含量. 方法: 采用Kromasil C₁₈(250 mm×4.6 mm,5 μm)色谱柱,以水(A)-乙 腈(B)为流动相,梯度洗脱,流速1.0 mL·min^-1,柱温30 ℃,以电喷雾检测器检测(检测温度:30 ℃). 结果: 7个成分均达到基线分离,线性关系良好,7个成分的加样回收率为97.8%~101.1%,RSD(n=6)均小于3.0%.5批样品中黄芪甲苷、黄芪皂苷Ⅱ、异黄芪皂苷Ⅱ、cyclocephaloside Ⅱ、黄芪皂苷Ⅰ、异黄芪皂苷Ⅰ、cycloastragenol-3-O-β-D-(3",4"-di-O-acetyl)-xylopyranosyl-6-O-β-D-glucopyranoside 7个成分的含量依次为3.30~4.43、2.64~3.44、1.45~1.98、1.16~1.53、0.95~1.54、1.43~2.01、0.49~0.66 mg·支^-1. 结论: 本方法准确,灵敏,简便快速,重复性好,可以实现注射用芪红脉通的多指标质量控制.

Objective: To establish a quantitative method for simultaneous determination of seven astragalosides(astragaloside Ⅳ,astragaloside Ⅱ,isoastragaloside Ⅱ,cyclocephaloside Ⅱ,astragaloside Ⅰ,isoastragaloside Ⅰ,cycloastragenol-3-O-β-D-(3",4"-di-O-acetyl)-xylopyranosyl-6-O-β-D-glucopyranoside)in Qihong Maitong injection by high performance liquid chromatography with charged aerosol detector(HPLC-CAD). Methods: The chromatographic separation was performed on a Kromasil C₁₈ column(250 mm×4.6 mm,5 μm)by using water and acetonitrile as the mobile phase with the gradient elution at a flow rate of 1.0 mL·min^-1,the column temperature was 30 ℃,and the charged aerosol detector(CAD)was selected as the detector(the testing temperature was 30 ℃). Results: The good resolution can be achieved among seven astragalosides and the method was linear over the investigated concentration range.The average recovery was between 97.8% and 101.1% with all relative standard deviations no more than 3.0%.The contents of astragaloside Ⅳ, astragaloside Ⅱ,isoastragaloside Ⅱ, cyclocephaloside Ⅱ,astragaloside Ⅰ,isoastragaloside Ⅰ,cycloastragenol-3-O-β-D-(3",4"-di-O-acetyl)-xylopyranosyl-6-O-β-D-glucopyranoside in 5 batches of Qihong Maitong injection were 3.30-4.43 mg per ampoule,2.64-3.44 mg per ampoule,1.45-1.98 mg per ampoule,1.16-1.53 mg per ampoule,0.95-1.54 mg per ampoule,1.43-2.01 mg per ampoule,0.49-0.66 mg per ampoule. Conclusion: The developed method is accurate,sensitive,simple and reproducible,which could be applied to quality control of multiple components in Qihong Maitong injection.