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目的:建立当归补血片中黄芪甲苷的含量测定方法。方法:以吡啶-苯甲酰氯(2.5∶1)为衍生化试剂,对黄芪甲苷进行苯甲酰化,采用HPLC测定样品中黄芪甲苷含量。色谱柱:Phenomenex Gemini C18柱(50mm×4.6mm,5μm);流动相:乙腈-0.1%三乙胺溶液(98∶2)洗脱30min;流速1.0mL·min-1;检测波长230nm;柱温20℃;进样量10μL。结果:黄芪甲苷进样量在0.074～0.925μg范围内线性关系良好(r=0.9999),重复性好(RSD=0.17%),平均回收率(n=3)为98.6%～99.9%(RSD=0.32%～0.95%)。结论:该法样品前处理简单,专属性强、准确度高、灵敏度高、重现性好。
Objective: To establish a method for determination of Astragaloside Ⅳ in Danggui Buxue Tablet. Methods: Benzopyriflavone was synthesized by pyridine-benzoyl chloride (2.5:1) as the derivatization reagent. The content of astragaloside IV in the sample was determined by HPLC. Column: Phenomenex Gemini C18 column (50mm × 4.6mm, 5μm); mobile phase: acetonitrile-0.1% triethylamine solution (98: 2) for 30min; flow rate 1.0mL · min -1; 20 ℃; injection volume 10μL. Results: The good linearity (r = 0.9999), good repeatability (RSD = 0.17%) and average recoveries (n = 3) were 98.6% ~ 99.9% = 0.32% ~ 0.95%). Conclusion: The sample pretreatment is simple, specific, high accuracy, high sensitivity, good reproducibility.