当归胶囊中三种有效成分含量测定的方法学验证

目的:建立当归胶囊中三种有效成分藁本内酯、阿魏酸、粗多糖的含量测定方法,并对检测方法进行方法学验证。方法:藁本内酯、阿魏酸采用高效液相色谱法,粗多糖采用紫外分光光度法,进行系统适应性、专属性、线性、检出限、准确度、精密度、重复性、稳定性等的方法学考察。结果:藁本内酯在20~60 μg/mL线性良好,r=0.9996,平均加样回收率为99.72%(RSD=2.99%),精密度、重复性、稳定性RSD均≤1%;阿魏酸在6~18 μg/mL线性良好,r=0.9990,平均加样回收率为96.11%(RSD=4.18%),精密度、重复性、稳定性RSD均≤2%;粗多糖在0.05~0.15 mg线性良好,r=0.9987,平均加样回收率为103.52%(RSD=4.79%),精密度、重复性、稳定性RSD均≤5%。结论:三种方法准确、可靠,可用于当归胶囊中三种有效成分藁本内酯、阿魏酸、粗多糖的含量测定。

Method Validation for the Determination of Three Kinds of Active Ingredients in Angelica Capsules

Objective:To establish methods for ligustilide,ferulic acid and polysaccharide content determination in angelica capsules and validate the methods,respectively. Methods:The HPLC analysis was performed for determination of ligustilide and ferulic acid,UV spectrophotometry was performed for determination of polysaccharide. Method validation included system adaptability,exclusivity,linearity,detection limit,accuracy,precision,repeatability and stability. Results:Good linearity of ligustilide was achieved in the range of 20~60 μg/mL(r=0.9996). The average recoveries was 99.72%(RSD=2.99%),RSD of precision,repeatability and stability were all less than 1%. Good linearity of ferulic acid was achieved in the range of 6~18 μg/mL(r=0.9990). The average recoveries was 96.11%(RSD=4.18%),RSD of precision,repeatability and stability were all less than 2%. Good linearity of polysaccharide was achieved in the range of 0.05~0.15 mg(r=0.9987). The average recoveries was 103.52%(RSD=4.79%),RSD of precision,repeatability and stability were all less than 5%. Conclusion:The three methods are accurate and reliable. It can be used to assay the content of ligustilide,ferulic acid and polysaccharide in angelica capsules,respectively.