芪板青颗粒质量控制研究

Study on Quality Control of Qibanqing Granules

为建立芪板青颗粒中绿原酸、咖啡酸和黄芪甲苷含量测定的方法。测定绿原酸和咖啡酸采用Agilent Eclipse XDB-C18 250 mm×4.6 mm 5μm色谱柱,流动相为0.05%磷酸溶液-乙腈(92∶8,V∶V),进样量10μL,柱温30℃,流速为1.0 m L/min,在190 nm～400 nm范围进行扫描,记录327 nm色谱图;测定黄芪甲苷采用Waters symmetry C18 5μm 4.6 mm×250 mm色谱柱,进样量10μL,漂移管温度35℃,雾化器温度35℃,气流速度1.2 L/min,流动相为水-乙腈(65∶35,V∶V),柱温30℃,流速1.0 m L/min。绿原酸在3.611～72.23μg/m L范围内线性关系良好,r为0.99999,平均加样回收率97.1%;咖啡酸在3.060～61.20μg/m L范围内线性关系良好,r为0.99999,平均加样回收率96.2%;黄芪甲苷在1.0～10μg范围线性关系良好,r为0.9997,平均加样回收率为98.0%。该方法定性、定量准确,适用于芪板青颗粒含量测定。

To establish a method for the determination of chlorogenic acid, caffeic acid and astragaloside in Qibanqing granules.Agilent Eclipse XDB-C18 250 mm×4.6 mm 5 μm column was used for the determination of chlorogenic acid and caffeic acid.The mobile phase was 0.05% phosphoric acid solution-acetonitrile (92∶8, V∶V ), the injection volume was 10 μL, the column temperature was 30 ℃, and the flow rate was 1.0 mL/min.The chromatograms were scanned in the range of 190 nm to 400 nm and recorded at 327 nm.Waters symmetry C18 4.6 mm×250 mm 5 μm column was used for the determination of astragaloside.The mobile phase was water-acetonitrile (65∶35, V∶V).The column temperature was 30 ℃ and the flow rate was 1.0 mL/min, the injection volume was 10 μL.The drift tube temperature of ELSD was 35 ℃,the atomizer temperature was 35 ℃ and the gas flow rate was 1.2 L/min.The result indicated that chlorogenic acid was in linear over the range of 3.611 to 72.23 μg/mL, r was 0.99999, the average recovery was 97.1%;caffeic acid was in linear over the range of 3.060 μg/mL to 61.20 μg/mL, r was 0.99999, the average recovery was 96.2%;astragaloside was in linear over the range of 1.0 to 10 μg, r was 0.9997, the average recovery was 98.0%.The method was accurate in qualitative and quantitative analysis, and suitable for the determination of Qibanqing granules.