芪板青颗粒质量控制研究

Study on Quality Control of Qibanqing Granules

关键词:  芪板青颗粒  绿原酸  咖啡酸  黄芪甲苷  高效液相色谱法  二极管阵列检测器  高蒸发光散射检测器

Key words:  Qibanqing granules  chlorogenic acid  caffeic acid  astragaloside  high performance liquid chromatography  diode array detector  evaporative light scattering detector

摘要:

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 5 μm色谱柱，流动相为0.05%磷酸溶液-乙腈（92∶8，V∶V），进样量10 μL，柱温30 ℃，流速为1.0 mL/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 5 μm 4.6 mm×250 mm色谱柱，进样量10 μL，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 mL/min。绿原酸在3.611～72.23 μg/mL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3.060～61.20 μg/mL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1.0~10 μg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。

Abstract:

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.