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芪板青颗粒质量控制研究
林仙军,王彬,陈晓林,蔡文金
0
(浙江省兽药饲料监察所)
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。
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
DOI:
投稿时间:2019-02-19修订日期:2019-04-29
基金项目:
Study on Quality Control of Qibanqing Granules
()
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.
Key words:  Qibanqing granules  chlorogenic acid  caffeic acid  astragaloside  high performance liquid chromatography  diode array detector  evaporative light scattering detector

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