高效液相色谱-蒸发光散射法测定气血双补口服液中黄芪甲苷的含量

Evaporative light-scattering detector high-performance liquid chromatography for determination of astragaloside Ⅳ in Qixueshuangbu Oral Liquid

目的气血双补口服液现行质量标准仅采用薄层色谱法对黄芪进行定性鉴别,而无相应的定量检测项目。文中建立适用于气血双补口服液中黄芪甲苷的高效液相色谱测定方法,为有效控制该产品质量,制订该制剂新的质量标准提供参考依据。方法采用高效液相色谱-蒸发光散射法(High-performance liquid chromatography evaporative light-scattering detec-tor,ELSD-HPLC),色谱柱:汉邦ODS-C18柱(250 mm×4.6 mm,5μm);流动相:甲醇-水(79∶21);体积流量:0.8 ml/min;柱温:室温;漂移管温度:70℃,载气流速:2.24 L/min。结果黄芪甲苷在2.51～12.55μg范围内线性关系良好,黄芪甲苷平均回收率为99.01%,相对标准偏差(relative standard deviation,RSD)为1.34%。结论该方法简便易行,方法学验证符合要求,可用于气血双补口服液的质量控制。

Objective For the quality evaluation of Qixueshuangbu Oral Liquid, only thin-layer chromatography （TLC） is used to identify Radix Astragali Mongolici without any assay of its constituents. This study aimed to establish a method of assaying As- tragaloside by high-performance liquid chromatography （ HPLC ） to provide some evidence for the quality control and quality criteria for- mulation of Qixueshuangbu Oral Liquid. Methods We used an evaporative light-scattering detector HPLC （ELSD-HPLC） to evalu- ate the quality of Qixueshuangbu Oral Liquid, with the Hanbang ODS-C18 column at 250 mm×4.6mm,5μm, the mobile phase of methanol-water at 79：21, the flow rate at 0.8 ml/min, the column temperature at 25 ℃, the tube temperature of the detector at 70℃, and the flow rate of air at 2.24 L/min. Results The calibration curve was linear within the range of 2.51 - 12.55 μg of Astragalo- side IV, with an average recovery of 99.01% （ RSD = 1.34% ）. Conclusion The method is simple, accurate and repeatable, which can be used for the quality control of Qixueshuangbu Oral Liquid.