高效液相色谱法测定藿苏养胃口服液中黄芪甲苷的含量

Determination of Astragaloside IV in Huosuyangwei Oral Liquid

目的：建立藿苏养胃口服液中黄芪甲苷前处理及含量的HPLC测定方法。方法：前处理方法如下：100 m L样品中加入67 m L浓氨水,振荡后静置5 min,转移至D101大孔树脂柱上,上样完毕后,依次以100 m L氨试液、100 m L水和100 m L 40%乙醇洗脱,弃去洗脱液,然后以100 m L 70%乙醇洗脱,收集洗脱液,蒸干,用甲醇溶解并转移至5 m L容量瓶中,以甲醇溶解;测定方法如下：采用Agilent ZORBAX Eclipse XDB C18（4.6×150 mm,5.0μm）色谱柱,以乙腈-水（33：67）为流动相,流速1.0 m L·min-1,柱温35℃;ELSD检测器的参数为：氮气流速1.60 SLM、雾化器温度30℃、蒸发器温度80℃。结果：黄芪甲苷线性范围为0.262~15.696μg（r=0.9992）,平均加样回收率为99.46%（n=6）,RSD为2.3%。结论：所建立的前处理方法简便易行,准确度高,重复性好;检测方法可作为藿苏养胃口服液的质量控制方法。

Objective： To establish a HPLC method for the pretreatment and determination of Astragaloside IV in Huosuyangwei Oral Liquid. Methods： The pretreatment method was as follows： 67 m L ammonium hydroxide was added into 100 m L sample, shaked and stood for 5 mins, then transfered to the column filled with D101 macroporous resin. And then to elute it with 100 m L of water, 100 m L of 40% ethanol orderly and discard the elution buffer. Finally, 100 m L 70% ethanol was added into the column to collect the sample,the elution buffer was gathered and evaporated to dryness, which was dissolved with methanol and transfered into 5 m L volumetric flask.The HPLC-ELSD determination method was as follows： the separation was performed on an Agilent ZORBAX Eclipse XDB C18 analytical column（4.6×150 mm, 5.0 μm I.D） with mobile phase consisting of acetonitrile-water（33： 67）. The flow rate was 1.0 m L·min-1,while the column was kept at 35 ℃. ELSD was employed as the detector. The temperature of nebuliser and evaporator was set at 30℃and 80℃, respectively. The flow rate of N2 was 1.60 SLM. Results： The linear of Astragaloside IV was 0.262-15.696 μg（r = 0.9992） and the average recovery was 99.46% with RSD of 2.3%（n=6）. Conclusion： The pretreatment method with a high accuracy was simple and convenient. The HPLC method of Astragaloside IV determination was suitable for the quality control of Huosuyangwei Oral Liquid.