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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 method for the determination of Astragaloside IV in Huoxu Yangwei Oral Liquid by HPLC. Methods: The pretreatment method was as follows: 67 mL of concentrated ammonia water was added into 100 m L sample and allowed to stand for 5 min after shaking. The solution was transferred to a D101 macroporous resin column. After loading, 100 mL of ammonia solution ml of water and 100 ml of 40% ethanol. The eluate was discarded and then eluted with 100 ml of 70% ethanol. The eluate was collected, evaporated to dryness, dissolved in methanol and transferred to a 5 ml volumetric flask , And dissolved in methanol. The determination method was as follows: The column was eluted with an Agilent ZORBAX Eclipse XDB C18 (4.6 × 150 mm, 5.0 μm) column with a flow rate of 1.0 mL · min -1 using acetonitrile-water (33:67) Temperature 35 ° C; ELSD detector parameters: nitrogen flow rate 1.60 SLM, atomizer temperature 30 ° C, evaporator temperature 80 ° C. Results: The linear range of Astragaloside was 0.262 ~ 15.696μg (r = 0.9992). The average recovery was 99.46% (n = 6) and the RSD was 2.3%. Conclusion: The established pretreatment method is simple and easy to operate with high accuracy and good reproducibility. The detection method can be used as quality control method for Huguang Yangwei oral liquid.