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目的建立HPLC-ELSD法测定芪芍方有效部位中黄芪甲苷含量和可见分光光度法测定黄芪总皂苷含量的方法,有效控制芪芍方有效部位质量。方法黄芪甲苷含量测定,采用HPLC-ELSD法,Hypersll-C18色谱柱(250mm×4.6mm,5μm),流动相为乙腈-水(31:69),流速1.0mL/min,柱温30℃,漂移管温度101℃,空气流速2.7L/min。黄芪总皂苷含量测定,采用可见分光光度法,MCI柱层析技术分离黄芪总皂苷类,再经反相C18固相萃取小柱纯化,5%香草醛冰醋酸溶液和高氯酸为显色剂,于543nm处测定。结果HPLC法及可见分光光度法中,黄芪甲苷分别在1.30～7.80μg、0.0108～0.065g/L的范围内呈现良好的线性关系,平均加样回收率分别为95.95%、96.58%,RSD分别为2.46%、2.28%。结论本试验建立的方法简便、准确、重复性好,可用于芪芍方有效部位中黄芪皂苷类的质量控制。
OBJECTIVE To establish a HPLC-ELSD method for the determination of Astragaloside IV in the effective fractions of Astragalus and Radix Paeoniae Alba and the method of visible spectrophotometry to determine the content of Astragalus total saponin, and to effectively control the quality of the effective fractions of Astragalus. Methods The content of astragaloside Ⅳ was determined by HPLC-ELSD with a mobile phase of acetonitrile-water (31:69) at a flow rate of 1.0 mL / min on a Hypersll-C18 column (250 mm × 4.6 mm, 5 μm) Drift tube temperature 101 ℃, air flow rate 2.7L / min. Astragalus total saponin content determination, using visible spectrophotometry, MCI column chromatography separation of total saponins of Astragalus, and then by reversed phase C18 solid phase extraction cartridge purification, 5% vanillin glacial acetic acid solution and perchloric acid as a color reagent , Measured at 543 nm. Results In HPLC and visible spectrophotometry, astragaloside showed a good linear relationship in the range of 1.30 ~ 7.80μg and 0.0108 ~ 0.065g / L, respectively. The average recoveries were 95.95% and 96.58% 2.46%, 2.28%. Conclusion The method established in this study is simple, accurate and reproducible. It can be used for the quality control of Astragalus saponins in the effective fractions of Qishao Fang.