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[摘要]
目的 建立HPLC波长切换法同时测定威喜丸中猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸的方法。方法 采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5 μm);流动相:乙腈–0.05%磷酸溶液,梯度洗脱;0~24.0 min在248 nm波长下检测猪苓酮B和猪苓酮A,24.0~50.0 min在210 nm波长下检测去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸;体积流量1.0 mL/min;柱温30℃;进样量为10 μL。结果 猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸分别在5.79~115.80、1.66~33.20、3.28~65.60、7.07~141.40、1.46~29.20、0.88~17.60μg/mL与峰面积线性关系良好;平均加样回收率分别为98.75%、97.60%、98.23%、99.49%、97.10%、96.81%,RSD值分别为0.75%、1.66%、1.44%、0.90%、1.15%、1.38%。结论 本方法简便、准确、重复性好,为威喜丸的质量控制提供了实验依据。
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[Abstract]
Objective To establish an HPLC with wavelength switching method for determination of polyporusterone B, polyporusterone A, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid in Weixi Pills. Methods The separation was carried out on Agilent Eclipse XDB-C18 chromatography column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of acetonitrile - 0.05% phosphoric acid solution with gradient elution. The detection wavelengths were set at 248 nm in 0 - 24.0 min (determination of polyporusterone B and polyporusterone A) and 210 nm in 24.0 - 50.0 min (determination of dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid and pachymic acid). The flow rate was 1.0 mL/min, temperature of column was set at 30℃, and volume of injection was 10 µL. Results The linear ranges of polyporusterone B, polyporusterone A, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid were 5.79 - 115.80, 1.66 - 33.20, 3.28 - 65.60, 7.07 - 141.40, 1.46 - 29.20, and 0.88 - 17.60 μg/mL, respectively. The average recoveries were 98.75%, 97.60%, 98.23%, 99.49%, 97.10%, and 96.81%, with RSD 0.75%, 1.66%, 1.44%, 0.90%, 1.15%, and 1.38%. Conclusion The method is simple, accurate and reproducible, and provides an experimental basis for the quality control of Weixi Pills.
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