目的:优化与提升蒙药制剂钦汤散的质量标准。方法:采用薄层色谱(thin layer chromatography,TLC)法对钦汤散中五灵脂和红花进行定性鉴别;采用高效液相色谱(high performance liquid chromatography,HPLC)法测定穗花衫双黄酮的含量,色谱条件为C18色谱柱(250 mm×4.6 mm,5 μm),流动相为甲醇-0.1%磷酸水(66∶34),柱温为25 ℃,检测波长为330 nm,流速为1.0 mL/min。结果:TLC法结果显示,供试品在与对照品或对照药材色谱图相应位置上显示相同颜色斑点,且阴性对照无干扰,专属性强;HPLC法结果显示,穗花衫双黄酮峰面积在12.0~21.6 μg/mL范围线性关系良好,回归方程为y=119 894x-253 379(R2=0.999 3);高中低加样回收率试验,平均回收率为104.5%、102.9%、103.5%,RSD为1.15%、1.63%、0.28%;穗花衫双黄酮含量在0.012 84%~0.012 93%区间范围内。结论:本研究所建立的蒙药钦汤散的鉴别和含量测定方法准确可靠,灵敏度高、重复性好、精密度高和专属性强,可以用于优化与提升蒙药制剂钦汤散的质量标准。
Objective:To optimize and improve the quality standard of Mongolian medicine Qintang powder. Methods: TLC (thin layer chromatography, TLC) was used for the qualitative identification of safflower and Wulingzhi in Qintang. HPLC (high performance liquid chromatography, HPLC)was used to determine the content of amentoflavone. The chromatographic separation was preformed on a C18(250 mm ×4.6 mm, 5 μm) column with mobile phase of methanol -0.1% phosphoric acid. The detection wavelength was set at 330 nm, with the flow rate of 1.0 mL/min. Results: The TLC spots were clear without negative interference. The linear ranges of amentoflavone were 12.0~21.6 μg /mL, and the regression equation was y=119 894x-253 379 (R2=0.999 3). The average recovery rates were 104.5%, 102.9% and 103.5% respectively in high-, middle- and low recovery rate tests, with the RSD of 1.15%,1.63% and 0.28%. The content of amentoflavone was 0.012 84%~0.012 93%. Conclusion: The identification and content determination methods of Qintang powder established in this study are accurate and reliable, with high sensitivity, good repeatability, high precision and strong specificity, which can be used to optimize and improve the quality standard of Mongolian medicine Qintang powder.
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