[關(guān)鍵詞]
[摘要]
目的 建立高效液相色譜聯(lián)合電噴霧檢測器（HPLC-CAD）測定小柴胡片中琥珀酸、鹽酸麻黃堿、黃芩苷、漢黃芩苷、柴胡皂苷a、柴胡皂苷d、甘草酸、甘草次酸、棕櫚酸的分析方法。方法 采用GL Science Inertsil ODS-3色譜柱（250mm×4.6mm，3μm）；流動相：5mmol/L甲酸銨（甲酸調(diào)pH值至4.2）–乙腈，梯度洗脫；柱溫：35 ℃；進樣量：20μL；體積流量：0.7mL/min；CAD霧化器溫度為35 ℃，氣壓為61.0psi，采集頻率為10Hz。結(jié)果 琥珀酸、鹽酸麻黃堿、黃芩苷、漢黃芩苷、柴胡皂苷a、柴胡皂苷d、甘草酸、甘草次酸、棕櫚酸的線性范圍分別為0.94～18.74、1.23～24.66、8.90～178.06、3.51～70.20、1.52～30.36、1.25～25.02、3.48～69.54、2.50～50.04、1.23～24.56μg/mL；平均回收率分別為97.05%、97.82%、97.85%、96.46%、98.53%、97.58%、97.05%、97.65%、97.03%，RSD值分別為1.46%、2.16%、0.83%、1.00%、1.74%、1.49%、0.75%、1.68%、1.46%。結(jié)論 本法簡便、準確，為小柴胡片的質(zhì)量標準提升研究提供有效的技術(shù)手段。
[Key word]
[Abstract]
Objective To develop an HPLC-CAD method for simultaneous determination of succinic acid, ephedrine hydrochloride, baicalin, wogonoside, saikosaponin a, saikosaponin d, glycyrrhizic acid, glycyrrhetinic acid, and palmitic acid in Xiaochaihu Tablets. Methods The chromatographic separation was performed on a GL Science Inertsil ODS-3 column GL (250 mm×4.6 mm, 3 μm) with 5 mmol/L ammonium formate (formic acid ajust pH 4.2)-acetonitrile as the mobile phase with gradient elution. The column temperature was set at 35℃, injection volume was 20 μL, and flow rate was 0.7 mL/min. For CAD, the nebulization temperature of detector was set as 35℃, the gas pressure was 61.0 psi, and acquisition frequency was 10 Hz. Results The linear ranges of succinic acid, ephedrine hydrochloride, baicalin, wogonoside, saikosaponin a, saikosaponin d, glycyrrhizic acid, glycyrrhetinic acid, and palmitic acid were 0.94-18.74, 1.23-24.66, 8.90-178.06, 3.51-70.20, 1.52-30.36, 1.25-25.02, 3.48-69.54, 2.50-50.04, and 1.23-24.56 μg/mL, respectively. The average recoveries were 97.05%, 97.82%, 97.85%, 96.46%, 98.53%, 97.58%, 97.05%, 97.65%, and 97.03% with RSD values of 1.46%, 2.16%, 0.83%, 1.00%, 1.74%, 1.49%, 0.75%, 1.68%, and 1.46%, respectively. Conclusion The method is simple and accurate, which can provide an effective technical means for the study on the improvement of the quality standard of Xiaochaihu Tablets.
[中圖分類號]
R286.02
[基金項目]
中國醫(yī)學(xué)科學(xué)院醫(yī)學(xué)與健康科技創(chuàng)新工程項目（2019-I2M-5-020）
