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目的建立同时测定中药鲜地黄中主要的3种低聚糖的HPLC-ELSD含量测定方法。方法采用HPLC-ELSD对鲜地黄中主要的低聚糖进行研究,采用Waters XBridgeTMAmide 3.5μm(4.6 mm×150 mm)色谱柱为固定相,乙腈-水-70∶30为流动相,流速为0.5 mL.min-1,柱温:25℃。ELSD检测器:漂移管温度40℃,雾化气体2.07 L.min-1,喷雾模式:冷却。结果该方法下,鲜地黄中3种低聚糖分离效果良好,具有良好的线性范围,分别为0.184～9.2μg(r=0.999 8),0.458～11.45μg(r=0.999 7)和0.924～11.55μg(r=0.999 2),平均加样回收率为96.94%(RSD,1.87%),98.87%(RSD,1.98%)和101.02%(RSD,3.23%)。结论该方法稳定、可靠、精密度高、重复性好,为有效控制鲜地黄药材的内在质量提供科学依据。
Objective To establish a HPLC-ELSD method for the simultaneous determination of three major oligosaccharides in fresh rehmannia glutinosa. Methods The main oligosaccharides in fresh rehmannia were studied by HPLC-ELSD. The mobile phase consisted of acetonitrile-water-70:30 with a flow rate of 0.5 mL using a 4.6 μm × 150 mm column with Waters XBridge TMAmide as the stationary phase. .min-1, column temperature: 25 ℃. ELSD detector: drift tube temperature 40 ° C, atomizing gas 2.07 L.min-1, spray mode: cooling. Results Under this method, the separation of three kinds of oligosaccharides in fresh rehmanniae was good and the linear range was 0.184 ~ 9.2μg (r = 0.999 8), 0.458 ~ 11.45μg (r = 0.999 7) and 0.924 ~ 11.55 The average recovery was 96.94% (RSD, 1.87%), 98.87% (RSD, 1.98%) and 101.02% (RSD, 3.23%), respectively. Conclusion The method is stable, reliable, accurate and reproducible. It provides a scientific basis for the effective control of the intrinsic quality of fresh rehmannia.