解毒浓缩丸中黄芩苷的含量测定及提取工艺的研究

Study on the determination and extraction of baicalin content in the detoxification concentrated pill

目的：制定解毒浓缩丸中黄芩苷的含量测定方法及制备工艺的研究。方法用高效液相色谱法测定。色谱柱：十八烷基硅烷键合硅胶柱，流动相：甲烷-水-0.2%磷酸溶液（43：57：0.2），流速（0.9 mL/min）,检测波长315 nm，柱温：27℃。采用正交实验设计，以黄芩苷含量为指标优化提取工艺。结果线性范围：0.2142～0.4998μg。稳定性：RSD＝0.94%，n＝5。精密度：RSD＝0.97%，n＝6。重复性：RSD＝0.74%，n＝5。回收率：98.26%，RSD＝0.47%，n＝5。样品含量测定数据：不得少于26.0 mg。最佳提取工艺为ABCD，即每次加水10倍量，煎煮2次，每次0.5 h，提取温度60℃。结论本法简便、准确、专属性强，可用于解毒浓缩丸的含量测定。经过优化后制备的解毒浓缩丸各项指标符合药典规定，工艺重复性好，适于规模化生产。

Objective Study on preparation method and determination of baicalin content of detoxification concentrated pill. Methods The analysis was used with a C18 column and a mobile phase of methanol-water-phosphoric acid（43：57：0.2）by HPLC.The flow rate was 0.9 mL/min and column temperature was 27℃. The detection wavelength was set at 315 nm.Through the orthogonal experimental design, the extraction process was optimized by using the content of baicalin as index.Results The linear range：0.214 2 ~ 0.499 8μg. Stability：RSD = 0.94%, n= 5. Precision：RSD = 0.97%, n= 6. Repeatability：RSD = 0.74%, the recovery rate：98.26%, RSD = 0.47%, n= 5. The content of the sample：not less than 26.0 mg. The best extraction process is ABCD, which means 10 times amount of water, decocting for 2 times, each time 0.5h, extraction temperature 60 ℃ . Conclusion The method is simple, accurate, reproducible, and can be used for the determination of detoxification concentrated pill. After optimization of detoxification concentrated pill, every index conform to Pharmacopoeia.The method is repeatable, and is suitable for large-scale production.