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目的:优选黄蒲通窍胶囊的最佳提取工艺。方法:采用L9(34)正交表,以浸膏得率、浸膏中大黄和石菖蒲有效成分含量为指标,考察不同因素水平对提取工艺的影响。采用UPLC法,以BEH C18(50mm×2.1mm,1.7μm)色谱柱为固定相;以甲醇:0.1%的磷酸(85:15,v:v)为流动相;波长检测254nm;柱温30℃测定大黄素、大黄酚、大黄素甲醚总含量;以BEH C18(50mm×2.1mm,1.7μm)色谱柱为固定相;以水:乙腈(38:62,v:v)为流动相,检测波长257nm;柱温30℃测定β-细辛醚含量。结果:以浸膏得率、浸膏中大黄和石菖蒲有效成分3个指标综合评定,确定最佳提取工艺条件为:乙醇浓度为70%,10倍8倍量提取2次。第1次回流2h,第2次回流1.5h,残渣加8倍量水,煎煮1h。UPLC法同时测定3种大黄成分及β-细辛醚含量方法快捷、准确、重复性好。结论:实验优选出来的提取工艺有效成分提取率较高,提取工艺简便、可行。
Objective: To optimize the best extraction process of Huangpu tongqiao capsule. Methods: L9 (34) orthogonal test was used to evaluate the effects of different factors on the extraction process, taking the extract yield, the content of active ingredients in Rhubarb and Acorus calamus as indexes. The mobile phase consisted of BEH C18 (50mm × 2.1mm, 1.7μm) column with UPLC and methanol: 0.1% phosphoric acid (85:15, v: v) The total content of emodin, chrysophanol and physcion was determined. The mobile phase consisted of BEH C18 (50mm × 2.1mm, 1.7μm) column and water: acetonitrile (38:62, v: v) Wavelength 257nm; column temperature 30 ℃ Determination of β-asarone content. Results: The optimum extraction conditions were as follows: the concentration of ethanol, the concentration of ethanol was 70%, the amount of 8 times of 10 times and the amount of extract of rhubarb and Acorus calamus active ingredients were comprehensively evaluated. The first reflux 2h, the second reflux 1.5h, the residue plus 8 times the amount of water, boiling 1h. UPLC method for the simultaneous determination of three kinds of rhubarb composition and β-asarone content method is fast, accurate and reproducible. Conclusion: The optimum extraction rate of active ingredients extracted from the experiment is high, the extraction process is simple and feasible.