HPLC法同时测定银黄制剂中9个成分的含量

目的: 建立同时测定银黄制剂中9个成分(绿原酸、咖啡酸、木犀草苷、黄芩苷、木犀草素、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A)含量的高效液相色谱方法。 方法: 采用Sepax GP-C₁₈ 色谱柱(250 mm×4.6 mm,5 μm),以0.1%甲酸甲醇溶液-0.1%甲酸水溶液为流动相,梯度洗脱,流速1.0 mL·min^-1,黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A的检测波长为275 nm,绿原酸和咖啡酸的检测波长为320 nm,木犀草苷和木犀草素的检测波长为350 nm,柱温30℃,进样量20 μL;液质联用法确认化合物的结构。 结果: 9个成分在考察的浓度范围内,浓度与峰面积之间呈良好的线性关系(r>0.9997);回收率(n=9)均在97.1%~103.9%范围内,RSD均小于2.6%。批内精密度RSD均小于1.0%,批间精密度RSD均小于1.7%。 结论: 本方法简便、准确,精密度高,重复性好,可用于银黄制剂的质量控制。

Objective: To establish an HPLC method for simultaneous determination of nine components(chlorogenic acid,caffeic acid,luteoloside,baicalin,luteolin,wogonoside,baicalein,wogonin and oroxylin A)in Yinhuang preparations. Methods: The chromatographic separations were obtained on a Sepax GP-C₁₈ column(250 mm×4.6 mm,5 μm)with a gradient elution using the mixture of 0.1% formic acid methanol solution and 0.1% formic acid water solution at a flow rate of 1.0 mL·min^-1.The detection wavelengths were respectively set at 275 nm(baicalin,wogonoside,baicalein,wogonin and oroxylin A),320 nm(chlorogenic acid and caffeic acid)and 350 nm(luteoloside and luteolin).The column temperature was set at 30℃.The injection volume was 20 μL.The constituents were confirmed by(-)electrospray ionization LC-MS. Results: All calibration curves were linear(r >0.9997)over the tested ranges.The average recoveries(n=9)ranged from 97.1% to 103.9% with RSD value below 3.0%.The RSDs of within-run and between-run precision were below 1.0% and 1.7%,respectively. Conclusion: The established method is simple,fast,and with high precision,sensitivity and repeatability,which can be used efficiently in the quality control of Yinhuang preparations.