经典名方大山楂丸质量标准的改进和提升研究

Study on the improvement and promotion of quality standard of classical herbal prescription Dashanzha Pills

[目的]探讨经典名方大山楂丸质量标准的改进和提升.[方法]采用薄层色谱法(TLC)对制剂鉴别进行方法学改进,增加山楂中槲皮素的定性鉴别;优化并建立大山楂丸中熊果酸和齐墩果酸含量HPLC同测技术:采用Ace Excel 5 C_(18)色谱柱(4.6×250 mm,5μm),流动相甲醇-0.5%(体积分数)磷酸(83∶17),进样量为10μL,流动速度为1.0 mL·min^(-1),柱温30℃,检测波长为212 nm.[结果]TLC鉴别槲皮素斑点清晰,专属性强;熊果酸在0.0311~0.9380 g·L^(-1)梯度质量浓度范围呈良好的线性关系(r=0.9999),平均回收率为100.96%,RSD=0.43%;齐墩果酸在0.0081~0.2343 g·L^(-1)梯度质量浓度范围呈良好的线性关系(r=0.9999),平均回收率为96.61%,RSD=0.60%.[结论]改进和提升后的质量标准科学可行,可用于经典名方大山楂丸的质量控制.

OBJECTIVE To explore the improvement and promotion of quality standard of classical herbal prescription Dashanzha Pills.METHODS Thin layer chromatography(TLC)was used to improve the method of preparation identification and increase the qualitative identification of quercetin in Dashanzha Pills.HPLC method for the simultaneous determination of ursolic acid and oleanolic acid in Dashanzha Pills was optimized and established.Ace Excel 5 C_(18)column(4.6×250 mm,5μm)was adopted.The mobile phase was a mixture of methanol and 0.5%(volume fraction)phosphoric acid(83∶17).The injection volume and flow rate were 10μL and 1.0 mL·min^(-1),respectively.The column temperature was 30℃,and the detection wavelength were 212 nm.RESULTS TLC could identify quercetin spots clearly and specifically.Ursolic acid showed a good linear relationship in the range of 0.0311-0.9380 g·L;(r=0.9999),and the average recovery rate was 100.96%,RSD=0.43%.Oleanolic acid showed a good linear relationship in the range of 0.0081-0.2343 g·L;(r=0.9999),and the average recovery rate was 96.61%,RSD=0.60%.CONCLUSION The improved and promoted quality standard is scientific and feasible,and can be used for the quality control of classical herbal prescription Dashanzha Pills.