基于一测多评法对肠胃散中8种物质的质量控制

Quality control of eight substances in Changwei San based on quantitative analysis of multi-components by single-marker

目的建立一测多评法同时测定肠胃散中棕矢车菊素、异泽兰黄素、柠檬苦素、吴茱萸碱、吴茱萸次碱、肉桂醇、肉桂酸和桂皮醛的含量。方法色谱柱:Waters Symmetry C18柱(250 mm×4.6 mm,5μm);流动相:乙腈(A)-0.1%磷酸溶液(B),梯度洗脱,流速:1.0 ml/min;检测波长分别为345 nm(检测棕矢车菊素和异泽兰黄素)、215 nm(柠檬苦素、吴茱萸碱和吴茱萸次碱)和275 nm(肉桂醇、肉桂酸和桂皮醛)。以吴茱萸碱为内参物,分别建立其他7种成分的相对校正因子,并用相对校正因子计算含量,实现一测多评;同时与外标法测定结果进行对比,验证一测多评法的准确性和可行性。结果棕矢车菊素、异泽兰黄素、柠檬苦素、吴茱萸碱、吴茱萸次碱、肉桂醇、肉桂酸和桂皮醛分别在0.98~19.60、2.67~53.40、4.06~81.20、1.98~39.60、2.69~53.80、0.56~11.20、1.49~29.80和8.77~175.40μg/ml范围内线性关系良好(r≥0.9992),平均加样回收率(RSD)分别为98.77%(0.96%)、99.38%(1.01%)、100.02%(0.83%)、97.80%(1.40%)、98.91%(1.18%)、96.99%(1.13%)、98.09%(1.24%)和99.10%(0.67%),一测多评法计算结果与外标法实测值无明显差异。结论所建立的方法简便、准确,可用于肠胃散的质量评价。

Objective To establish a quantitative analysis of multi-components by single marker(QAMS)method for the simultaneous determination of jaceosidin,eupatilin,limoni,evodiamine,rutaecarpine,cinnamyl alcohol,cinnamic acid and cinnamaldehyde in Changwei San.Methods The Waters Symmetry C18 column(250 mm×4.6 mm,5μm)was used for the separation,and the mobile phase was the acetonitrile(A)and 0.1%phosphoric acid(B)solution in a gradient elution at a flow rate of 1.0 ml/min.The detection wavelengths were set at 345 nm for jaceosidin and eupatilin,215 nm for limoni,evodiamine and rutaecarpine,and 275 nm for cinnamyl alcohol,cinnamic acid and cinnamaldehyde.With evodiamine as an internal reference standard,the relative correction factors for the other 7 components were established and their contents were calculated with the relative correction factors to achieve the QAMS,and then the differences between the calculated values by QAMS and measured values by the external standard method(ESM)were compared to validate the accuracy and feasibility of the QAMS method.Results Jaceosidin,eupatilin,limoni,evodiamine,rutaecarpine,cinnamyl alcohol,cinnamic acid and cinnamaldehyde showed good linear relationships within the ranges of 0.98-19.60,2.67-53.40,4.06-81.20,1.98-39.60,2.69-53.80,0.56-11.20,1.49-29.80,and 8.77-175.40μg/ml(r≥0.9992),whose average recoveries(RSD)were 98.77%(0.96%),99.38%(1.01%),100.02%(0.83%),97.80%(1.40%),98.91%(1.18%),96.99%(1.13%),98.09%(1.24%)and 99.10%(0.67%),respectively.No significant difference was observed between the calculated values by QAMS and the measured values by ESM.Conclusion The established QAMS method is simple and accurate,which might be used to evaluate the quality of Changwei San.