七味糖脉舒片HPLC指纹图谱建立及其中6种成分同时测定

Establishment of HPLC fingerprints of Qiwei Tangmaishu tablet and simultaneous determination of six constituents

目的建立七味糖脉舒片的HPLC指纹图谱,并同时测定麦角甾苷、马替诺皂苷、毛蕊异黄酮葡萄糖苷、五味子醇甲、芒柄花素、五味子甲素6种成分含有量。方法该药50%甲醇提取液的分析采用Waters Symmetry C18色谱柱,柱温30℃;检测波长分别为330 nm(检测麦角甾苷、马替诺皂苷)和254 nm(检测毛蕊异黄酮葡萄糖苷、五味子醇甲、芒柄花素、五味子甲素);流动相:乙腈-0.2%甲酸水溶液,梯度洗脱,体积流量1.0 ml/min。结果10批样品中有13个共有峰,相似度均>0.9;麦角甾苷、马替诺皂苷、毛蕊异黄酮葡萄糖苷、五味子醇甲、芒柄花素和五味子甲素分别在1.47~36.75、0.66~16.50、0.89~22.25、2.58~64.50、1.91~47.75、0.77~19.25μg/ml范围内线性关系良好(r≥0.9993),平均加样回收率分别为97.57%、99.22%、96.69%、100.01%、98.79%和96.77%,RSD分别为0.79%、1.54%、0.61%、0.64%、0.83%和0.36%。结论该法操作简便、重复性好,可用于七味糖脉舒片的质量控制。

Objective To establish HPLC fingerprints of Qiwei Tangmaishu tablet and simultaneously determine the contents of the six constituents,acteoside,martynoside,calycosin 7-O-β-D-glucopyranoside,schisandrin,formononetin and deoxyschizandrin.Methods The analysis of 50%methanol extract of this drug was performed on a 30℃thermostatic Waters Symmetry C18 column,with the mobile phase comprising of acetonitrile(A)-0.2%formic acid solution(B)flowing at 1.0 ml/min in a gradient elution manner.The detection wavelength was set at 330 nm for acteoside and martynoside,254 nm for calycosin 7-O-β-D-glucopyranoside,schisandrin,formononetin and deoxyschizandrin.Results There were thirteen common peaks in the fingerprints of ten batches of samples with the similarities more than 0.9.Acteoside,martynoside,calycosin 7-O-β-D-glucopyranoside,schisandrin,formononetin and deoxyschizandrin showed good linear relationship within the ranges of 1.47-36.75,0.66-16.50,0.89-22.25,2.58-64.50,1.91-47.75 and 0.77-19.25μg/ml(r≥0.9993),and their average recoveries were 97.57%,99.22%,96.69%,100.01%,98.79%and 96.77%,with the RSD of 0.79%,1.54%,0.61%,0.64%,0.83%and 0.36%,respectively.Conclusion The established method is easily operable and repeatable,which could be used for quality control of Qiwei Tangmaishu tablet.