超高效液相色谱波长切换法同时测定二母宁嗽丸中7个成分含量

目的建立超高效液相色谱(ultra performance liquid chromatography,UPLC)波长切换法同时测定二母宁嗽丸中栀子苷、橙皮苷、黄芩苷、甘草苷、甘草次酸、甘草酸铵和五味子醇甲的含量。方法采用Phenomenex Kinetex C18色谱柱(4.6 mm×100 mm,2.7μm),以甲醇(A)-0.05%磷酸溶液(B)为流动相,梯度洗脱,流速0.6 ml/min;栀子苷、甘草苷、甘草酸铵、甘草次酸检测波长为237 nm,黄芩苷、橙皮苷检测波长为280 nm,五味子醇甲检测波长为250 nm;柱温35℃,进样量2μl。结果栀子苷、橙皮苷、黄芩苷、甘草苷、甘草次酸、甘草酸铵和五味子醇甲分别在10.294~205.888、4.552~91.036、6.212~124.248、8.974~179.484、2.629~52.580、5.371~107.416、8.905~178.104 ng范围内线性关系良好(r为0.9996~0.9999);平均加样回收率分别为98.47%、99.04%、100.76%、98.27%、100.50%、98.79%、99.37%(RSD<2.0%,n=6);精密度、重复性、稳定性(24 h)试验的RSD<2.0%(n=6)。结论该方法简单、有效、结果准确,可用于二母宁嗽丸中上述7个成分含量的同时测定。

Simultaneous determination of seven constituents in Ermu-Ningsou Pills by UPLC with wavelength switching method

Objective To develop a method for simultaneous determination of the contents of geniposide,hesperidin,baicalin,liquiritin,glycyrrhetinic acid,glycyrrhizic and schizandrin in Ermu-Ningsou Pills by ultra performance liquid chromatography(UPLC)with wavelength switching.Methods The analyses were carried out on an Phenomenex Kinetex C18 column(4.6 mm×100 mm,2.7μm)with the mobile phase consisting of methanol(A)-0.05%phosphoric acid(B)in a gradient mode at a flow rate of 0.6 ml/min.The detection wavelength was set at 237 nm for geniposide,liquiritin,glycyrrhetinic acid and glycyrrhizic,280 nm for baicalin and hesperidin,250 nm for schizandrin.The column temperature was set at 35℃and the injection volume was 2μl.Results The linear relation of geniposide,hesperidin,baicalin,liquiritin,glycyrrhetinic acid,glycyrrhizic and schizandrin were excellent within the range of 10.294-205.888,4.552-91.036,6.212-124.248,8.974-179.484,2.629-52.580,5.371-107.416,8.905-178.104 ng(r≥0.9995,n=6).Average recoveries were 98.47%,99.04%,100.76%,98.27%,100.50%,98.79%,99.37%(RSD<2.0%,n=6).RSDs of precision,reproducibility and stability tests(24 h)were lower than 2.0%(n=6).Conclusions The method is simple,effective,accurate.It can be used for simultaneous determination of 7 active constituents in Ermu-Ningsou Pills.