HPLC同时测定健脾益肾颗粒中的7种成分

Simultaneous determination of seven components in Jianpi Yishen granules by HPLC

目的采用高效液相一测多评法(HPLC-QAMS)同时测定健脾益肾颗粒中党参炔苷、丁香苷、红景天苷、女贞苷、特女贞苷、白术内酯Ⅲ、白术内酯Ⅰ等成分的含量。方法采用Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm)色谱柱,柱温30℃,流动相为乙腈-0.2%磷酸水溶液,梯度洗脱,流速1.0 mL·min^(-1)。以特女贞苷为内参物,建立其他6个成分的相对校正因子,并计算各成分的含量。结果党参炔苷、丁香苷、红景天苷、女贞苷、特女贞苷、白术内酯Ⅲ、白术内酯Ⅰ的线性范围分别为3.69~92.25、0.57~14.25、2.89~72.25、6.46~161.50、9.78~244.50、1.19~29.75、0.96~24.00μg·mL^(-1)(r≥0.9993),平均加样回收率分别为98.46%、97.85%、99.41%、99.09%、100.06%、97.63%、96.97%,RSD分别为1.07%、0.99%、1.14%、0.81%、0.69%、1.39%、1.28%。一测多评法所得结果与外标法无明显差异。结论所用方法准确、重复性好,可用于健脾益肾颗粒中7种成分的质量控制。

OBJECTIVE To establish an HPLC-QAMS method for the simultaneous determination of lobetyolin,syringin,salidroside,ligustroflavone,specnuezhenide,atracylenolideⅢand atracylenolide I in Jianpi Yishen granules.METHODS An HPLC-QAMS method was adopted on Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm).The mobile phase consisted of acetonitrile-0.2%phosphoric acid aqueous solution with gradient elution.The flow rate was set at 1.0 mL·min^(-1).The column temperature was 30℃.Specnuezhenide was used as an internal standard to calculate the relative correction factors of the other six constituents,then the content determination was made.RESULTS Lobetyolin,syringin,salidroside,ligustroflavone,specnuezhenide,atracylenolideⅢand atracylenolideⅠshowed good linear relationships within the ranges of 3.69-92.25,0.57-14.25,2.89-72.25,6.46-161.50,9.78-244.50,1.19-29.75,and 0.96-24.00μg·mL^(-1)(r≥0.9993),respectively.The average recoveries(RSDs)were 98.46%(1.07%),97.85%(0.99%),99.41%(1.14%),99.09%(0.81%),100.06%(0.69%),97.63%(1.39%)and 96.97%(1.28%),respectively.There was no significant difference in assay results between QAMS and the external standard method.CONCLUSION The method is accurate and has a good repeatability,which can be used for the quality control of seven components in Jianpi Yishen granules.