加减玉液颗粒的质量标准研究

Study on Quality Standard of Jiajianyuye Granule

目的建立加减玉液颗粒质量标准。方法运用薄层色谱对制剂中葛根、山茱萸进行鉴别;通过高效液相色谱-蒸发光散射检测器对制剂中黄芪甲苷进行含量测定:色谱柱为Waters Xbridge C18(4.6 mm×250 mm,5μm),柱温40℃,流动相为乙腈-水(32∶68,V/V),流速1 mL·min^-1,检测器为蒸发光散射检测器,漂移管温度为45℃,载气流速为1.5 L·min^-1。结果葛根、山茱萸TLC斑点清晰,分离良好,无阴性干扰;黄芪甲苷在0.0721~0.5771 mg·mL^-1范围内呈线性关系(r^2=0.999),精密度、稳定性和重复性试验RSD小于3%,平均加样回收率为102.02%。结论本研究所建立的质量标准方法准确可靠,可用于加减玉液颗粒质量控制。

OBJECTIVE To establish quality standard of Jiajianyuye granule.METHODS Puerariae lobatae radix and Corni fructus were identified by TLC from Jiajianyuye granule.The content of AstragalosideⅣfrom the granule was measured by HPLC-ELSD.The assay was carry out on the Waters Xbridge C18 column(4.6 mm×250 mm,5μm)with column temperature at 40℃,the mobile phase consist of acetonitrile-water(32∶68,V/V)at the flow rate of 1 m L·min^-1,ELSD was equipped with the drift tube temperature at45℃and the carrier gas flow rate at 1.5 L·min^-1.RESULTS TLC of Puerariae lobatae radix and Corni fructus had clear,well separated spots and without negative interference.Astragaloside Ⅳ showed good linear relationship between 0.0721-0.5771 mg·m L^-1(r^2=0.999).RSD was less than 3% in precision test,stability test and repeatability test.The average recovery rate was 102.02%.CONCLUSION The established quality standard method is accurate and reliable,which could be applied to quality control of Jiajianyuye granule.