白及颗粒质量标准研究

Quality Standard of Baiji Granules

目的建立白及颗粒的质量标准。方法采用薄层色谱(TLC)法对白及颗粒中白及药材进行定性鉴别;采用高效液相色谱(HPLC)法测定白及药材中指标性成分1,4-二[4-(葡萄糖氧)苄基]-2-异丁基苹果酸酯的含量,色谱柱为Diamonsil Plus C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(22∶78,V/V),流速为1.0 mL/min,检测波长为223 nm,柱温为30℃,进样量为10μL。结果白及TLC图中特征斑点清晰,阴性对照无干扰。1,4-二[4-(葡萄糖氧)苄基]-2-异丁基苹果酸酯进样量在0.0834~2.5011μg范围内与峰面积线性关系良好(r=0.9999,n=7);精密度、稳定性、重复性试验的RSD均小于2.0%(n=6);平均加样回收率为101.81%,RSD为0.56%(n=6)。结论所建立的方法操作简便,结果准确,稳定性和重复性均较好,可用于白及颗粒的质量控制。

Objective To establish the quality standard of Baiji Granules.Methods The thin-layer chromatography(TLC)method was used for the qualitative identification of Bletillae Rhizoma in Baiji Granules.The high-performance liquid chromatography(HPLC)method was used for the content determination of militarine in Bletillae Rhizoma.The chromatographic column was Diamonsil Plus C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.1%phosphoric acid solution(22∶78,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 223 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The characteristic spots of Bletillae Rhizoma in the TLC chromatograms were clear,and the negative control had no interference.The linear range of militarine was 0.0834-2.5011μg(r=0.9999,n=7).The RSDs of precision,stability and repeatability tests were less than 2.0%(n=6).The average recovery opf militarine was 101.81%with RSD of 0.56%(n=6).Conclusion The method is simple,accurate,stable and reproducible,which can be used for the quality control of Baiji Granules.