柴葶宁肺颗粒质量标准研究

Quality Standard of Chaiting Ningfei Granules

目的建立柴葶宁肺颗粒的质量标准。方法采用薄层色谱(TLC)法定性鉴别制剂中丹参、白芍、黄芩、钩藤4味药材;采用高效液相色谱法同时测定柴葶宁肺颗粒中芍药苷、黄芩苷、丹酚酸B、甘草酸、汉黄芩素的含量,色谱柱为Tabitha RZ-C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为1 mL/min,检测波长为245 nm,柱温为30℃,进样量为10μL。结果丹参、白芍、黄芩、钩藤的TLC图斑点清晰,分离度好,阴性对照无干扰。芍药苷、黄芩苷、丹酚酸B、甘草酸、汉黄芩素质量浓度分别在13.01~130.14μg/mL、14.85~148.53μg/mL、9.49~94.86μg/mL、1.28~12.76μg/mL、1.25~12.54μg/mL(r>0.9996)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.0%(n=6);平均加样回收率分别为99.80%,100.68%,101.68%,102.65%,99.50%,RSD分别为1.48%,1.52%,0.95%,1.91%,1.35%(n=6)。结论所建立的方法可用于柴葶宁肺颗粒的质量控制。

Objective To establish a quality standard of Chaiting Ningfei Granules.Methods Salviae Miltiorrhizae Radix et Rhizome,Paeoniae Radix Alba,Scutellariae Radix and Uncariae Ramulus cum Uncis in the preparation were identified by the thin layer chromatography(TLC)method.The contents of paeoniflorin,baicalin,paeonianolic acid B,glycyrrhizic acid and baicalein in Chaiting Ningfei Granules were determined by the high-performance liquid chromatography(HPLC)method,the chromatographic column was Tabitha RZ-C_(18)column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.1%phosphoric acid solution(gradient elution),the flow rate was 1 mL/min,the detection wavelength was 245 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The TLC spots of Salviae Miltiorrhizae Radix et Rhizome,Paeoniae Radix Alba,Scutellariae Radix and Uncariae Ramulus cum Uncis were clear and well separated,and the negative samples had no interference.The mass concentrations of paeoniflorin,baicalin,paeonianolic acid B,glycyrrhizic acid and baicalein showed a good relationship with the peak area in the ranges of 13.01-130.14μg/mL,14.85-148.53μg/mL,9.49-94.86μg/mL,1.28-12.76μg/mL and 1.25-12.54μg/mL(r>0.9996),respectively.The RSDs of precision,stability and repeatability tests were less than 2.0%(n=6).The average recoveries of the five components were 99.80%,100.68%,101.68%,102.65%and 99.50%with RSDs of 1.48%,1.52%,0.95%,1.91%,1.35%(n=6),respectively.Conclusion The established method can be used for the quality control of Chaiting Ningfei Granules.