丹栀颗粒的质量标准研究

Study on Quality Standard of Danzhi Qranules

关键词:  丹栀颗粒  质量标准  薄层色谱  高效液相色谱法

Key words:  Danzhi granules  quality standards  TLC  HPLC

摘要:

目的 建立丹栀颗粒的质量标准。方法 采用薄层色谱法对处方中的栀子、白芍和黄芩进行定性鉴别；采用HPLC同时测定芍药苷和丹酚酸B的含量，色谱柱为Agilent C₁₈柱（250 mm×4.60 mm，5 μm），以乙腈（A）-0.1%磷酸溶液（B）为流动相进行梯度洗脱，检测波长为230 nm，流速1.0 mL·min^–1，柱温25℃，进样量10 μL。结果 栀子苷、芍药苷和黄芩苷的薄层色谱斑点清晰，分离度好。芍药苷在6.1~54.9 μg·mL^–1内与色谱峰面积呈良好的线性关系（r=0.999 5），平均加样回收率为99.08%，RSD为1.53%；丹酚酸B在6.8~61.2 μg·mL^–1内与色谱峰面积呈良好的线性关系（r=0.999 9），平均加样回收率为99.39%，RSD为0.89%。结论 该方法灵敏度高，专属性强，重复性好，可用于丹栀颗粒的质量控制研究。

Abstract:

OBJECTIVE To establish the quality standard of Danzhi granules. METHODS Gardeniae Fructus, Paeoniae Radix Alba and Scutellariae Radix were identified by TLC. The contents of paeoniflorin and salvianolic acid B were determined by HPLC. The chromatographic column was Agilent C₁₈(250 mm×4.6 mm, 5 μm)_.The mobile phase was acetonitrile(A)-0.1% phosphoric acid solution(B) and gradient elution was performed. The detection wavelength was 230 nm. The flow rate was 1.0 mL·min^-1. The column temperature was 25℃. The injection volume was 10 μL. RESULTS TLC spots of geniposide, paeoniflorin and baicalin were clear with good separation. There was a good linear relationship between the concentration and the chromatographic peak area. The liner ranges were 6.1-54.9 μg·mL^-1 for paeoniflorin(r=0.999 5). The liner ranges were 6.8-61.2 μg·mL^-1 for salvianolic acid B(r=0.999 9). The average recoveries of paeoniflorin was 99.08% and RSD was 1.53%. The average recoveries of salvianolic acid B was 99.39% and RSD was 0.89%. CONCLUSION The method is sensitive, specific and reproducible, which can be used for the quality control of Danzhi granules.