清咽利喉胶囊的质量标准研究

Quality standard for Qingyan Lihou Capsules

目的建立清咽利喉胶囊(丁香、甘草、诃子等)的质量标准。方法采用薄层色谱法对处方中丁香、冰片、甘草、诃子予以鉴别;丁香酚、甘草酸的定量测定采用高效液相色谱法。应用Diamonsil C18(4.6 mm×250 mm,5μm)色谱柱,丁香酚以甲醇-0.14%磷酸溶液(65∶35)为流动相,体积流量为1 mL/min,检测波长为280 nm,柱温为30℃;甘草酸以甲醇-0.2 mol/L醋酸铵溶液-冰醋酸(67∶33∶1)为流动相,体积流量为1 mL/min,检测波长为250 nm,柱温为30℃。结果薄层色谱检出了丁香、冰片、甘草、诃子,特征斑点分离清晰,阴性对照无干扰。丁香酚在0.248～1.490μg范围内,与峰面积具有良好的线性关系,相关系数为0.999 9;平均回收率为98.27%,RSD为1.06%(n=9)。甘草酸在0.098 5～0.344 6μg范围内,与峰面积具有良好的线性关系,相关系数为0.999 8;平均回收率为98.53%,RSD为1.09%(n=9)。结论该方法灵敏准确、专属性强、重复性好,可用于清咽利喉胶囊的质量控制。

AIM To establish the qualitiy standard for Qingyan Lihou Capsules（Caryophylli Flos,Glycyrrhizae Radix et Rhizoma,Chebulae Fructus,etc.）.METHODS TLC was applied to the identification of Caryophylli Flos,Borneolum Syntheticum,Glycyrrhizae Radix et Rhizoma and Chebulae Fructus in the prescription.The contents of eugenol and glycyrrhizic acid were measured by HPLC with Diamonsil C18（4.6 mm×250 mm,5 μm）.The mobile phase for eugenol alas carbinol-0.14% phosphoric acid solution（65∶ 35） with the flow velocity of 1 mL/min,detection wavelength of 280 nm and column temperature of 30 ℃.The carbinol-0.2 mol/L ammonium acetate solution-glacial acetic acid（67∶ 33∶ 1） was the mobile phase for glycyrrhizic acid with flow velocity of 1 mL/min,detection wavelength of 250 nm and column temperature of 30 ℃.RESULTS TLC of Caryophylli Flos,Borneolum Syntheticum,Glycyrrhizae Radix et Rhizoma and Chebulae Fructus had distinct separation of characteristic spots and there was no interference in negative comparison.Eugenol possessed a favorable linear relationship between the peak areas and sample sizes ranging from 0.248 to 1.490 μg.The correlation coefficient was 0.999 9.The average recovery was 98.27% with RSD of 1.06%（n=9）.With the ranges sample sizes from 0.098 5 to 0.344 6 μg,glycyrrhizic acid possessed a favorable linear relationship with the peak areas.The correlation coefficient was 0.999 8.The average recovery was 98.53% with RSD of 1.09%（n=9）.CONCLUSION This method proves to be sensitive,precise and of strong specificity and high reproducibility,and can be used for the quality control of Qingyan Lihou Capsules.