清咽颗粒质量标准研究

摘要

目的：建立清咽颗粒的质量标准。方法采用薄层色谱法对清咽颗粒中的主要药味山豆根、南沙参、忍冬藤、麦冬进行定性鉴别。采用高效液相色谱法测定甘草中甘草苷、甘草酸的含量,色谱柱为Thermo Syncronis C18(250 mm×4.6 mm,5µm),流动相为乙腈(含0.05%磷酸,A)-0.05%磷酸溶液(B),梯度洗脱(0～8 min,19%A；8～35 min,19%→50%A),检测波长237 nm,流速1 mL/min。结果薄层色谱斑点清晰,在与对照品或对照药材相应的位置上显相同颜色的斑点,阴性对照无干扰。甘草苷的线性范围为0.05～0.5µg,r＝0.9999,平均回收率为99.97%,RSD＝1.74%(n＝9)；甘草酸铵的线性范围为0.1～2µg,r＝0.9999,平均回收率为99.74%,RSD＝1.28%(n＝9)。结论本方法简便可行,结果准确可靠,重复性好,可作为清咽颗粒的质量控制方法。%Objective To establish the standard for quality control ofQingyan Granule. Methods The chief components of the preparation, Sophora Tonkinensis radix et rhizoma, Adenophorae radix, Lonicera japonica caulis, and Ophiopogonis radix were identified by TLC qualitatively. The contents of licorice glycosides and glycyrrhizic acid were determined by HPLC. The separation was performed on Thermo Syncronis C18 column (4.6 mm×250 mm, 5μm) with mobile phase consisted of acetonitrile with 0.05% phosphoric acid solution (A)-0.05% phosphoric acid solution (B), and gradient elution (0-8 min, 19%A;8-35 min, 19%→50%A). Detection wavelength was 237 nm, and flow rate was 1 mL/min.Results The spots in TLC were clear. There were spots with same color on the corresponding location of reference substance and reference herbal, negative control without interference. The linear range for licorice glycosides was 0.05-0.5μg (r=0.999 9). The average recovery was 99.97%, RSD=1.74% (n=9). The linear range for glycyrrhizic acid was 0.1-2μg (r=0.999 9). The average recovery was 99.74%, RSD=1.28% (n=9). Conclusion The method is simple, accurate, with high reproducibility, which can be used for quality control ofQingyan Granule.