五倍子颗粒质量标准研究

Study on the quality standard of Galla Chinensis granules

试验旨在建立五倍子颗粒质量控制标准。采用薄层色谱法(TLC)对五倍子药材进行定性鉴别,采用高效液相色谱法(HPLC)测定没食子酸含量,色谱柱为Waters Xselect?HSS T3柱(250.0 mm×4.6 mm,5μm),流动相为乙腈-甲酸溶液(pH值3.2),梯度洗脱,流速0.5 mL/min,检测波长273 nm,柱温30℃。同时,对五倍子颗粒粒度、水分、溶化性和装量进行检查。试验结果显示,没食子酸在16.05~256.80μg范围内与峰面积线性关系良好(R^(2)=0.999 9)。精密度试验、稳定性试验、重复性试验RSD均小于等于1.0%;平均加样回收率为95.83%,RSD为1.29%。五倍子颗粒粒度、水分、溶化性和装量等均符合2020年版《中华人民共和国兽药典》颗粒剂项下的规定。本研究建立的TLC和HPLC方法专属性强、重复性好、准确可靠,能够有效评价五倍子颗粒质量。

To establish a quality control standard for Galla Chinensis granules.Thin layer chromatography(TLC)was used to qualitatively identify Galla Chinensis medicinal materials,and gallic acid content was determined by high performance liquid chromatography(HPLC),the column was Waters Xselect®HSS T3(250.0 mm×4.6 mm,5μm),the mobile phase was acetonitrile-formic acid solution(pH 3.2,gradient elute),the flow rate was 0.5 mL/min,the detection wavelength was 273 nm,and the column temperature was 30℃.Additionally,the particle size,moisture,solubility and loading capacity of Galla Chinensis granules were checked.The results showed that galic acid had a good linear relationship with the peak area in the range of 16.05-256.80μg(R^(2)=0.9999).The RSD of precision test,stability test and repeatability test was not more than 1.0%;the average dosing recovery rate was 95.83%with RSD of 1.29%.The particle size,moisture,solubility and loading volume were in line with the provisions under granules in the 2020 edition of Chinese Veterinary Pharmacopoeia.The presented result suggested TLC and HPLC methods had strong specificity,good repeatability,accuracy and reliability,and could effectively evaluate the quality of Galla Chinensis granules.