穿心莲配方颗粒的质量标准及指纹图谱研究

Study on Quality Standard and Fingerprints of Andrographis paniculata Dispensing Granule

目的:初步拟定穿心莲配方颗粒的质量标准,并建立其高效液相色谱(HPLC)指纹图谱。方法:分别采用薄层色谱法、HPLC法对穿心莲配方颗粒中穿心莲内酯和脱水穿心莲内酯进行定性鉴别和定量分析,根据2015年版《中国药典》(简称"药典")对其水分、粒度、溶化性、浸出物进行测定;绘制10批穿心莲配方颗粒的HPLC指纹图谱,并与对照指纹图谱进行相似度评价。结果:供试品薄层色谱在对照品色谱相应的位置上显相同颜色的斑点,穿心莲配方颗粒的水分、粒度、溶化性、浸出物测定结果均符合药典标准。穿心莲内酯和脱水穿心莲内酯检测质量浓度的线性范围分别为10.983～274.583、11.355～283.886 mg/L(r均为0.999 9),精密度试验的RSD分别为0.50%、0.29%(n=6),重复性试验的RSD分别为0.99%、0.51%(n=6),室温下24 h稳定性试验的RSD分别为0.19%、0.53%(n=6),平均回收率分别为99.03%、102.24%(RSD分别为1.98%、1.86%,n=6),含量分别为(12.18±0.16)、(7.53±0.24)mg/g(n=3)。10批穿心莲配方颗粒样品HPLC指纹图谱与HPLC对照指纹图谱相似度均>0.99。结论:建立的穿心莲配方颗粒质量标准及其HPLC指纹图谱,可用于穿心莲配方颗粒的质量控制。

OBJECTIVE:To formulate the quality standard of Andrographis paniculata dispensing granule preliminarily,and to establish its HPLC fingerprints.METHODS:TLC and HPLC method were used for qualitative identification and quantitative analysis of andrographolide and dehydro-andrographolide in Andrographis paniculata dispensing granules.According to 2015 edition of Chinese Pharmacopeia(called“Pharmacopeia”for short),the moisture,granularity,solubility and extract were determined.HPLC fingerprints of 10 batches of A.paniculata dispensing granule were drawn,and similarity of it with control fingerprint was evaluated.RESULTS:In TLC of test sample,the same spots were found in corresponding position as chromatogram of control sample.The moisture,granularity,solubility and extract of A.paniculata dispensing granule were all in line with the standard of Pharmacopeia.The linear range of andrographolide and dehydro-andrographolide were 10.983-274.583(r=0.999 9)and 11.355-283.886 mg/L(r=0.999 9).RSDs of precision tests were 0.50%and 0.29%(n=6).RSDs of reproducibility tests were 0.99%and 0.51%(n=6).RSDs of stability tests were 0.19%and 0.53%within 24 h at room temperature(n=6).Average recoveries were 99.03%(RSD=1.98%,n=6)and 102.24%(RSD=1.86%,n=6).The contents of andrographolide and dehydro-andrographolide were(12.18±0.16)and(7.53±0.24)mg/g(n=3).The similarity of HPLC fingerprints for 10 batches of A.paniculata dispensing granule with control HPLC fingerprints were all higher than 0.99.CONCLUSIONS:Established quality standard and HPLC fingerprint of A.paniculata dispensing granule can be used for quality control of A.paniculata dispensing granule.