祛风消癜合剂质量标准研究

Quality Standard of Qufeng Xiaodian Mixture

目的建立祛风消癜合剂的质量标准。方法采用薄层色谱(TLC)法对祛风消癜合剂中忍冬藤、防风、炙甘草进行定性鉴别。采用超高效液相色谱(UPLC)法对该制剂中的原儿茶醛、马钱苷和5-O-甲基维斯阿米醇苷进行含量测定,色谱柱为Waters Acquity UPLCBEH C18柱(100 mm×2. 1 mm,1. 7μm),流动相为乙腈-0. 2%磷酸水溶液,梯度洗脱,流速为0. 3 mL/min,检测波长为232 nm,柱温为30℃,进样量为1μL。结果忍冬藤、防风、炙甘草的TLC图斑点清晰,分离度较好,阴性无干扰。原儿茶醛、马钱苷和5-O-甲基维斯阿米醇苷进样量分别在2. 86~28. 56μg,12. 32~123. 20μg,4. 44~44. 40μg范围内与峰面积线性关系良好(r=0. 999 9);平均加样回收率分别为97. 86%,99. 46%,100. 41%,RSD分别为3. 20%,0. 84%,3. 24%(n=6)。结论该方法简便可行,专属性、重复性好,可用于祛风消癜合剂的质量控制。

Objective To establish the quality standard of Qufeng Xiaodian Mixture.Methods Rendongteng,Fangfeng and Zhigancao in Qufeng Xiaodian Mixture were qualitatively identified by thin layer chromatography(TLC).The contents of protocatechuic aldehyde,loganin and 5-O-methylvisammioside in the Mixture were determined by ultra-high performance liquid chromatography(UPLC).The chromatographic column was Waters ACQUITY UPLCBEH C18 column(100 mm×2.1 mm,1.7μm)with mobile phase of acetonitrile-0.2%phosphoric acid solution flowing at 0.3 mL/min in a gradient elution,the detection wavelength was 232 nm,the column temperature was 30℃,and the injection volume was 1μL.Results TLC images of Rendongteng,Fangfeng and Zhigancao showed clear spots,good separation and no interference from the negative control.The linear ranges of protocatechuic aldehyde,loganin and 5-O-methylvisammioside detection were 2.86-28.56μg,12.32-123.20μg and 4.44-44.40μg respectively(r=0.9999).The average recoveries were 97.86%,99.46%and 100.41%,and the RSDs were 3.20%,0.84%and 3.24%,respectively(n=6).Conclusion The method is simple and feasible with good specificity and repeatability,and can be used for the quality control of Qufeng Xiaodian Mixture.