摘要
目的通过对祛寒逐风颗粒进行定性鉴别、定量分析,建立该制剂的质量控制方法。方法参照《中华人民共和国药典》方法,对秦艽、威灵仙及毒性成分乌头碱进行定性鉴别;采用Waters Symmetry C18色谱柱(250 mm×4.6 mm,5μm),柱温25℃,流速1.0 mL/min,进样量10μL,以甲醇-0.1%磷酸水溶液为流动相进行梯度洗脱,波长275、322 nm,同时测定龙胆苦苷、阿魏酸、藁本内酯、欧当归内酯A含量;采用Waters Symmetry C18色谱柱(250 mm×4.6 mm,5μm),柱温30℃,流速1.0 mL/min,进样量10μL,以乙腈-0.1%磷酸(90∶10,V/V)水溶液为流动相,波长210 nm,测定齐墩果酸含量。结果薄层色谱斑点清晰,专属性强,分离度高,阴性无干扰,能有效鉴别秦艽、威灵仙,并对乌头碱进行限量检查。龙胆苦苷、阿魏酸、藁本内酯、欧当归内酯A、齐墩果酸分别在0.686~6.86μg(r=0.9994)、0.0134~0.134μg(r=0.9996)、0.016~0.16μg(r=0.9996)、0.002~0.02μg(r=0.9990)、0.011~0.088μg(r=0.9995)范围内呈良好的线性关系,平均加样回收率分别为99.90%、99.44%、99.14%、97.74%、95.32%,RSD分别为1.49%、2.69%、2.24%、1.61%、2.79%。结论本研究建立的方法简便、准确,稳定性、重复性好,可用于祛寒逐风颗粒的质量控制。
Objective To establish the method for quality control of Quhan Zhufeng Granules through qualitative identification and quantitative analysis.Methods According to Chinese Pharmacopoeia,the qualitative identification methods of Gentianae Macrophyllae Radix,Clematidis Radix et Rhizoma and the toxic components of aconitine were established.With Waters Symmetry C18 column(250 mm×4.6 mm,5μm),the column temperature of 25℃,the flow rate of 1.0 mL/min,the injection volume of 10μL,mobile phase of methanol-0.1%phosphoric acid aqueous solution;the wavelengths of 275,322 nm,the contents of gentiopicrin,ferulic acid,ligustilide and angelica lactone A were determined simultaneously.With Waters Symmetry C18 column(250 mm×4.6 mm,5μm),the column temperature of 30℃,the flow rate of 1.0 mL/min,the injection volume of 10μL,the mobile phase of acetonitrile-0.1%phosphoric acid(90:10,V/V)aqueous solution,the wavelength of 210 nm,the content of oleanolic acid was determined.Results TLC spots were clear,specific,highly separated,negative and no interference,which could effectively identify Gentianae Macrophyllae Radix,Clematidis Radix et Rhizoma and aconitine.Gentiopicrin,ferulic acid,ligustilide,Angelica lactone A and oleanolic acid were in a good linear relationship in the range of 0.686?6.86μg(r=0.9994),0.0134?0.134μg(r=0.9996),0.016?0.16μg(r=0.9996),0.002?0.02μg(r=0.9990),0.011?0.088μg(r=0.9995),respectively.The average recovery rates were 99.90%,99.44%,99.14%,97.74%and 95.32%,respectively,and RSD were 1.49%,2.69%,2.24%,1.61%,2.79%,respectively.Conclusion The method is simple,accurate,stable and reproducible,and can be used for the quality control of Quhan Zhufeng Granules.
作者
李喜香
张志瑞
毕映燕
张亚会
李季文
王雪梅
LI Xixiang;ZHANG Zhirui;BI Yingyang;ZHANG Yahui;LI Jiwen;WANG Xuemei(Gansu Province Hospital of Traditional Chinese Medicine,Lanzhou 730050,China)
出处
《中国中医药信息杂志》
CAS
CSCD
2020年第2期53-58,共6页
Chinese Journal of Information on Traditional Chinese Medicine
基金
中医药行业科研专项(201507001)。
