栀芩合剂质量控制方法的研究

摘要

目的 提高并完善非标准制剂栀芩合剂质量标准.方法 采用薄层色谱法(TLC)对栀芩合剂中栀子、黄柏、黄芩的定性鉴别;采用高效液相色谱法(HPLC)测定栀芩合剂中黄芩苷的含量.色谱柱:Diamonsil C18(250 mm×4.6 mm,5μm),以甲醇-0.1%磷酸溶液(45:55)为流动相,流速为1.0 mL·min-1,检测波长为280 nm.结果 在TLC定性鉴别中,供试品在与对照药材(或对照品)相应位置上出现相对应的特征斑点,阴性对照在相对应位置无干扰,专属性强;HPLC法可以测定黄芩苷的含量,黄芩苷的线性范围为0.0964~0.8676μg(r=1),平均加样回收率为99.08%(n=9,RSD=1.17%).结论 该质量标准确保栀芩合剂快速定性、定量分析,实验方法简单、重复性良好、结果稳定、可靠,能够用于栀芩合剂的质量控制.%Objective To improve and complete the quality standards of the off-standard preparation of zhiqin mixture.Methods TLC was used to make qualitative identification of gardenia,golden cypress and Scutellaria baicalensis in zhiqin mixture;HPLC was used todetermine the content of the baicalin in zhiqin mixture.Diamonsil C18 column (250 mm ×4.6 mm,5 μm)was adopted,with the mixtureof methanol-0.1% phosphoric acid (45:55)as the mobile phase.The flow rate was set at 1.0 mL·min -1 ,and the wavelength for detectionwas 280 nm.Results In the qualitative identification of TLC,the test samples had correspondent characteristic spots in the locationsin accordant with that in contrasted medicines(or contrasted articles),while the negative control was not disturbed in the correspondentlocations,which manifested strong specificity.The content of baicalin was determined by HPLC,the linearity range was goodwithin 0.0964 ~0.8676 μg (r =1),and the average recovery was 99.08%(n =9,RSD =1.17%).Conclusions The method toguarantee the quick qualitative analysis and quantitative analysis of Zhiqin mixture by establishing the quality standard is simple,repeatible,stable and reliable,which can be used for the quality control of zhiqin mixture.