蒙药材黄花黄芩定性定量方法研究

Qualitative and quantitative analysis on Mongolian medicine Scutellariae Viscidulae Radix

目的:建立蒙药材黄花黄芩定性定量方法,为提高黄花黄芩药材的质量控制水平提供依据。方法:参照《中华人民共和国药典》(简称《中国药典》)2015年版附录相关方法及《国家药品标准工作手册》要求,对黄花黄芩药材的水分、总灰分、酸不溶性灰分及醇溶性浸出物进行测定;以聚酰胺薄膜为薄层板,甲苯-乙酸乙酯-甲醇-甲酸(10∶3∶1∶2)为展开剂,以黄芩苷、黄芩素和汉黄芩素为指标成分,在紫外灯365 nm处检视,建立薄层色谱鉴别方法;采用HPLC法建立黄花黄芩中黄芩苷的含量测定方法,使用Waters HHS T3(4.6 mm×250 mm,5μm)色谱柱,以甲醇-0.4%磷酸水溶液(47∶53)为流动相进行洗脱,流速1 mL·min^(-1),检测波长为280 nm处,柱温40℃,进样量为10μL。结果:在上述薄层色谱条件下,供试品色谱中与指标成分色谱相应的位置上,显相同颜色的斑点,斑点Rf值适宜,显色清晰,色谱分离好,且信息量多。在HPLC条件下,黄芩苷质量浓度在10.32～103.2μg·mL^(-1)范围内,与峰面积呈良好的线性关系(r=0.999 7),平均加样回收率为93.7%～103.2%,RSD为0.78%～1.7%(n=9)。7批次黄花黄芩测定结果表明,黄芩苷的百分含量为5.65%～12.76%,水分为5.62%～6.65%,酸不溶灰分为0.33%～0.59%,醇溶性浸出物为44.10%～48.28%,以干燥品计算,黄花黄芩中黄芩苷的含量以不少于8.0%为佳。结论:建立的蒙药材黄花黄芩定性定量方法专属性强,准确度高,操作简便,可用于黄花黄芩的质量控制。

Objective：To establish the qualitative and quantitative methods of Mongolian herbal medicine Scutellariae Viscidulae Radix and to improve the quality control level of the drug.Methods：The water,total ash,acid-insoluble ash and alcohol-soluble extract of Scutellariae Viscidulae Radix were determined by referring to the relevant methods in the National Standard for Pharmaceutical Standards and the Chinese Pharmacopoeia 2015 edition.The polyamide film was used as the thin layer and a mixture solution of toluene-ethyl acetate-methanol-formic acid（10∶3∶1∶2）was used as the developing solvent.Baicalin,baicalein and wogonin were used as the index components.The developed plate was examined at 365 nm,and the thin layer identification method was established.The HPLC method was used to determine the content of baicalin in Scutellariae Viscidulae Radix.The separation was performed on a Waters HHS T3（4.6 mm×250 mm,5 μm）column and the mobile phase consisted of methanol-0.4% phosphoric acid solution（47∶53）at a flow rate of 1 mL·min^（-1）.The detection wavelength was 280 nm,the column temperature was 40 ℃ and the injection volume was 10 μL.Results：Under the above thin layer conditions,the spots in the chromatogram obtained with the test solution corresponding in position and colour to the spots in the chromatogram obtained with the reference solution.The Rf values of the spots were appropriate and the spots were and well separated,showing abundant information.Under the condition of HPLC,the linear range of baicalin was 10.32-103.2 μg·mL^（-1）（r=0.999 7）and the average recovery was 93.7%-103.2% with RSDs within 0.78%-1.7%（n=9）.The results showed that the content of baicalin was 5.65%-12.76%,the water content was 5.62%～6.65%,the acid-insoluble ash was 0.33%-0.59% and the alcohol-soluble extract was 44.10%-48.28%,calculated with reference to the dried drug.Scutellariae Viscidulae Radix with the content of baicalin more than 8.0% was better.Conclusion：The quality standard of Mongolian medicinal herbs is specific,accurate and easy to operate,which can be used for the quality control of Scutellariae Viscidulae Radix.